Document 8NpaKj52J5yGg5J6rOJkkO8d

in JU u&x rI Distribution on last page "INDEXED" Iar30'SI. E,,X,, DU K>m m NEMOURS & COMPANY FABRICS AND FINISHES DEPARTMENT CHEMICAL DIVISION ifffttl c&py mi mu amuwm PARLIN LABORATORY CLASS A~I RESEARCH REPORT NO, PROJECT NO, J~Xo44 SUBJECT8 SANDING AIDS FOR FURNITURE SEALERS DATE ISSUED* JUNE 23, 1950 PERIOD COVERED* NOV, 20 ,, 194? TO DEC, 19^9 PREVIOUS RSPQBTS ON SAME SUBJECT* NONE NOTEBOOKS? 2222* 2246, 2266 PREPARED BY* APPROVED BY3 N 29354 TABLE OF OOMTWfl Introduction Objectives .Summary and Conclusions Action Taken Patents Experimental A, Baofcgro and Studies 1,, Specification of an Ideal Sanding Aid 2* Tbeorp of Sanding Aida 3, Evaluation Procedures Be Improved Sealer Formulation 1, Bole of Zinc Stearate 2* Sandabtlity versus Appearance and Quality 3o Jiew Sanding Alda Ca). Metallic Soaps (b) Organic Materials Co) Inorganic Substances Cd) Miscellaneous 4t Zinc Stearate Stability in 193^0 Sealer 5 Two Package Sealers 6* Zinc Stearate as an External Sanding Aid Appendix TABLE OF CONTENTS Introduction Objectives Summary and Conclusions Action Taken Patents ' Experimental A* Background Studies I, Specification of an Ideal Sanding Aid 2 Theory of Sanding Aide 3. Evaluation Procedures Be Improved Sealer Formulation !<, Bole of Zinc Stearate 2o Sandabillty versus Appearance and Quality 3, Hew Sanding Aide Ca) .Metallic .Soaps,' (b) Organic Materials Co) Inorganic Substances (d.) Miacellaneoue Zinc Stearate Stability in 193^0 Sealer 5* Two Package Sealers $4 Zinc stearate as an External Sanding Aid Appendix PAGE 1 1 2 3 DUP030001184 PARUN LABORATORY REPORT N0 $$J SUBJECTS SANDING AIDS FOR FURNITURE SEALERS INTRODUCTION . A sanding sealer serves as an undercoat for the top coat, Aether the latter be lacquer, a baking synthetic or a. varnish* The sealer is applied after the stain, wash coat and filler* The main purpose of a sanding sealer is to produce a smoothly sanded surface for the application of topcoats0 Be cause sanding involves Considerable labor, furniture manufactur ers demand sealers which can be sanded with a minimum of labor after a very short drying time* The sealer must therefore cut to a smooth surface rapidly, with a minimum of scratches and without gumming or clogging of the sandpaper* Ease of sanding is universally obtained by means of zinc stearate. A sanding sealer is one of the weakest con stituents of a furniture finishing system* Sanding sealers are brittle and impair the quailty and clarity of an otherwise highly satisfactory furniture .finish* It is for this reason that occasionally on high grade furniture and usually on pianos, a sanding sealer Is not used* msmsm Project J~I044, Parts I, IX, III and IV, provided funds for the Investigation of the factors which control ease of sanding and Intercoat adhesion, with a view toward arriv ing at sealer compositlona which represent a superior balance between the two than exists in currently available sealers, either of our own manufacture or marketed by competition* In our general background study of sealers the following was established? 1. Zinc stearate functions as an efficient sanding aid primarily because of Its lubricating properties* 2* Zinc stearate embrittles the sealer film and im pairs topcoat adhesion* 3<> When a sealer ages for sontime in the package be fore use, particularly under conditions of relatively high temperature, the intercoat adhesion.is still further reduced* 4. Zinc stearate is fairly soluble in aliphatic and aromatic hydrocarbons* Consequently their presence Or absence in the solve teomposltion largely deter mines the package stability of a sanding sealer* DUP030001185 -a* i" 1 On the "basis of the above the problem of formulating an improved sealer was approached from several directionsfc (a) Evaluation of materials other than zlno stearate as sand* ing aids, (b) improvement of the stability of zinc stearate sealers through solvent adjustments and/or encasing the zinc stearate particles in an insoluble envelope* and .Co) utilization of zinc stearate as a dry sanding aid. Although a great; many inorganic and organic materials were evaluated as sanQlng aids* none 'tms sufficiently promising to warrant replacing zinc stearate. Low molecular weight poly thene and methylol stearsmide were among the more promising materials examined. By replacement of hydrocarbons with alcohols* the solvent of 193&0 sealer was reformulated to secure about a 60/5 . improvement in stability, This sealer is susceptible to temporary blushing and its solvent composition is more expensive, A similar Improvement in stability can b affected by packaging the hydrocarbon diluent separately* to be added at the time th sealer is applied. By packaging the zlno stearate separately in dispersion form, to be added to the 193^0 Clear at the time of application* a 10Q/S improvement in stability can be obtained. These three systems were recommended to the Sales Department In Parlin Laboratory Release Letter Bo, 421, Attempts to tnsoiubiZize the zinc stearate particles with sundry insoluble coatings proved to be unsuccessful. An entirely new and original approach was the utiliz ation of zinc stearate as a dry lubricant either dusted on the sealer or coated on the sandpaper. By this means sealers con taining no sanding aid Can be sanded with great ease. Of course the film properties are markedly improved and the Instability problem is completely eliminated. Although this new method permits easier sanding than the conventional sealer* rite of abrasion per stroke is less* so that the relation of work to abrasion Is about the same in either ease. On August g, 19^9 Parlin Laboratory Release Letter Bo, 421 was: issued recommending the following, listed in the order of preferences 1, Packaging the zinc stearate mill'base separately, to b added to the clear sealer at the time of application, . 2, Packaging the hydrocarbon diluent separately* to b added to the sealer at the time of applicaMon, 3. Replacing the hydrocarbon diluent with ethyl alcohol, not reouiring separate packaging* DUP030001186 Subsequently It x/as mutually agreed with Induetrial Sales not to me out for the time being along the lines of Nos* 2 & 2 or with the ooated sandpaper but to confine Sales efforts.to recommendation No. 3* To date progress on this has been limited* patents A patent proposal* PFP-loiS* covering zinc stearate . ooated sandpaper was submitted to* the legal Department. Manage ment decided not to proceed with this because the benefits to be derived dia not warrant the cost of obtaining a patent and the case xms not a strong one* It was thought equally as much could be derived by disclosing this idea to one of the sand paper manufacturers* like Behp-Hannihg xdio is a customer of ours* {reference Dr, C,E, BartsOh's letter January 3, 1950 with attached correspondence5 * A* Baekgroand Studies ;* gpeci^lcations of an Ideal Sanding Aid / Vhm work was originally started on this project the characteristics of an ideal sanding aid were considered* Such a material should promote easy and efficient sanding by minimiz ing drag, dogging and rolling of the sandpaper, it should not Impair the adhesion, color* clarity and quality of the finish* It must be stable in the package by not dissolving in the sealer upon long-time storage and must be permanent in the dried film Moot blooming out* Finally it should b cheap and readily ailabieo > 2*: IfoggpE.MJm&m, MM Sarly in our study some attrition was given to determining how a sanding aid functions. Does it promote sanding by serving as a lubricant* by making the film more friable or in some other way? Unfortunately it was hot possible to obtain a complete answer to this question* It was not possible to obtain good sanding properties via friability alone* For example the substitution of low yageosity nitrocellulose Cl/P or lower) versus high viseoslty, 15*. to P) and the introduction of brittle gums like ester gum* gave very little if any improvement in sanding properties* On the other hand good sanding properties were in variably associated with lubrication ihsome form or other* For example mineral oil or. soap and water applied to the dried film, and talo or lanolin added to sealer composition, markedly aided Banding* Apparently a lubricant whether internal or external* not only serves to reduce friction, but permits the sandpaper to bite into the film and prevents the abraded film DUP030001187 Jfc. . partiolea from clogging the sandpaper* Furthermore, as will be discus aed later la this -report* zinc stearate* whether a com* ponent of the sealed film itself or applied to the sandpaper* functions about as well either way* In the absence of data that any other characteristic or property of a sanding aid promotes easy sanding to the degree that the lubricating pro parties do* It was concluded that this is by far the predominat ing factor* 3* Evaluation Procedures Aside from noting the general chemical and physical properties of any material under consideration as a sanding aid, major attention was given tog how well it promoted sanding* its effects on appearance* durability and quality of the finish* and its effect on the package stability of the sealer,, Sealer 19330 with 6*5$ zinc stearate on the solids* was selected as the standard for comparison, This is our largest moving sanding sealer which .we currently market and field experience has shown that 6*5$ zinc stearate represents the absolute minimum which can be incorporated into the formula without encountering complaints from our customers on bard sanding* Comparisons were made with the 19360 control in respect to dispersion* settling, sanding ohamoterletios, film properties including intercoat adhesion* scratch resistance and durability and stability, . The usual , method of dispersing the sanding aid was to grind the finely divided material with solvents in a one quart ,mill with porcelain balls. Grinding was continued until a satisfactory dispersion was attained* indicating proper particle site and sufficient wetting* The resulting mill base was then added to olear 19330 in a ladder c levels considered to cover the range of interest as a sanding aid* The experimental sealers were tested for the follow ing sanding properties with 6-0 MM sandpaper at a film build of one mil after about forty-five minutes dry* Ratings from 0 to 10 were based on a standard of 10 for 19380* Start - ease of sanding the first six strokes Ease - ease of sanding the next ten strokes Flour - the amount abraded with a standard weight CIO lbs, on 4 sq,in.) in five strokes Glog . the amount of clogging of the sandpaper with twenty heavy strokes* Film properties of the experimental sealers were evaluated in complete test finishing systems on mahogany and walnut veneer panels* Half of each panel was coated with the experimental sealer and half with 19330 control, thus tan system was identical on the whole panel except for the DUP030001188  c"5<" sanding aid "being compared to the standard sine stearate in the sealer coat, Tests with coin and knife for mar resist ance, scratch areal stance, toughness, and adhesion were made on the green finish after one day dry at room temperature and again after three days additional dry at 120"F, Whenever it was deemed necessary, old crack and even durability tests were run. Coin Test Ratings 0 White, complete separation of film 1 m Heavy, white streak 2 * Medium, white streak 3 m light, t#hite streak 4 Indentation only Ibife Test Ratings 0 lifts m continuous sheet 1 m Lifts in strip easily 2 *. Outs off strip cleanly 3 Outs off pieces tilth good resistance 4 Film removes raggedly tidth bits of wood It should be noted, that adhesion and toughness sore two separate and distinct characteristics of any surface Coat ing, in practice they are so closely related that the practical furniture finisher seldom attempts to distinguish between them. Brittleness and poor adhesion are present in finishes that scratch white or mar easily at the slightest impact. For example a piano lacauer {like types B or H) will invariably produce a more brittle finish over a sanding sealer like lBi5$ than the same lacouer directly over wood or a primer like 1366, The toughness of the topoeat is entirely lost by the brittleness of the undercoat. In this report we shall attempt to differentiate between brittleness and poor adhesion. Package stability of the liquid sealers was tested, for the most part, by accelerated aging. The sealers were aged simultaneously for three days at room temperature and at 125F. with 193&O as a control* The aging at elevated temperature was found to ..closely reproduce the aging effect on X93$o of about three to six months at room temperature. In the case, of the most promising sanding aids, these data were supplemented by actual aging for long periods at room temperature. In either case the aged sealer was tested for sanding and film properties versus unaged sealer, Wherever variations from this general pattern cf test procedure wero necessitated by the peoularlties of the sanding aid unuer vest, brief descriptions of the modified techniquea are given. DUP030001189 TabCr Abraser -Bo effort was made to establish our tests on a semi-quantitatlve basis through the use of a Haber Abraser, The Haber Abraser Is a testing instrument for measuring the rate of wear of surface finishes subjected to rubbing abrasion, Bobber* abrasive containing discs rest on the material under test which is mounted on a turn-table. Rotation of the table cause the abrasive discs to rotate with an abrading action. Abrasion is measured by the number of cycles to wear through the test material or by the weight of the material abraded in a selected number of cycles, Com parison may be made to a standard material or to standard values expressed in. cycles or weight, The coarseness of the abrasive wheel and the weight on it may be varied to suit the material under test. It was thought that the Haber Abraser might be use ful to measure sandabiiity of sealers, The method of weight loss of abraded material was chosen for several reasons. The wear through method requires even film builds accurately measured. It requires close watching and varying and longer test runs. The weight loss method requires two weighings but was considered subject to greater accuracy. Aluminum panels were found to yield greater accuracy than steel in weighing to 1 milligram. Tests were conducted with sealers containing'calcium silicate* polythene* and varying amounts ofzino stearate. Best results were obtained by using a CS-lTf wheel with 250 gms, ' Weight, 1000 cycles, and the film dried 16 hours at .120*S\ Whii the variations in Banding aid did reflect in the amount of sealer abraded* the reproaucibility and sensitivity could hot be developed to show superiority to hand sanding tests. The indicated correlation between the Taber Abraser data and Shown sanding quality did not Justify the more involved maohin test. The Timber Abraser was also evaluated as a means of testing adhesion, finishes were coated on small plywood panels to fit the turn table. Ball and coin shaped tools tested on the finishes were found to require a weight far in* excess of the capacity of the machine. The ^Shear-Hardness Attachment , a . tool with a cutting edge* was found of some use$ but inteipretation of results depended on visual evaluation of the out film* This did not prove to b a very valuable test method. DUP030001190 -7- ' B* Improved Seal eg Formulation 1. Role of Zinc Stearate Practically all wood forntture la coated tilth a lacquer sealer* This sealer Is dry-sanded smooth before the application of any topcoats* To facilitate the dry sanding* a lubricant* known as a sanding aid/is incorporated into the sealer* The sanding aid used throughout the industry is zinc . stearate* Zinc stearate is a smooth* slippery soap. It minimizes scratching of the film and clogging of the sandpaper* 2* fahdabillty. versus Appearance, and quality. A Sanding aid* like ztno stearato/ always etracts from the toughness and adhesion of the finish* Sealers heavily loaded with zino stearate to give easy* powdery sanding after a short air dry, give good hold out and are economical ih labor but produce a brittle finish* The zinc stearate in sealers tends to settle* If not well stirred before use* the sealer from the bottom of the container will contain too much zinc stearate and the.film will be brittle* The sealer drawn from the top Will not con tain enough sanding aid and will be difficult to sand* Serious consideration was gives to reducing the zinc stearate in X93SO to improve the film properties* Although changes over a fairly wide range were made from time to time, the demands of the furniture trade, as evidenced by actual field experiences indicated that 6*5$ zXfto stearate on the solids is the minimum acceptable to maintain the re outred ease of sanding* Zino stearate varies ohly slightly in. composition and properties between the various grades available* By way of illustration, a variety sold under the trad# nameHMetallac" and highly recommended by the manufacturer. (Metasap Chemical Co*) was found to be Identical in properties. As a sandihg aid to the grade used in 193$ under the code G-6di* The prospeots for obtaining an improved sealer through the selection of a superior grade of zinc stearate aid hot appear promising* As already discussed the inclusion of zinc stearate embrittles the sealer film and impairs topcoat adhesion* Further more ample evidence was obtained to show that when a sealer con taining zinc stearate ages for some time in the package before use, particularly under conditions of relatively high temper ature, the tatereoat adhesion la still further reduced* DUP030001191 A very considerable amount of time was devoted to the search and evaluation of new sanding aids In comparison with zinc stearate# Numerous organic and Inorganio materials were examined among which were the followings (a) Metallic Soap M&Mil Apa Bms&M Re evaluated ever a range of coneentratlonsTas sanding aids in 19300 Sealer, In place of zinc stearate* They were introduced In the same manner, namely in the form of ball mill ground dispersions, similar to the zinc stearate base MS-167 used in preparing 1930 Magnesium stearate yielded a mill base like zinc stearate, thick in consistency! but the mill bases of the barium and lead soaps Were thin and milky. As sanding aids the magnesium sbap wae shout equal to^he zinc, while the barium liras slightly Inferior and the lead decidedly inferior. Sealer i.9300 formulated with either barium or lead or magnesium stearate as sanding aids was comparable to standard 19300 in respect to general film properties, clarity, adhesion to filled wood and interooat adhesion with I63O3 Type 111 and I50O2 Type 0 topcoats. ' All four sealers were rated equal In cold orack resistance teste under 169QO VB topcoat. In respect to stability and heat aging, zinc stearate was better than magnesium, and barium and lead were a poor third and fourth. Heat aging in general tended to dissolve the stearates. This increased the gloss and impaired dry,hardness, sanding and adhesion. Agitation at room temperature accelerated the . solution of these stearates in the sealer, increasing the viscosity. The results parallelled the effect of heat. In that zinc and magnesium have the least effect on vis00sity while that of lead and barium are greater. Calcium Stearate Several concentrations of calcium stearate were tested, A level of 0$ calcium stearate on the solids 1ft 19300* Imparted ease of sanding comparable to standard 1930 with 6.5$ zinc stearate* However, flouring was slightly less and clogging was slightly greater. Adhesion was superior to 19^* By increasing the amount of calcium stearate to 12$, flouring was eoual to standard but clogging increased also. Adhesion was comparable to standard. Calcium stearate appeared slightly more stable than zinc stearate, but the overall balance of properties did not warrant further interest. DUP030001192 'lithium Stearate Lithium stearate was directly substituted for zinc stearate in the preparation of M3&167 Mill Base, lithium stearate liras difficult to disperse. Concentrations of 4.7%a 6,5# and 9,t# on the solids were tested in 19360, The higher concentrations of lithium stearate gave excessive clogging upon sanding and inferior film properties compared with standard 19360* The sealer with K?$ lithium stearate was only Slightly inferior in sanding and adhesion. Stability was comparable or slightly superior to standard. Lithium stearate reduoed sealer viscosity about tea seconds (#7 eup) below that obtained with zinc stearate on the same basis. Lithium stearate darkened the sealer, which color change became very pronounced upon heat aging. This color change was one of the most serious deficiencies of lithium stearate. The balance of properties exhibited by lithium stearate did not recommend its substitution for zino stearate* Strontium Stearate Strontium stearate when substituted pound for pound for zinc stearate in 19360, imparted somewhat inferior sanding and was comparable for adhesion. Stability sms superior in heat aging tests, A 50$ higher strontium stearate content was required to secure sanding properties equal to standard 19360, At this higher level, film properties were inferior and stability as poor as standard. Aluminum,Stearate Aluminum stearate was not tested because of its lack of stability as previously established in a study of f urniture ttPucot, topcoats, - Zinc Salts A number of zinc salts were evaluated as sanding aids. Dispersion of these materials obtained in powder form, was ac complished by grinding in a ball mill with the earns solvent blend as is used with zinc stearate in HB-167 (70^ butyl acetate, 16$ butyl alcohol, and 12$ isopropyl alcohol). Solids in the res-, peotive mill bases ranged from 15,2# to 32,6#, Samples 2256-16 and 2258-17 (See Tabl I) became plastic masses In contact with solvent and were mtot given any further oonsideration. , h remaining substancesincorporated into 19380 clear sealer in proportions ranging from 3 to 11# on the sealer solids. The dispersions were in general initially satisfactory In oases there was subsequently objectionable settling, 0 pounds 2256-15* 2256-16 and 2258-19 settled to a soft paste not easily redispersed,' Ali the experimental sealers were tested for sanding stability. The more promising were tested for film properties and DUP030001193 -ioTABLE 1 Code Zlno Salt of - ' '* T.S* in MB % Sanding Aid on Sealer Solids Film Heat Sanding Proper- Age Quality... ties stability 0-661 220>215 0-16 Aeld . 23.6 . -*1 Boslffc-ialelc acid 23.6 adduct 6.5 Excellent Fair Poor 6o5 Poor Fair - . 2205-223 ? Stearic acid and 23,,6 rCsln-maleic acid adduct 6.5 Pair Good Fair. 2205-224-. 2205-224- 2205-272 2256-12 BoediMaaleio acid adduct C-i4- acids (Weeolin AAB) 6*22 acids 6-12 to 0-22 acids 23.6 23*6 >v 19*6 15.2 6.5 Fair 6.5 Good >9 Poor 4-o 5 Pair Good Fair, Good Good Poor Poor - 225S-13 2256-15 2256-16 2256-I7 2256-16 2256-19 2256-29A 0-16 to 0-22 acids * Half ester of styrene Maleic anhydride 20.6 30.6 Biphenyl ether dlolelo acid adduct JS.G, Hydrogenated dimer acids N.G0 Polythene Di-lso 20.0 propanolsmine sulfonate Dimer acids. 30.0 Adduct from dry- oil acids 12-bydro stear!0 20. h acid 6.0 Good 9.0 Excellent 3-10 Poor .~ - c* Good Good - - Faih * : : . ;Vi: :V1 . '.V 'V: 1-11 Poor >11 Poor 4-11 Poor *- ,,;4- .- - :3i '* ." '' * 224-6-242 Sebecie aold 250 4-ii Poor m DUP030001194 Only one zinc salt (2258-13) ms found to to compar able to zino stearate in sanding and film properties Im parted to 19380s the teat age> stability appeared slightly superior to zinc stearate. However, this material Is the zino. salt of C-16 to C-22 acids} and becInelS its composition and properties are so close to zinc stearate, ohly limited.: consideration. was given to it. Zinc laurate (2205*22*1*) offered good sanding quality hut it proved to he more soluble than, zinc stearate* The dissolved zino laurate impaired sanding hut did not appear to affect adhesion and toughness* As a heoh On the preparation of the zino salts listed In Table I, a laboratory hatch of sin stearate (2250-30) was evaluated* While it was not identical to Q6oi in all respects, the two soaps imparted very'similar properties to 19300 Sealer m respect to processing, film properties and stability. These results imply that the general method used in preparing these materials ms satisfactory. Aluminum Soane Aluminum palpitate and aluminum aebaeate were evaluated as sanding aids. Neither material imparted desire* able shading properties* (*>) 0^anlc..Materi^B ' - Stsaramtdeg Methylene dlstearamlde and methylol stearamid were evaluated as sanding aids. The latter was found to he of greater interest* At a concentration of 4$ on the sealer Solids it imparted fair sanding quality with film properties equal to standard. Initial accelerated aging tests at 125". for three days showed excellent stability with little or no degradation of film 'properties# However, aging tests at room temperature over a period of several months revealed that the methylol Steahiaside Slowly dissolves resulting in poor sanding, but without impairing aahBsloi| and toughness* The following were evaluated as sanding aids and rejected because they were poor lubrioantsi ?^1637 Stearaiaiaoiaeislayi acetate MP-163S Mono-octadecyl urea MPPl639 bi-ootadecyl urea MHX.1640 N-00tadecyl carbamate MPJX.X675 Di-octadecyl carbonate DUP030001195 -12- Fine dispersions of polythene Ip finishes are Known to impart slip to the surface of the film This lubricating feature was thoroughly investigated as a basis for the develop ment as a sealer sanding aid, It was established that polythene will impart ease of sanding about equal to zinc stearate* but with more clogging and less fluaring* Stability and settling properties were excellent. Unfortunately* at the maximum level of polythene affording good topcoat adhesion, sanding is un satisfactory. Low Molecular Weight Polythene K&.3411 ' KG-3KII was dissolved in ah equal weight of xylol vB-503) at 12O0, On cooling, the gel formed was ground in isopropyl alcohol (H-69). The resulting Mill base (J-MB-X, 0077) with 25^ solids was of paste-like consistency. Sanding improved up to a level of 2.5% K<3-3Hll on the sealer solids where it was stall inferior to standard 19300, At this level intercoat adhesion was comparable or slightly inferior to standard* Glarlty of . the polythene .sealer was superior to 19300, Polythene 6641-93 # Polythene 6641-93 hade at the Experimental station, as an aqueous dispersion .with an-azO catalyst and having a particle size of o,5 - 3.9 microns, was evaluated, this polymer is soluble not* in the Usual solvents and fuses at 120*0, Polythene 6641-93 was dissolved in xylol at 1300, and rapidly cooled with constant agitation to a gel which was subsequently ground overnight in a bail mill, the re sulting grind was coarse and poor ih respect to dispersion, tfe did not succeed in dispersing Polythene 6641-93 satis factorily, 1 0 2*0% of 6641-93 was added to 19300 Clear, the results were of limited interest since the poorly dispersed polythene gave a rough sealer. Polythene 6641-165 was prepared at the Experi mental Station with a persulfate catalyst and at a particle size of approximately 0,3 microns* this polymer is, insoluble and does not fuse below 250*0. o-a.o^polythene 6641-165 was tested in sealer films, the sealer with 1,3# polythene, compared with standard, had better starting and greater ease of sanding but waeinferlor ih flouring and clogged the sand paper.topoOat adhesion was comparable or better than standard. On heat aging, this polythene sealer maintained a superiority in, adhesion and film properties*, '. DUP030001196 -13- Polythene 6623-3.02 Polythens 662^102 received from the Experimental Station was ground to a smooth mill base in butyl acetate (B6). The solids content ms 22.70 polythene and 90 processed linseed oil (B~l4l)., A range of 1.5 * S.Q/6 polythene on the sealer solids was tested. At %$ polythene 6623*102, adhesion' was comparable to standard. At this level there was good.ease of sanding but some clogging and Very boor flouring. Polythene 6625*102 was submitted as an equivalent to 66AI-165, However, with the latter* better sanding' and comparable adhesion were obtained at the 0 level. Polythene From the Polycheialoals Department v'< " Four samples of polythene were obtained from the Arlington Laboratory of the Folyohemloais Department, Code jfegjftigj m SM5S2 D15 115 115 i' gHvit 0.3 *%ams extruded Ih 10 minutes at 190^, through a standard orifice." .0*. These materials were supplied % a particle size too coarse to b ground for use as a sanding aid. 55 was dispersed by cooling a solution in hot xylol and grinding to a mill base of 0-100 ^blids, , . Properties of the sealer were about equal to those obtained with other pdlythenes such as KO-3hll when treated in a similar manner, difficulty was encountered in making dispersions of these four polythenea fine enough in particle size to be usable in sealers, both from the point of view of appearance and sanding. The first grind of D-55 required So hours for reduction to tb necessary particle size. The other three polythenea, even on prolonged grinding, were too coarse for use in sealers. To produce finer particles various grinding media were tried, such as, heavy petroleum naphtha (S~200), butyl acetate, methyl isobutyl ketone, blown castor oil, processed, linseed oil, perchloroethylene, xylol and toluene. This approach did not give the desired reduction of particle size. The Banbury mixer was investigated as a meant bf producing fine particle size polythene,-' Thedispereed poly, thene was much too coarse to be usable. DUP030001197 Another approach was to try more rapid oooling of dilute polythene solutiona, Concentrations were reduced from a range of 25-5Q/& to about 15$, Very rapid cooling was ob tained by shook coolly the hot polythene solution in a dry ice* kerosene bath tdth rapid mechanical agitation. Extremely rapid precipitation was obtained by the addition of a second portion of old solvent just as the first polythene'particles appeared. By pretreatlng &55 in this manner it whs pdlSsible to disperse it by biremight grinding to yield a satisfactory particle size, S~g82, 8~Bf$ and 9-15 did not respbWd satisfactorily to this treatment, .., v:>>s. - v galvthe&s Dispersion Without Grinding . 1' .Still another approach to the problem.;of polythene dispersion was the rapid cooling of very dilute.solutions, 1.0 - 1,5$ ih toluene (B*47), and direct incorporation into : the s#ier without grinding, The resulting dispersion were inf erior as judged by pours on glass. However* it was found that spraying greatly improved the degree of dispersion, pro ducing much smoother fiXi> f it was also established that a colloid mill {Diaper Mill) ifould effect good dispersions in , -ftfa&.;&eeXer, of shook cooled ^polythene, 0-34X1 and S-879yielded the finest^ diapersions and IU55 ana Dul5 the coarsest. In Mineral, sanding and adhesion Of these sealers shotted no great,firiationso p-34ll seemed slightly better in sanding and slightly poorer in adhesion,. while D-15 seemed slightly inferior,1C sanding and superior ih adhesion. It is possible that theseMifferences may be related to particle stse and degree or dispersion, These reeuXia indicated that the polythenes S^arte&xelatXar properties as sanding aids and that particle size, mspersion, as well as proportions were of great importance, IMimprbvemeat in the sanding - adhesion balance of properties was obtained with this method of dispersion, Maismiajsisi To cross cheek the vehiole of 191^0 as a testing medium for polythene sanding aids, 0,7 - 6,7^6 X0-3^11 was evaluated in 19155 Clear Sealer, Polythene KGUlhll imparted good ease of sanding, but this was accompanied by logging and poor flouring at the low proportions necessary for good topcoat adhesion. These results roughly paralleled those obtained with 193SO Clear, However* since 19380 was'the superior sealer, it was deemed advisable to test polythene in the better medium to avoid any masking effect of the poorer properties of 15?155 DUP030001198 *3.5=* polythene -with Zinc Stearate The partial replacement of zlno stearate with poly thene In 193&0 was thoroughly investigated, - Results showed that not enough zinc stearate could he replaced to Improve stability T/lthout Impairing sanding properties to an unaooeptable degree* Ethylene Folysulfone A sample of ethylene polyaulfone 0C-2-16X was ob tained from Dr, I,L, Haag of the G-rasselli Chemicals Depart ment, Cleveland, Ohio Laboratory, This material was ground with solvents in a ball mill, and the resulting mill base was added to 19380 Clear, Proportions ranging from 2-10$ of the sealer solids were evaluated. Ethylene polyaulfone did not offer the ease of sanding of polythene. It clogged badly and was low in flouring. Topcoat adhesion was much less adversely affected by ethylene polysulfohe than by polythene when Used on a pound for'pbund basis in 19300 Clear, ' %SwH A sample of ethylene polyaulfone OTE.65i.6~g was obtained from Dr* AB, Nehs of the Experimental station, This Was tested in ooi^ari son with 00-2-161, Dispersion of CDKB651o*S was better,, and consequently the sealer film . clarity was alsO> better* It was slightly superior in sanding and about equal in adhesion.i i Anhi'di'CU lanolin HtJSP Map Lanas) was added to 19^0 Clear Sealer m proportions of 2,5*20$ of the film solids, At the lp$ level, sanding ws almost equal to standard tilth more slip but less tinuring, Th film was slightly softer than stand ard, but topcoat adhesion was satisfactory. In the aged finish, the lanolin appears to exude somewhat through the topcoat* Seat age stability was good except for more pronounced exudation. Polymerized RC-000 . RCWSoo is the monomer, tetraethylene glyool dlmethacrylate. It was thought that by tumbling or grinding, a solu tion of the xaonomer,.might Polymerize to fine particles rather than a solid c&he. Tumbling would offer continuous agitation* while a ball, ill would off|s* in addition a grinding action during polymerization, Tumbling did not convert 5, 10 or 25$ solutions in three days, and this method was hot further con sidered, Fourteen grinds were run with, varied proportions of RC-fOO and solvents, catalyst, and processed linseed oil 18-141) as a dispersing agent* Difficulty was encountered due to: the fact that the conchti^ti<>h;df:'B<i!iC& necessary: to convert resulted in rather Immobile mixtures and ineffective grinding. Seventeen percent ^s found to be the minimum level for conversion, This level {2246-52aQ) was selected for further study. DUP030001199 -i62246-52- EC-800 HB-6 E~12 H-69 Cobalt Hitrate Benzoin' Hl4l 100 3Z 54 4 4 -sir After polymerlzati on* consistency was reduced for further grinding by, addition of 2$ grams of the solvents alia 25 grams of HX410 The grinding effected gradual improve ment up to 34 hours, the mill "base 52-0 and 193^0 clear Were combined in several proportions. Fine particle sire polymerized BC-gQO offered some ease of sanding along the line of friability* but it was very harsh and hard with none of the smooth slip and Mte of a good sanding aid, the clogging incurred was undesirable* and the flouring was extremely poor, . ' , fo) H'8antobel^ 0 ' ' t'.'y. " .... l`" ' . k? ,/ . *Santoeel* 6- is a fine partiole silica raarhetedby fh Monsanto Chemical Co, as a flatting agent, Xta possibilities as a sanding aid were investigated, ttSantooelM -0 ground in !. solvents and added to 193SO Clear tended to disperse poorly. Addition Of plasticizer to the grind gave a satisfactory die* persons :-s - Santooei 0 in 19380 Clear did not adversely affect viscosity and settled to a soft thick layer which rdispersed readily. As a sanding aid MSantooelw 0 was not comparable to zinc stearate and was of little value. From 0,6 - 7.6J <BantoelB 0 in the sealer film gave optimum results# whereas 10-12$ adversely affected film properties, Low levels of wSantoeel" 0 afforded improved adhesion to topcoats. Heat age stability of MSantocelK 0 was excellent, wSantocelw 0 and Polythene It was considered that the poor sanding but good adhesion imparted by "Santooel*' C might be improved or balanced by the better sanding bat inferior adhesion imparted by poly thene, Varying proportions of l,$aatocslw and polythenes 664l-l65 and XC^3^XX vespeotiveiy*were evaluated in 19380 Clear, fhe sand ing: 'properties' of' the- 'Straight.'polythene:-' sealer were degraded :, : % the addition of Chhtoo#" 0 without any corresponding im provement in adhesion. Heat age stability was good. DUP030001200 *17. . HSmt6oellt g * Polythene . 2Ino Stearate Unsuccessful attempts were mad to blend "SantooelB polythene and zlne stearate to achieve a balance of good sanding, good stability, and satisfactory adhesion* \` Lanolin and "Santooel" C ` t% was considered that lanolin might be combined. td.th "Santoeel ts to advantage as a sanding aid* Although a fairly high degree IST ease of sanding was attainable, clogging of the Sandpaper and %eduoed flouring were encountered. Topcoat adhesion Was satisfactory. Package stability was superior to 19380, However, .^.previously mentioned, lanolin tends to exude from the dried film Upon aging. -f Lepisll, ;a grade of calcium silicate obtained from the Owens-Illinois Glass Company, was evaluated as sanding aid m 19980 and 16020, While calcium silicate did impart ease of sanding, this was inferior to nine stearate C? vs, 10), Twp percent calcium silicate was considered the optimum proportion, since more than this did not improve sanding and tended to impair film clarity, toughness and adhesion. Calcium silicate in 19380 Clear settled rapidly to a solid, pasty layer which was difficult to redisperse. One percent of Nylon (Type SAl-DV-o&o) on the calcium silicate was added to the mill base, it was hoped that the Nylon would aid in the suspension of the calcium silicate, The addition of Nylon did not reduce the hard settling, v` . Combinations of calcium silicate and polythene (K&f 3411) were evaluated. As the proportion of calcium silioate Increased, sanding quality was reduced and adhesion improved, No worthwhile balance of properties could be attained with these materiais, ' ; ' 1^132 is a hydrated magnesium silioate of tabular structure. This talc was ground with thinner in a bail mill for forty hours. The resulting mill base Was adde# in vafying proportions to 193S0 Clear, The jperimentai sealers in pours on glass were coarse, showing poor dispersionj but spraying produced smooth films, microscopic examination showed a good distribution of particles with some scattered larger particles or agglomerate imparts good ease of sanding but with a harsh feel and rasnsound rather than soft and essentially noiseless sanding with sine stearate. There was a slight' tendenoy.t cleg and flouring DUP030001201 -16was extremely poor.. i&hding' did not Improve much with Increased proportions of talc* Film properties and.,adhesion. *rere satisfactory and superior to 193&O in complete test finishing systems* Talc reduced film clarity to an undesirable degree* Mlagonized Asbestine Micron!zed ashestine was ground with thinner in a hall mill* Quantities of 2 to lojl were added to 19360 Clear on a solids basis. Dispersion was good, hut hard setting was encountered* Micron!zed asbestine gives fairly good ease of sanding hut with excessive clogging and low flouring. Adhesion of topcoats is not seriously impaired* Clarity is reduced, especially at the higher levels of mioronized asbestine. . mmrnS Polymer K (hydrated nlekelous oxide) was evaluated as a sanding aid* A pulp process pigment dispersion of Polymer t was used to replace MSEKL67, zinc stearate ip 19360 Sealer* Proportions of 5 and 10# on the sealer solids were tested for sanding properties. These tests showed no indication that Polymer K is of any value as a sanding aid. (d? Miscellaneous ' in our search for ways and means to obtain ease of sanding, without zinc stearate or with reduced amounts of the latter# the brittleness or friability of the dried sealer film was varied over a reasonably wide range, For example# nitro cellulose of different viscosities, the introduction of a brittle gam and a change in type and amount of plasticizer were studied. These and other studies added to the'evidence that friability per ee does not produce good sanding properties. A lubricant of some type is required. To investigate the effect of nitrocellulose,,viseosity on sealers, 19360 was made with 10-15 ops.# 1/6", lAw# 4-6% and 4o-60s grades respectively. Standard 1936O is formulated with a 1/6 - lA-n blend of nitrocellulose, in all cases zino stearate was required for good sanding properties, AH the sealers exhibited comparable sanding properties. Although the Vo" and 1/4B grades were sometjhat superior in package stability, in no case was the stability afforded zinc stearate outstandingly superior. No basis for altering the nitrocellulose viscosity in 1936O was establishedo DUP030001202 Estep Gum la an attempt to Improve Bandings 10^ and 20$ of the nitrocellulose in 19360 Sealer were replaced with, ester gum (&-6bg) The resulting sealers were tested with & no stearate and polythene-zinc stearate, as sanding aids. The substitution of ester gum slightly reduced ease of sanding and increased clogging with either sanding aid* The ester gum impairs film properties in the Complete finishing system as measured by coin and knife tests* v Triphgnyl phosphate (&-628) was evaluated as a plasticiser in place of blown linseed oil (E141) in 193SO* various proportions of this plasticiser and hltroceilulose were tried, yielding a range of. films from very brittle to overplastioisedo Sanding was poor with rolling and dogging in the absence of sine stearate* : ** && Magate. StabUlty in 1.9360 dealer ,: ;' Since the r#lacement of zinc stearate did not,-c appear possible Without unacceptable sacrifices especial sanding propsrties, :seviral avenues of minimizing the de ficiencies of zinc etesrate were investigated* ft was decided first to make a study of the instability of zinc stearate in 193^0 Sealer to determine vrhat happens on aging and why* "v:y '..Wikk 19380 ages the main stability factor of interest is the impairment of adhesion and toughness in a finish* ing system as measured by coin and knife tests* For the purposes fit this investigation* changes in'the following were oonsideredi 1.- Appearance 2* Viscosity Acid value Dissolved zmo Stearate Fii Properties I: Wood Adhesion interooat Adhesion .The amount of water in 19360 Sealer Was one of the first factors considered in regard to the stability of zinc stearate* The only material of standard quality that would yield mors than a trace of water in I93SO is the nitrocellulose* This contributes about 0*5$ to the seder* The effect of 0-4$ water was evaluated la 193^0* Water decreased the viscosity of the lacouer but had little other effect* Anhydrous 193^0 was found to offer no improvement In stability with zinc stearate* DUP030001203 "20= Inorganic Acids Another factor considered was acidity. Standard grades of nitrocellulose may toe expected to introduce 0,01$. acid to 19330; The effect of 0-0,1^ acid (%S04 and WQy) was evaluated,, Exoeae acid decreases the' viscosity* inoreases the aold valuer slows the drying, softens the film tout does not affect adhesion to wood nor topcoat. Excess aold in the "heat aged sealer appeared to increase sine stearate solubility tout not enough to account for the changes in adhesion to topcoats. Excess of tooth acid and water reduced viscosity, slowed drying, and embrittled the film tout did not impair adhesldno Addition of linseed oil fatty acids, to represent an Increase of 5 and 10 in the acid number of the ax4l, did not seem to affect the lacquer except to raise the aoid value, .. .Extensive tests were run to determine what the effect of stearic acid would toe from any possible hydrolysis of zinc stearate. If all the zinc stearate in 19380 hydrolyzed, there would toe 1,17* free stearic acid in the. laoquer. More than 0,2> stearic acid retarded drying and hardening of the sealer, The effect on adheeion was inconclusive. The main point learned from these tests was that more than a small amount of stearic acid would markedly slow up the dry of the sealer, Any amount less than this would not noticeably affect the film properties of the system. stearic acid was considered of less importance when an analysis of heat aged 19380 showed the presence of only minut amounts of stearic acid. Retarded drying was never obse-rved' w' ith-.'*}-*ag' ed sealers* ' -- w Triethanolamine A sample.of 193$5 Sealer, J-071052, several months old produced films that were soft and cheesy, imparting poor adhesion to topcoats* Addition of 1% tniothanolamlne made ' the film slightly softer and improved .adhesion very slightly* 19380 type sealers .-wars' prepared with * 2*70 And 5.5^ zinc stearate mill base MR-167* The'latter is the amount which was present in the standard formula. The sealers were aged for three days at room temperature, 110^F, and l4oP. DUP030001204  v /y .Jkika^ttsin of the aged sealers showed that at; room temperature 20^ of the zinc stearate dissolves. In 193210 (5*3$ VB-1GTX*. 22$ dissolved at 110*'., and Mft dissolved at lhoFo The sealers oontalned very little free stearlo acid since the combined free fatty aside were generally of the order of 0.01$ and not. more than 0.03$. At iloF. the viscosities of the three sealers dropped 7 to gn in No. 7 eapo At l^Q9. the decreases in viscosity were 13*, 19* and 22*, increasing with the amount of miXlbas present. The higher temperature caused darkening of the sealers, yellowing of the films* and impairment of sanding. With sealers aged at 110^F. the film properties of the finishing systems were unlmpalredo With the sealers aged at 140F,, there was only slight degradation in the case of the clear hut a pronounced impairment with the sealers containing zinc stearate* It may he concluded that elevated temperatures causes a large increase in the zinc stearate dissolved in 19380. This apparently correlates with a decrease in viscosity, a darkening of color, and an impairment of film properties la the finishing system. Solution of the zinc stearate does not result in an inoreased free steario acid content. wx Of the analytical data suggested that the zinh,:atehfa|e:imi^ht dissolve directly or possibly through. . some int^medii% ractlon. To determine impossible the mechanisme 'wherby aino stearate dissolved in the sealer vehicle, selected combinations of the ingredients in 193S0 were heat aged three daya at 12$F.. and the remaining ingredients were ; subsequently aided to complete the formula. DUP030001205 M 0 S*. 53 HH t* 0 5 ril a k m#: H H . . HI X8 p*m 43 H ME> H * H cn ra <* H *33 *3 St o X >.w ftrt H aos$ *3 Sp3i~! AXj iH >r-S WO! *8 *4#H M xd S3 A >5 h a w H ri H 4 o 30*' SXkJWHce4tfWirW6t ClOOHSOSJKfS0ii *CJ 03 38 Hrt 88 mw S3 HO P XHHCrV4ir{Ji (h,------- *2J5* +5 j o o *s (&, StnOs>* <o V O S4 i..p *40 <1 uo vHOOftt *<4 ra ko OO vostfl i *4 ' O. SJH * o h JHO &? H t44 Hf$I H HmfeC ' It >SA8P* 11 ,, 83 OH o tu .* 86 s* ^ H<M>H* Sp_. * H flj W Rro<H$g4 0 *a <H O 4> ^ 3 +d<4sS3a it! Hi4M3' <S O *rj <3 * g <ordd$ * <d3-43 Oa H 4= 0i , fijJ rt W iplJts ----- Ss S ra-j O . S3 *4 O *H &# 4&<St*0n\^-c ' " HI 4* iitW. i *? & A <S <tS U*4 t *"<.434>3 ` <N a> <W. :HI <* H i o . o ; ... .0 .as ' ,(fe: DUP030001206 gonoluslonsS i A, B and C darkened and viscosity decreased similarly to standard* These were the only formulae where nitrocellu lose was heated, and apparently this Isa factor in these changes* However, film properties are not necessarily related to viscosity or color changes, sine 1>, E, F and I showed that poor film properties may result even though oolor and viscosity remain unchanged^ A to F and I were poor in film properties and in nil these, instances the solvents were heated! G and :H were unimpaired in film properties and in thee cases no' sol vents were heated* In X, only the sino ate'shate and solvent were heat aged; and the resulting sealer exhibited by far the poorest film properties fids may have been due to the more concentrated solvent effect* E and G were repeated with check results on film properties but net on viscosity This .*oi!k- indicated that zina stearate dissolve* in and may possibly react with 19380 solvents* this evidence of the solubility of cine steafate in 19330. solvents, further investigation was conducted to determine the effect of each of the lacquer solvents and diluents. Aliphatic and aromatic hydrocarbons were found to have th greatest solvency while the lower alcohols had the least* Higher alcohols, bsters and ketones were inter mediate in effect but closer to the lower alcohols As a basis for formulating sealer solvents with ` low solvency for zinc stearate, considerable study was made of the limited llterataE available on th .subject* Ho direct information on zinc stearate was femmd, but data on related Compounds such as stearic acid and other soaps Were combed for leads* The literature showed a decrease in solubility for the longer chain compounds and a rise in solubility with an Increase In temperature* The metallic stearates vary in solubility, for example lithium stearate is reported more soluble than magnesium stearate Hydrocarbons were scarcely mentioned, but one reference showed stearic acid to be twice as soluble in toluene da in ethyl acetate Water in ethyl alcohol was shown to repress stearic acid solubility Butyl and isopropyl alcohols were given as better solvents for stearic acid than ethyl alcohol; ; Indications that methanol and nitromethane might be poor solvents for zinc stearate led to their evaluation in 19330 sealer, -They were found to be about ..equal to ethyl alcohol in improving stability. Being toxic they were of little further interest* - An attempt was made to determine the solubility of zinc stearate in common lacquer solvents and diluents at 20<3,, and 50C.:The data| were not considered very significant because petroleum naphtha (H~S9) was shown to be less of. a solvent than ethyl alcohol P*l) and no lead toward improving 19330 solvents to.reduce- zinc stearate solubility was indicated* DUP030001207 Zinc Stearate Solubility In Plasticizers 2% nag considered possible that triglyceride esters might react with either dissolved or undissolved zinc stearate in sealers* Investigation was made to determine whether a sealer tree of triglycerides would he more stable than 19360 containing nitrocellulose and blown castor oil. Sealers mad with nitrocellulose and dlbutyl phthalate were evaluated. Standard 19360 solvents and non-hydrocarbon solvents ifer in-* eluded in the study. This investigation did not indicate any marked superiority of dibutyl phthalate over blown castor oil in respect to sealer stability. However with conventional solvents there was a little evidence in favor of dibutyl phthalate. Where zinc stearate solubility was repressed with non-hydrocarbon solvents, there was no difference in f aror of dibutyl phthalate. ' Zinc Stearate and Water 2&ne stearate, acetone, and water 1*23.2 were mi^ed and the, mixture was air dried with the anticipation that, a maximum amount of water would be retained with, the soap. However* the treated sine stearate was no less stable than the untreated ziho stearate in 19360 stability tests. Two and four per cent of water were added to zinc stearate mill base MB-167, This resulted in bodying which required a 50 to 75# addition of solvents to reduce to normal mill base consistency. These mill bases yielded very inferior film properties in 193SO, although here the amount of water was only .1 and ,,2% on the film solids. Hill bases made with anhydrous and 95# ethyl alcohol yielded standard quality sealers. It Was considered of interest that the 95# ethyl alcohol added 3,6$ water to the grind, but this did not affect the sealer film properties. - Further work showed that 2% water added' to an aahyi drous ethyl alcohol mill base grind would not adversely affect adhesion and stability, while 2% added to a 'cutyl acetate grind would greatly body the mill base and seriously impair tiie adhesion of the sealer even when fresh. This deleterious effect is similar to that of aging 19360 at ordinary or elevated temperatures. It suggests that hydrophilic alcohol can repress the effect of water on the zinc stearate, whereas other relatively hydrophobic solvents do not. this suggested the followings Zinc stearate * water zinc hydroxide *' stearic acid Retention of water by alcohol would stabilize the zinc DUP030001208 -25- Analysis of mill base samples showed that addition of 2% water to increased the dissolved solids from to only l,lj of the total solids. This corresponds to an increase of ,04% to ,07$ of the sealer film solids* Additional tests indicated this figure to be under ,1& Since the die- ,, solved matter was so small and mostly stearic acid, it was not believed to account for the poor adhesion under discussion* Study of all Ihe Evidence available indicates that the effect of water in bodying the mill bases* where subsequent Impairment of the sealer is involved* is mainly a physical* surface " enomena* The zinc stearate does not appear to react or dissolve m the mill base* although this may happen sub sequently in the sealer* Small amounts of water added to the complete sealer do not have the same deleterious effect as when added to MB-167* This water is probably held % the lacquer solvents and thus does not promote solution of the zinc stearate* The improvement in stability obtained by the ehbstit'ftlon of alcohol for hydro carbons suggests some relationship which bears Some further investigation* tetij^^no^^earate An investigation was made of the possibility of coating zinc stearate particles with an insolubilizing substano that would not impair sanding* Four HB-167 grinds were prepared with additions ofI la) 1$ of a 10$ solution of polyvinyl alcohol 70-05 in water* Cb) p*8j of 0-650 ureafonaaldehyde Co) K7% of a 10$ solution of Vinyl!te VXEF in methyl ethyl ketone* Id) 4,7$ of a 10$ solution of Vinylite VMCH in methyl ethyl ketone* Sealers made with these mill bases sanded comparably to 19360* but no improvement in stability on aging could be demonstrated* Zinc stearate was mixed with 2. 5, 10* 25, 50, 100 and 200$ of RC-600 dissolved in acetone. Four percent each of cobalt nitrate and benzoin based on the RG-SSoo were added as a catalyst* These batches were treated as'follows* Excess solution was drained off, and the mixture was baked overnight at 130", to polymerize the RC-BOO* The resulting oake was ground in a ball mill tdth MB-167 type solvents for several ours to a satisfactory degree of dispersion. Experimental sealers tvere prepared with these respective mill bases and with MB-I67 fhw cmmpafison. The sealers were all aged three days at room temperature and at 130F* DUP030001209 .26 The treatment: of zinc stearate with polymerised RC-SOO slightly impairs its properties as a sanding aid due to the coarser ilarticXe size produced, The treated, sanding aids showedjno improvement in stability, although one or two sealers showed improved adhesion attributable to the larger particle size* . Attempts were maae to ooat zinc stearate particles with polymerized ureaformaldehyde to improve stability in sealers. Zinc stearate was misted with 20, 50 and XOtm of HO"721 end 10% of Cl?h catalyst based on the RCTM721. ^heee. batches were treated in a manner analogous to RC-SQO dee** oribed above and the results were very similar. The coating experiments may have been negative for the following reasons*. i>- .... 1* Polymerization may . not have been complete., . * . 2, The polymers may not have enveloped the zinc stearate particles. 3, The coatings may have been abraded off in grinding, 4, The coated particles may have been deduced in size on grinding, 5, The coating may have dissolved in the solvents* Any possible further work should he prefaced by a careful study of the surface r&DerptiOfc chargetori sties of zinc stearate. Zinc sfcesrat might be statAiised by the chemical or physical bonding to some additive. However this may be accompanied by impaired sanding properties^ ; Alcohol Sealers- Replacement of the hydreoarbone in X93&0 by ethyl alcohol resulted in improved package stability. The solvents were formulated to increase the aloohol content to a mazimiam and minimize larger solvent molecules by use of only enough ethyl acetate (H-136) to dissolve the ni tre cellulose, A ; further reduction in active solvents ms attempted' through the use of alcohol soluble nitrocellulose (0SP3C), This'was unsatisfactory because of excessive blushing due to the greater water content in the SSR3C and to its greater sensitivity to water. The ethyl acetate* ethyl alcohol (R-X36/R-X) formulations while offering improved stability had the related, bad features of poor sanding (rough film? and blushing, due to rapid evaporation rates. ^Wt DUP030001210 -27~ The effect on stability of higher boiling alcohols* esters* and ketones was determined* Those found nearly as good as ethyl alcohol and ethyl acetate were butyl aloohol (BLi.2)* aethyl isobutyl carbincl (H-48)* butyl acetate (H-6), amyl acetate (H-go)* aethyl ethyl ketone (B~35)e and methyl isobutyl ketone (B~44)b , It was found that excessive temporary blushing could not be eliminated in a high aloohol content sealer* but that the resistance to permanent blushing may be maintained by large proportions of high boiling solvents or the use of a retarder* la low proportion of a very high boiler). Formulas 226b*254iX-ahd 2265*-25hH are examples of sealers with excessive temporary blush but permanent blush equal, to 19380, isfifeggg- sm- .aa.,7i" B*75d H~4g ft* ->120 HS-lll HB-167 5,0 34,0 6,0 30,8 i0i. T3to?S 2a6&.g5H-g tv B.120 H-lll HB-167 11.7 M 4:1 U 2265-25^*H was set dp as formula J19000-X 10533 end recommended for field testing in Farlin Laboratory Release Letter Ho, 4-21, This sealer is considered to offer about a w% improvement in stability over 19380, It also reduces the appearance of'gray-poras through a leaching effect on dye type stains. The cost per gallon is slightly higher than 19380, Hie stability of 19380 may be improved about 60/2 by packaging the hydrocarbon diluent separately* to be added to the sealer at the time of application. This type is recommended under the codes J-19000-3&-10532 and J-3$00-X~10535 in Farlin Laboratory Release Letter 4-21, Ho differences in ingredient cost compared to 19380 are involved. The instability of I938O may be completely eliminated by packaging the zinc stearate mill base separately* to be added to the dear sealer at timeasf application. This sealer is recommended as y*49000~^10531 and J-Jffl~X~10534 in Farlin Laboratory Release Letter Ho,'aalj DUP030001211 6* 2a.no Stearate as an External Sanding Aid Study of the background of data developed in this project led to the theory that the.main purpose of a sanding aid is to act as a lubricant and prevent clogging of the sandpaper hy abraded particles of the sealer, This suggested the use of zinc stearate as a dry lubricant* preferably applied as a spray coating of MB-I67 on the sandpaper* ' f ' . V: , It was shown that a Characteristic curve exists . for certain sealer films when sanding rate is plotted against zinc stearate coating weight on the sandpaper* A conventional lacquer sealer without sanding aid sands with difficulty* causing rolling and clogging of ordinary untreated sandpaper* * with, for example, 19380 Clear, the rate of abrasion can be greatly In creased with a very light coating of zinc stearate on the sand paper* Further improvement In sanding quality,.including rate of abrasion, can be effected by adjusting the stearate coating to an optimum weight per unit area of sandpaper* , Zinc stearate in excess of the optimism range promotes easier sanding but re duces the rate of abrasion (See Graph 2)* It appears that as the abrasive becomes ..coarser, . the curve is displaced and becomes flatter, reflecting the greater cutting power of the coarser abrasive and, the diminished effect of excess zinc stearate on rate of abrasion, Am automotive primer-surf.aeer is eh example of a pigmented finish foemuiated for ease of sanding. Zinc stearate oated on sandpaper makes no improvement in abrasion rate since the finish does not roll or clog in sanding. However, a test on a red ffBueos showed that a pigmented lacquer with poor sand ing characteristics exhibits the same relation of eandabllity to zln etearate coated sandpaper as the 19360 Clear, It was also established that abrasives of silicon arbide, aluminum oxide, and flint yield to similar improvement In sanding efficiency by coating with zinc stearate* In the comparison of uncoated sandpaper on X$y&Q and coated sandpaper on 193SQ Clear, the latter method offers much greater ease of sandingwith a corfpsponding decrease in abrasion rate of 30v5 '5Hmt total work emended is estimated to be the same by. either* method. With very short drying oycles of less than thirty minutes, the coated sandpaper shows less clogging aad^a more favorable rate of abrasion than uncoated sandpaper. dl standard 19380, The following salts of steario acid were tested as sanding aid coatings on sandpaper? aluminum, barium, calcium, lead, magnesium, strohtiam, and zinc. Two grades of polythene* methylene distearamide, and. methylol stearamidewere also tested, All of these compounds imparted improved sanding quality, bat none excelled zinc stearate, stearamide and paraffin imparted ease of sanding but with excessive clogging. DUP030001212 DUP030001213  . Some worh was done investigating the coating off abrasives byohemieal reaction, A coating might ither polymerise on or react with an abrasive to form a chemical, bond. Such materials as dimethyl dl oblorosilane, ootadecytnohlorosilane, (silicones)* and butyl tltanat offered, little or no improvement in sanding quality* ' - , The great advantage of the new technique of coating abrasives Is of course that it provides excellent sanding while Seeping the sanding aid, put of the finish. Wo degrada tion of the finish by the presence of a sanding aid can occur. The sealer stability problem is also completely eliminated* This innovation should be thoroughly investigated for possible exploitation in industry* yFT&HCM ;| \' ' : Af;:.;! DUP030001214 -30* Ag Sealer 19160 (10-11-46) fg&l8g&$& HBb PX^TjOoCl?1* in H-l-G 5015> 4.9# 7a 9.$ 3224 s$ m . 3,,0 $ ik mlgals 7.60 lt>s 25*05, Vises 55-.65B 7 cP 25, Color * light Reduction - None mm P3E ' H-l4l< solid) Ov-eoi MLer 19155 (1^47) jfeJSS&fiSS' 4,|# P3U74oo I501I" 10'5 H-75-d 4,5 *47 MH-B1*21567 .:12*1 4>1 2g.g 1,7 _ ,* 7.67 ifce. _ , rise* $5-105* lOoap 25*0. Color ~ Medium Reduction ~ 30# mm mm m 10,, 5 10.0 10, f 10,2 s? 1,7 1,6 3*3 DUP030001215 Mill Grind Data , mil s ' H m/ssLlz (Gr,) 7.55 Ratio? 60/70/75* 2 Cycle? Gs&M 2 lire* s& pall -/I M : V DUP030001216 J-a9OO0~XlO5$L ''OTCO1' SEALER First Portion h L'I^ roue p x .760o )So * PX76io)5oi5 Saec-ounad .Portion HA.136 S~X2 H-2$h a-to R-29 B-l H-120 R3SL.H1 5*3 9*1 7*2 10,4- *6 12,7 11,1 19*6 6.2 1.2 JSSjBf wt/gal; 7.4-7 lbs. 25*0, moos 60-70" 7 cup 25*0. Flits F S If Color? Light Reductions 51 to E of J~MB~x.i0534 "by Types 193^0 Solids , Px 12; A-120 6*2 HBU111 . 1.2 Theo s Anal? 19*5# Ratio iOof> 5*0 . Xo0 ICG Class* Liquid Flash Point?- 20*"$Q*F,, Alcohol Usage Code H,,011 For information re Perlin Lab. . Release Letter Ho* 4-21 . PATENT KARKINGs-NOfl e e * 4> & # j-MB^X*1053h . SEALER SAUCING' AIC MBl6? 100*0# tft/gai? 7.h9 lb; 250o ICC Class? Liquid Flash Points 20^60 .PATENT jiARJtiNOs NONE For information re Parlln Lsfe. Release Letter No. 4-21 ::y-y'yy:MyM:y DUP030001217 ~33 J-19000-3UX0532 !,PUC0W SEALER First Portion 6.9* HB6 10.0 ^7600) ax 16,2 px -7610)50x5 fLls(i 609 Second Portion HA.136 11,9 9o4 tt-12. H-.222?- 13.5 1,1 TUI fl-120 6,9 6.1 Hffi.Ul KB~X67 1,5 7.6 . ' '"ioo;o$ Wt/gall ?,6l lbs, Q 35Go Fiscs 6o7o" 10 cap .25-*0,, Flits 100 mesh -4.re Colors light Redactions of J-3600-3C.10535 by volume Tyr>e 19360 Solids PX E-120 FQB-111 G-60X fheo? Anal j 16.2$ 6.1 1.5 1.6 ?7o 2$ .Ratio 10,0 5.0 S 1.1 ICG Class? Liouid Flash Point? 20~60Fo Alcohol Usage Code NoOil For Information re Periln Lab, Release .Letter No, ^21 PATRNI JIAHKIB? HONS - > C #. #. * * "* 4f 48- . . J-19000-X-10535 K.^7 H~29 61,6$ 56,2 IBSSt ICG Class1 Llould ,, Flash Point ? 20-60% PATENT MARKING-S NOWf 5RINNSR XJ 6,70 lbs, # 25 0., For information re Parlin Lab. Release Letter No, ^21 DUP030001218 J-19000-3&-I0533 vp>4^ PX,7600)2'5il 8C-7&0J56&5 sr B.120 SU11X m-167 . ,0% 3 1V7 5.0 16 ;g 3oQ 56,6, MA C/ * SOD Class Liquid Flash Point f &Lohol Usage CM Kto01X f,mjGOl! n?Mim tft/gal* 7.32 W>. 25 0, Tiscs 65-75" ? up 25*0. Flits Oent.srlf.ttge Colors Light Beduotlons fSone Tjpez 19360 Solids P% ' S-100 KBLU1 0v6oi l!heos Mals Eatlo .1.1.7^ 3.0.0"' 53. . 5a U. . '2u0Aft03^y' 33% For Information re Pa.iri.in Laboratory. Release Letter He. 4-si. J!PT*KCM ^:s m < DUP030001219 -35* ' Haw Material Codes ' E-l 23A Specially Denatured Alcohol Bld 2^-BDA/7$ water^ ethyl alcohol of dehydration HB-6 Butyl Acetate (90$) $.12 , Butyl alcohol BU29 Petroleum naphtha (ggVUte^O and A, P, 55 C) K~35 Methyl ethyl ketone EMJ4 Methyl ieohutyl ketone B-4-7 Toluene :, - &-69 Anhydrous isopropyl alcohol isopropyl alcohol (95$) 'H-Ht phthalate B-isO'. Pal''lfoxi)n $astor Oil $-12$ Butyl Stearate $-136 Ethyl Acetate B-lAl ' Mom linseed lacquer oil S-202 Hydrocarbon (13O-19O0, ana AeP0 2C) Butyl Oeiloeolt 0-601 G6og Zinc Stearate Ester Sum DUP030001220 Report Mo* 9S7 Dp, Davis, FI Mr, R.E, Tfeo&as* H Mr* J.W. lUff* Phila, Dp* G0D. Gpaves-RooE D-7O14,Ti0.1h i Dp* ;r*D* MoBumoy* t&liB* >Sn tufflft Mr* J.B. Baiiltt, mim. ) Mr* Matt Denning* Mllra. Mr* H*J, Haoa, mXm. Mp* F.B, Cochran* MiXm* Mr* J.D Shlels, Mm. Dp* L.G* Miss, Exp, Station* M2Lim. -Mr, A*K* Borlce, Ulraington Mp, B,I. Ffridfiy* FarXin j: DUP030001221 Distribution on last page 18 MIRSHIIL LABORATORY LIBRABIT t-.. a~ U*'* \ Ealft DU PONT PE NEMOURS & COMPANY FABRICS AND FINISHES DEPARTMENT CHEMICAL DIVISION PARLIN LABORATORY ftEFOENCE ? , w m ciiciifflii CLASS iUII(a) RESEARCH REPORT NO, 990 PROJECT 'NO. J*2023 SUBJECT? EVALUATION OF BCM CRG-gOO) AS A FINISH INGREDIENT DATE ISSUED? Jon 1$, 1950 PERIOD COVERED? JUNE g, 19^ TO APRIL % 19^9 PREVIOUS REPORTS QN SAME SUBJECTS PARLIN LAB.REPORT NO. 933 m MESSRS. O.L. HARGIS AND tfoK. MOFFETT NOTEBOOK NOS. 2201# 22619 22JB an d 2303 PREPARED BY? G,,CL MDRPmV CS^^ry APPROVED BX? N 29355 DUP030001223 TABLE OF G0HTSITS PA0E X Introduction 1 XX * Objectives xxx- Summary and Conclusions IV Action Taken V Patents vx EaPer&mental (A) Study of Topcoats Cl) Application (2) Plasticization (3) Processing {k) Shrinkage (5) Adhesion C6) Stability C7) Cost (6) Catalysts (9) Oold Crack Resistance CIO) Blue Haze 1 .1 2 2 3 3 3 5 6 9 10 10 13 13 XA lA <B) Study of the Components of the Undercoat System 16 Cl) Stain (2) Wash Coat 1$ 17 C3) Filler (A) Sealers 19 19 C5) lazing stains and Shading Lacquers CO) Competitive Thermosetting Finishes 20 20 vxx - &EWP&S IA) Rating Chart CB) Compositions of RC-SOO Finishes 21 21 22 <C) Recommended Built-up Systems PA DUP030001224 PARhIN LABORATORY REPORT NO. 990 PROJECT NO. J~202'5 SUBJECT2 EVALUATION OF BCM (RC-gOO) AS A FINISH INGREDIENT I. Introduction . This report covers the work done intett&ttently''from June l<?4d to date on the subject project* JPret'iottB work had Indicated that furniture.finishes with very attractive properties can he formulated with RC-&00* modified with nitrocellulose ana an alkyd resin. Based on the results of previous work three compositions at three levels of RC-SQO appeared t o rthy of fur ther study; viz.* ratios of RC-SOO/nltsrecelluloee/alkyd resin of 55/35/10* %A5/10 ana 35/55/10. ,i; * II. Objectives' Three main objectives have guided the direction of the work as. covered in this report. They area 1. To critically study the three compositions men tioned above* with a view to ultimately offering for field test* a furniture topcoat finish based on the preferred ratio of these ingredients over a suitable undercoat system. This Involved a study of not only the physical and chemical properties of the RC-dOO containing topcoats but also of each component in the finishing system* from the wood up* through stain* wash coat* filler* sealer* shading lacquer and/or glaze to the top coat! establishment of methods of "application* processing* dry ing times and baiting temperatures* as well as* catalyst/inhibitor ratios to give the maximum shelf life consistent with the lowest possible conversion temperature. 2. To evaluate modifiers for RC-dOO* other than those mentioned above* with a view to obtaining a more flexible and possibly a more thermoplastic film* at a lower cost. This In volved a study of other film formers in place of nitrocellulose and also of plasticizers other than alkyd resin. Considerable attention was given to the possibility of achieving internal plasticization by copolymerizing in situ of RC-dOQ with a mono-functional linear type monomer* suoh as the monomeric alkyl esters of acrylic and methaerylie acids and other similar materials. 3. To evaluate other thermosetting materials and any commercial finishes as they, appeared on the market from time to time* which might be competitive with RC-dOO. III. Summary and Conclusions The results of our evaluation of RC-SOO/nltroeellulose/alkyd resin compositions may be summarized as follows? DUP030001225 At the 55$ RCMSOO level, maximum- quality (!e, hardness, heat and solvent resistance, toughness, etc,) Is obtained, where as at the 35$ level, the reverse Is true. On the other hand, RC-goo is an expensive ingredient and the more there is present, the higher the cost will b of any given composition. Consequentijr# a formula containing 45$ RC-800 the solids was selected for field testing, as representing a good compromise between cost 2'flBd quail ty0 *... , . In'a`small scale field teat at the Bassett Superior and Lane Companies* it was demonstrated that the application properties of the 45/45/10 * ROgOo/WC/lftL255 formula are satis factory for conveyorized furniture finishing. As anticipated, the man hours required for processing were from one and one-half to tb-ee times greater than that reattired for furniture wPucow . or "PCpjX*, Besides high ingredient and processing costs, RC-&OO formulae are accompanied by Certain technical difficulties. However, before mating additional expenditures to resolve the latter, it seems desirable to determine whether the furniture industry is sufficiently interested in RC-gOO finishes to pay the extra money for the superior quality obtainable. Relative to the other objectives, no plasticizer superior to the alkyd .resin currently used was uncovered, Efforts to plasticize RG-800 internally were unsuccessful. Copolymer!2ation with low molecular weight polyesters such as ethylene, and propylene glycol maleate/adipates, resulted in incompatibility. The replacement of nitrocellulose with thickening agents (,g, methyl methacrylate, ethyl cellulose, and polyvinyl butyral, respectively), which are soluble in cheaper solvents than eaters and ketones, has not proven feasible to date because of compati bility limitations and the higher conversion temperature <lgoF, versus I305) required. Two materials which have appeared on the market, *Phanoplastrt and Bakelite9 a XF-17911, are not likely to offer any serious immediate competition to RC-000 because of applic ation difficulties and other limitations, 1 Parlin Laboratory Release Letter Ho, 439 recommends a field testing program aimed specifically at determining whether the furniture industry is sufficiently interested in the im proved quality obtainable with the RC-SOO finish to accept the increased costs. Such a program has been arranged by Industrial Sales and is in the process of being carried out, V - Patents Patent 2,498,091 issued on February 21, 1950, in the name of w,K, Moffett and assigned to duPont, covers the formula it is proposed to field test, as per Parlin Laboratory Release Letter Ho, 439, DUP030001226 F,, Experimental The experimental work undertaken to reach the three objectives listed in the introduction of this report* may b divided into the following two main sections for the purpose of this report!. (A) a study of the properties of the topcoat (b) a study of the individual components of the undercoat system. A. A Study of the Topcoats In the study of the properties of the topcoats select ed from the results of previous work, the following built-up system was employed* Stain* Wash Coats Fillers Sealers Topcoats Luxol - air dried 30 minutes 1366 - air dried 30 minutes 27-5017 -air dried 4 hours 1300 - air dried I hour Air dried 1/2 hour* baked 2 hrs. 130 '. Application of the three initially selected basic topcoats over this undercoat system indicated the followings Cl) An showed varying degress of pinholing, depend ing upon the porosity of the piece of wood over which they were applied. (2) The 35/55/10 and 45A5/IO formulations showed fairly good levelling and freedom from surface defects (other than pinholing). This was parti cularly true of the 35/55/10 composition. (3) The 55/55/10 composition showed poor levelling and varying amounts of ridging and cratering. Preliminary experiments showed, the pinholing to be due to .the porosity of the wood. A discussion of the experi mental work to correct this defect* will b found later on in this report under the topic of undercoat system. (I) Application Early experiments to produce a'flat HC-000 topooat had indicated that Santo cel 8 01 had a behefioial effect on the levelling of the RI3-S60. topcoat. Experiments were under taken to follow up this lead and to overcome the surface de fects occurring with the 55/55/10 formula. _ It was found that the incorporation <of 0antoeel WC0 up to 10/ on the solids completely eliminated th ridging and cratering of this com position* and also tended to reduce the pinholing. It was also found that this was true regardless of whether the Santooel "0 was ground 15 hours in a laboratory crook or l4k hours. The DUP030001227 only errpc m or xne longer* grinding cycle was to increase the gloss (Reference? Notebook Pages 2201-140* 153, 166, 173* 101? 2261-4-0), Other pigments and materials examined for this purpose were as follows? (a) Aluiainum stearate (G-517)? This soap also eliminated ridg ing and cratering but did riot appear to have any effect on the degree of pinholing and did not yield as transparent a film as Santooel "C*1 (Reference? Notebook page 2201-157) (h) Llndeq s Coated Silica $30? This pigment also tended to eliminate craterlhg `and' 'ringing but did not seem to have any effect on pinholing. The films also were somewhat gritty. It is believed that this could be overcome by better disper sion (Re? Notebook Page 2201-161). Co) Blanc Fixe (-30)1 No apparent effect on blistering* ridg ing or bratering was noted at the same pigment level as Santocel l*C" but if the amount was increased to three times that of Santocel ,,C*' on a volume basis* it too eliminated these surface defects (Re? Notebook pages 2201-166* 172), (d) Sllex Silica (17-31)? Rid not eliminate ridging and. crater ing when used on an equal weight basis with Santocel flCs (Re? Notebook Page 2201-166), (e) Temmstt Cold Bond Silica? Did not eliminate surface defects when used on m ernai weight; basis with Santocel MCW (Res Note book Page 2201-166) ' (f) RBR Dispersions8 RV-62? Reduced pinholing and eliminated most surface deFects' tjn'an equal weight basis with Santocel "CB but did not yield as good clarity (Res Notebook Page 2201-103), tg) Iron Hydroxide? Did not eliminate surface defects when used on an equal wSghtTasis as Santocel "CB (Res Notebook page 2201100). (h) Chromium Tetrahvdroxide? Did not eliminate surface defects When used on.;-an auai t/eight" oasis as Santocel B0,{ (Re? Notebook Page 2201-194-). ' From these results, it appeared that Santocel BC was effective either because of its high bulking value and large surface area with adsorbed air or that it adsorbed something from the film whloh causes the ridging and cratering. Experiments were therefore conducted in which Santocel "Cy Blanc Fixe* Nuohar, a low absorbent sllloa OHS-440-52* mioronized asbestine* Sllex silica and Tamms8 silica* were added DUP030001228 to the composition In excess* thoroughly mixed and then filtered out. The filtered compositions showed no improvement in ridging* cratering* etc, This indicated that the effect of Santocei 11 C,} is probably that of a bulging value due to its large surface area* Other materials examined as possible, aids in eliminate ing surface defects which wouia still permit the formulation pf a clear were* (1) calcium teats and (2) G,E Silicone 6106$e Calcium Octoate inhibited the conversion while the G.E. Silicone 8X069 had no beneficial effect on ridging and cratering, (Re Notebook Pages 2261-92, 2278-4, 2261-84* 227& 62 and 2303-50, 5^)0 One additional experiment was conducted using an RC~ 600 syrup (R Notebook Page 2248-136) prepared at the writer's request by Mr, Claus Victorias in place of RG-Soo monomer. While cratering ana ridging of a 65/25/IO composition were not eliminated entirely they were decreased noticeably (Res Note book Page 2261-92). Therefore, for the present, it was decided to con fine future work to a clear, at the 45A5/IO ratio' and a flat containing .10? Santoeel BGW on the solids at a 55/40/5 ratio. (2) Plastic!zation Both of these formulations show good resistance to cold checking. However, they, were felt to be more brittle than is desirable and attempts were mad to improve their flexibility by the use of (1) external plasticizers, and (2) internal plasticization through copolymer!zation. It was felt that the latter might also Increase the thermoplasticity of the film and therefore reduce the labor needed in processing, ' Earlier work in which a large number of plasticizers . were evaluate tad indicated that BL-255, a castor oil modified alkyd resin, was the most satisfactory plasticizer for RC-sfoo/ nitrocellulose. Most of our efforts were therefore confined to attempts at internal plasticization. The following materials were examined* (a) Butyl. Cello solve Methacrylate Monomer (BCMa) (l) Castings made in an attempt to copolymer!ze RC-000 with BCMa showed only a slight fle&blllzing action below 23p BCMa - above this percentage, cheesiness, rather than toughening, was apparent. The joint polymerization rate of BCMa/RC-g00 decreased as the amount of RC-800 decreased. , DUF030001229 (2) In films, only a slight plasticizing action could be noted* being more apparent with ethyl cellulose as the bodying agent than with nitrocellulose* (R@ notebook Pages 2201-104, 196, 198, 200, 212, 226* 2261-26, 34). (b) Normal Butyl Methacrylate Monomer (n-BMa) $ Cl) Castings made in an attempt to copolymer!ze n-BMa v. with EC-600 showed only a slight flexibilization, less than with BCMs and again cheesiness rather than toughness developed as the amount of n-BMa monomer was increased* h@ joint polymerization rate of n BMa and RC-BOG also decreased as the amount of nBMa Increased. (2) Films showed only a slight plasticization (Res Notebook Pages 2201-206, 224j 2261-36). () hauryl Methacrylate Monomer (Ufa) (1) Castings made in an attempt to copolymerize IMa. with RG-Soo showed only a slight flcxlbillzing action, less than with BCMa and again heesiness rather than toughness developed when the IMa ratio was increasedo Again the joint polymerization rate of LMa and RC-600 was decreased as the ratio of LMa increasedo (2) Films showed only a slight plasticization (Res Notebook Pages 2201-203, 222) (d) 2-Ethyl Hexyl Acrylate (2EBA? Castings made in an attempt to copolymerize 2-EHA with RC-600 showed only a slight flesibilization, developing cheesiness rather than toughness as the amount of 2-ERA to RC-600 was Increased (Res Notebook Pages 2201-260)o Mlylpxy. E^l_teylat^lX0.3Q-lgfe). (AOEAl <1) In thin films with r c -BOO it tires too volatile at 130 F, (2) By itself, when catalyzed with cobalt nitrate hexahydrate and benzoyl peroxide, in a testHtube it would not convert in 65 hours at $ft*Co C^es Notebook Page 2201-246),, DUP030001230 (*) 1,4 aiallyloxy-2~buten0 <1,4- DAB) (X) Did not? polymerize "en masse" when catalyzed with cobalt nitrate hexahy&rate and benzoyl peroxide in 60 hours at 4oC. Incompatible with RC-gOO at ratios higher than 50$* 1*4 PAB, At this ratio it aid not appear to speed up the Joint polymerization with RC$00. (2) In thin films it volatilize from the film at 130F. (RS Hotebook Pages 2201-116, 246, 250), <8> Piallyl phthalate and Plallyl Slyoolate (PAP & PAG) Pld not appear to convert in RC-SOO system at 130F. Acted more like a non-drying oil alkyd (Res Notebook Pages 2201-14$, 214, 215 > (P) o/4o Allyl Acrylate/Styrene (PRGR-7176) Incompatible with RC*$00. Converted with cobalt catalyst in 2 hours at 130F. to a non-tacky, soft film (Reg Notebook P=ges 2201-236, 24$). (l) 50/30 Aiiyioxy Ethyl Aorylate/Styrene (PBCP-?l6$) Incompatible with RC~$00 yielding a hard brittle film of low strength {Res Notebook Page 2201-191)* (3) PBCP-&1522 Ca straight glycerol allyl ether phthalate resin) {!) I-aaen used as a plasticizer in the RC-gOO system, tended to embrittle the film C2) By itself with cobalt catalyst, it converted in 16 hours 150F. to a fairly tough film, (Reg Notebook pages 2201-11$, and 2261-6$), (k) PRCP-92135 Ca glyoerol allyl ether phthalate modified dehydrated oastor oil alkyd) _____ _ . .....' <1) When used as a plasticizer in the RC-$00 system it tended to embrittle the film. (2) By itself with oobalt catalyst it converted in 16 hours 150F 0 to a soraexvhat soft but fairly tough film. (Re? Notebook pages 2201-11$ and 2261-6$) (l) Propylene Glycol Naleate/Adipate (PHA) <l) Incompatible with RC-$00 when polymerized "en masse" at ratios of 25/73 to 75/25. Addition of monomeric styrene to RC-SOO/PHA produced a compatible polymer but did not speed up conversion. Castings were exceptionally hard and flexible but tended-to embrittle on aging indicating a loss of unreaoted styrene monomer. DUP030001231 (2) Thin films of BC-goo/PHA/styrene in which nl trocellulose was used as the hodying agent showed ex cessive cratering and'crawling (BeS Noteboofc Pages 2201-25^ 256* 266| 2261-42)* Cm) Polyethylene Glycol Maleate/Agjpate (PG-MA) Incompatible with BCWSOO* When catalyzed with oohalt nitrate and benzoyl peroxide, converted to a cheesy film in 2 hours 130^, which crawled and cratered on both glass and wood, (n) Plootyl Bhthalate (POP) This`plasticizer was tried as a replacement for RL-255 but when freshly prepared, the highest ratio of BOP that could be used without spewing out was HC-gOO/PX/DOP 55/40/5< On agihg several months, 5 even $$&% Composition showed some spewing (Be 8 Notebook Page 2201-162)* O) Processing f; As can be seen from the attached properties chart (see page 2./) the RGgoo formulations are muoh more difficult to process; than either BDueoR or nDULUXn,, This was found to b true in the laboratory and was substantiated In a small-eoale field test conducted at the Bassett Superior and the Lane Companies,, The following studies were made to reduce the work required'In processing* (a) Methods 1* Bgy^Sanding - Ho improvement (Re 8 Notebook Page 2* Camphor in Octyl Alcohol as Lubricant No improveIIHtlHei Nbtlefedk Page 22/6-5/ H 3* Silicone Oil (G-o B<, 61069) in Film - No improvement Pei NotetKJoM Page 22'f&*>b2)'0 " " r"`" (b) .Two-Stage Conversion Experiments had indicated that the labor of pro cessing the BC-goo finishes can be materially reduced, approach ing that of Duco, if the finish is partially converted to an ,, ! stage, processed, and then the conversion completed to the B" stage* Conversion to the flA8 stage was accomplished by overnight drying at 70F* or a short force dry such as, one hour at 110F. However, unless a thermosetting sealer was used, objectionable-shrinkage occurred? (Res Notebook Pages 2261,90s 2276-12, 76, 20, gg and 90)* DUP030001232 (4) Shrt.nka&e As stated above* when the topcoat hale was split to allow easier processing, objectionable shrinkage occurred when the film was completely converted to the final or ,rBtt stage,, The follot&ng factors were investigated in .an effort to control shrinkage? {a) Rg-gpo Syrup in place of Monomer - Seine improvement IH^'lSSmnwage'"P*eV WtTeboblHFage "2276-4). (b) Measure of volume change of film at various stages of ^^^^|^T^mi^ecreiseTMW^f5Se7HSrWr^ocarre^" DtweenTairdrying overnight and 2 hours lSOe" This was not a large enough change to explain the de gree of shrinkage being encountered* Indications were that most of the shrinkage was due to the under* coat system (He? Notebook Page 2278-64). (e) Effect of Filler 1* Length of Filler Dry - No effect on shrinkage, (Re? Notebook Page 2278-65). 2, Flash Dry vs* .27*5000 line Filler - No effeot (Re? Notebook Page 2278-70) 3* Double Filling - No effeot (Re? Notebook Page 2278-70). 4. XJ.F. Modified 27-5000 line Filler - No eff ect , (R? Notebook page 22/8-72# 7^)* (d) Effect of Sealer v >>.- 1. 1366 vs. nylon sealer - Nylon sealer was poorer, (Re? Notebook page 2278-82), ... 2, RC-800/PVB Sealer - retired a high baking temper ature or overnight at 120F. but essentially . elimin. ated shrinkage (Be* Notebook P: ag 22278-84). 3a RC-80C/7MGH Sealer - Required a high baking temper ature or overnight at 120^Fo but minimised shrink* age. Re* Notebook Page 2278$6), 4. Increasing dry of 1366 and/or nylon sealer - No improvement (Re* Notebook Page No, 2278-98). 5, RC-SOO/VYCC Sealer - Reauired a high baking temper ature or overnight at. 120F, but practically eliminated shrinkage (Re? Notebook Page 2278-102). jlSPts,; DUP030001233 6, Nylon Seller pins catalyst to crosslink - No improve-* msnt when nylon plus citric or maleic acid as catalysts 1to04c),rosslink n ylon* were used {Res Notebook page 22J&-*' '' . ..V"' 7 Topcoat as Sealer - Eliminated shrinkage essentially one hundred percent (Res Notebook page 227&-X06), >. S The above :resulte indicated that in order to reduce shrink*, age*, which occurs when RC-000 finishes are processed to an f{A,s stage and subsequently converted to a "BW stage*, it is necessary to use a thenaosetting sealer or one unaffected by the solvents of th topcoat, The.; extra cost of baking the thermosetting sealer* however* tends to neutralize any savings gained in reducing the labor needed for processing by splitting the bake, (5) Adhesion On occasions poor adhe'lon of the RO-dOO topcoat to the 1366 Sealer was encountered. It liras investigated as follows* (a) Effect off Pry of 1366 None (Re* Notebook page 227&-I65) (b) Effect of Film Thickness of 1366 Adhesion increased sl^htl^v&th increased build (Re? Notebook Page (c) Effect of Moisture Condensed on Sealer {1366) SurfaceNon {Re* Notebook Page 2276-16$) (d) Effect of Poor Prying Conditions During Entire Finish** ing Schedule - Promotes poor adhesion (Res Notebook Page 227S~X76)o (0) Effect of Heavy Coats of Stain - Promotes poor adhesion* particularly if not thoroughly dried (Qes Notebook Page 2276-176). (6) Stability Initial tests indicated that the shelf life off the 45/45AO formula without catalyst* at room temperature* in partially full glass containers Is approximately on month and in partially full tin containers it is approximately 3 weeks, (Re* Notebook Page 226l>6$) The 55/4o/5 formula containing 10/ Santoe el 0 on the solids* compared to the 45/45/10. composition in partially full phenolic-lined containers* had a shelf life at room temperature* of 12+ months versus six weeks. A further study of containers (Res Notebook Page 2261-94) wcoitmhpsotsoitriaogne. at 105-110*F. indicated the following for the %/45/lG DUP030001234 Class Iron Tin 7 days 40 hours 4- days i Res Notebook Page 22?gg Class Aluminum Stainless Steel Galvanized Iron Tin 7 days 7 days 4 days 4 days 4 days 1 Re8 Notebook Page 1 2276-39 1 This indicated that the best commercial container is either tin'for small quantities or phenollc-lined for larger quantities* A. study was then made of other methods of splitting the formula and of inhibitors (stability at 105-1X0 (a) Split Packaging (BeS Notebook Page 2303-134) V.;<- System X Clear topcoat minus catalysts at 4l'i k# T0S, 1 week ' Catalyst solution (cobalt nitrate 4 benzoin)- ho apparent deterioration, : System XI RCU600 ~ 1 week , Clear topcoat minus RC-600 but with batalysts. present. Ho apparent deterioration. Catalyst solution - Ho apparent deterioration. System XIX RCg0D - 1 week Clear topcoat minus RGgoo but with catalysts present. Ho apparent deterioration. System V? . RO-SOO/PX at 57.2% T.8, 1 week ,n:. RL-255 + catalyst solution ** No apparent deterioration. System V * RC~gOO/RL-255 at B$9X% T,S. - 3 weeks PX + catalyst solution. No apparent deterior ation. System VX - System X with 10$ nitrobenzene on RG-gOO g -weeks, This indicates that nitrocellulose does not improve the stability of RC-gOO but that RJU255 does* ana that nitro benzene is a stabilizer for RC-goo, * DUP030001235 (b) Effect of Various Stablll aers Cl) 10% nitrobenzene on the RC-SOQ In 45/45/10 formula Increases the shelf life at 105F o, In tin, from one to fife weeks (Res Notebook page 2303-56) (2) 30% nltroethan on the BO-SOO In 45/45/10 formula inorea-ed the shelf life at 105^,, In tin, from one to two weeks, (Re* Notebook page 2303-62),, <3) toluene In an amount equal to that In the final formula, added to RC-800 increased the shelf life of RG-800 from 10 days to 12 weeks olas, In tin at 105^, CR@o Notebook Rage 2,303-64)o (4) 20% nitrobenzene or nltree thane on the RC-800 in a 45/10 combination of R<J-600 and RL-.255 at 45$ TS, in toluene increased the shelf life from . three weeks to twelve weeks plus in tin at 105F* (Re8 Notebook page 230>?0), (3) 30% Terpen B on the RO-SOO in RG-$00/BL~255 * 45/10 reduced to k-3% T.S. with toluene, increased the shelf life from three weeks to six weeks plus In tin at 105^. (Res Notebook page 2303-114)6 C6) From 60-170 ppm, anhydrous NH3 on the RCUBOC in creased the shelf life of RO-SO0), in tin, at 105*F,, from one week to four weeks plus (Res Notebook page 2303~12B}, () Relative Stability of Various Lots of RCUgQO Lot 22 (received 5/9/49) . 10 months at R.T, in phenolic-lined containers Lot 46 (received 10/5/49)- 1 month in R.T. in phenoliclined containers. All stability tests except those on the split package tests listed under (a) above, were run on lot 22. The split packaged systems listed under (a) above employed lot 46, From these results It appears that one of the best ways to increase the shelf life of the RC~$00 monomer Is to reduce it with all of the toluene in the formula and/or add Terpene Be The best split system for shipping to the customer is that of packaging the RC~gOO/RL=25 at 45f T,,s. in a toluene/Terpene B mixture In on container (partially full and phenolic lined) with the nitrocellulose, nitrocellulose solvents and the catalysts in the second package. Tin-lined containers can be used for batches of a gallon or less. DUP030001236 (7) Redaction in Cost; As a means of reducing the cost an investigation of thickening agents other than nitrocellulose and ones soluble in hydrocarbons, was undertaken* Three film formers meeting th requirements of solubility in low cost solvents were examined vis*, methyl methacrylate, ethyl cellulose and polyvinyl butyral. (a) Methyl Methacrylate Satisfactory conversion cannot be obtained in 2 hre at lJOF* with cobalt nitrate and benzoin as catalysts* Temper atures of 180-190 F, are required. Wo low cost third modifier, compatible with MMa and/or RC-800 was uncovered* Hence an appreciable decrease in cost at the k$% l&rel of R0-80O was not possible* (Res notebook Pages 2303*26 66, 94, 102, 108, 110, 116, 122, 124)* Cb) Ethyl Cellulose Satisfactory conversion is not obtained m 2 hours at 130with cobalt nitrate and benzoin as catalysts. Temper* atures of 186-190*. or a longer bake at 120F, than 2 hours, are required* No low cost third modifier compatible with ethyl cellulose and/or BOW was uncovered, preventing an appreciable decrease in cost at the 45#, level of RG-800. Also poor adhesion on aging* to I366 Sealer, was obtained. (Reft Notebook Pages 2303*72, 74, 80, 86, 92, 112, 118, 120 - 2261-24). Co) Polyvinyl Bat.vral Satisfactory conversion is not obtained in 2 hours at 130'S', with cobalt nitrate and benzoin as catalysts. Tempers atures of 180190F. are required (Res Notebook page 2303*68). An appreciable reduction in cost per gallon (approxi* aately 20 cents) is indicated in the R&g00/ra/f^2p5 45/45A0 formula, by changing the catalysts from cobalt nitrate and benzoin to 00bait naphthenate. An equivalent degree of conversion was ob tained at an equal metallic cobalt content (Res Notebook pages 2303-58, 84). (8.) Catalysts A high spot investigation of the catalyst reouire- ments for the BC-iooA^yRl^255 (45/45Ao! formula indicated8 (a) A minimum metallic cobalt content on the RC-800 of 0.2^ (Res Notebook page 2261-33) (b) Benzoyl Peroxide xdthout cobalt nitrate is in effective as a catalyst at 130Fo (Res Notebook Page 2278-18)* DUP030001237 Co) In the presence of cobalt nitrate and benzoin the RC*gOO/^/KL*255 fomula can be converted in one hour under UV (weatherometer) equivalent to 2 hrs, at 130F, (Res Notebook Page 227S-36K (9) Cold Craok Realbtanse Cbld orach data indioate that the check resistance of the formulae, either at 115/45/10 or 55/40/5 plus 10/S Santooel HQne is very good even when 1/6" nitrocotton is used,, However when extra thick films are applied and for the highest quality fini eh, lA" nitrecot ton must be used0 This reduces the total solids at spraying viscosity for these formulae from to approximately 26~27^(Res Notebook Page 23G3-S8}, (10) Blue Haze From time to time various difficulties in the applic ation and formulation of the HC-SOQ finishes have arisen and have been overcome by one means or another. One difficulty that has occurred on only a few panels and for which we do not have an explanation but only a theory, is the occurrence of a blue haze. While we have not been able to reproduce this condition we be lieve it to be an incompatibility which arises as the panel ages. It tail occur in the dark, but heat or light accelerates It, Th following experiments trere-, undertaken to deter* min the cause of the difficulty, with negative results, They are being recorded here for reference purposes only, ' All systems were exposed either to carbon arc or to ultra violet, (a) Effect of Catalysts? None, cobalt nitrate plus, benzoyl peroxide,'.ooh'^tlSfrate plus benzoin and straight cobalt nitrate ~ baked 2 hrs, at 250F, - No blue haze, (b) Same as (a) except bakea 2 hrs, 130?. Wasre no catalyst was employed finish was baked 2 hrs, @ 250F, No blue haze, (%s Notebook page 227&-155), Co) Type of.Stain* No stain, NPh, Lux! and oil stain - no mu haze " W* Notebook Page 227^153), / ; * -'i- , (d) Effect of (a) Sealers None, 1366, 1366 * stain, nylon primer (He? Notebook Page 227&-163). Cb) Stains Normal and 5 times normal amount, NoTiaze in either case (Res Notebook page 227&-163), DUP030001238 -15*' <) ^fect of light anfl heavy ooata sealer 1*566 - No blue ^ ~u~~' it) Effect; of 1366 vs. RC-800/ethvl cellulose trash coat in a system employing a tEsCToset'trrig sealer - 'No . blue haze (net Notebook page 2278-167). (S) Sffect_pf mplstare opL.sealers 1366, 1366 * water, no sealer, and water on filler surface before 1360 wag applied - No blue haze (Re* Notebook page 2276-log},, (h) Ci> Effect of amount of stain and dry of ss tains No stain, HorSaTTOW.T'TCmea normal tCTB"j;aSr^rled 1/2 ftpur* and 5 times normal VSJJ469 force dried 2 hrs at 130 V.t aoh under 1366 and J-1300-X-IO362, < 1366 made with' PVB of our own manufacture)- No blue haze (Re Notebook Page No. 2278-178). U) Effect of Adding Film Formers to the Stain? Polyvinyl SutyraX and et^r oeirulo^e 'W"`Blue' haze (Res Note book page 2278-180). <k) Effect of Slow Solvents In 13661 Butyl laotate, ethyl Xactat e, CeXTosoive' and uelS^BoXve acetate ~ No blue hz (Res Notebook page 2276-163}. U) gomparlson of Oil Type, NFL and Luxol Stains Applied id nomajHandinextraheavy" coats - No blue haze <Bs Notebook Page 2278-163). Cm) Influence of Each Element in System with normal and 5 times^normal amount or stain - No Blue haze (Res Note book page 2276-16^-). Cm) Mash Coatg 5^.TeS0 RC-600/E,C. up to 25% RC-gOO/E.C. and X^fTs. RG-600/N.C. ~ No blue haze (Res Notebook page 227g-190)o <o) ip) - * "Ua *"* <q> Effect of D^^of^aah Coat - No blue haze (Res Note- <*) Effect of high aloohol 1366 va. So^lsiuehaze^^TTIoteBo" page Cellosolve DUP030001239 -16- <> Effect of 1166 vs* 1366 5$ ethyl butyral Over isorraal and heavy stain '& m bluehazeT^iT Notebook page 230>7> . (t> Effect of speeding up the dry of the system - Wo blue haze' (Mel" "notebook page 2303-idl <) Effect of normal and extra heavy_wet coats of topcoat - fToTHTua" haze."TMH s'. "WotebooiTpage ' . <r) Effect of^l366 In Topcoat Wo blue haze (Ret Notebook (w) Effect of stain in topcoat (NFL and Luxol) ifo blue Hizr^WT^o?eKoEpaie^03^22^---- <x) Effect of temperature of conversion of topooat ~ Ib^blue haze CKef'TTbteBoo^'^ge' ty) Effect of age of topcoats before application - No blue HazeTiwrmeesHrpigs^^--------- i%) Effect of excess phosphoric add In filler - No blue Haze ' '{'fie;..^oWoofpi|e~?3o3^6Tr^^-------~ * , (as) Effect of inhibitor In filler - No blue haze (Res Notebook page- ' (bb) Benzaldehyde as a Contaminant - No blue haze {B$ Nbte= Hbok page 23o3-f>2) " (eo) Effect of Urn as a Contaminant - No blue haze (ReS Nc^eW^ page.230^6577 B` -Study of the Components of the tla&erooat System Th recommended undercoat system for the preferred topooats consists of the followings a) Stain b) Nash coat c) Filler Sealer 14 aiding u^r] wbere nee4ea %y syetPia may vary from consisting of just sealer to containing all of the above components. Considering them Individually and in the order listed above* each was in vestigated as followss (1) Stain (a) Over close grain woods such as birch and maplee oil type stain has been found to be satisfactory if drlted '-> overnight or Its equivalent (ae: Notebook page 227&~62) - 'V, DUP030001240 (b) Over porous woods such as walnut os? mahogany, either a ttLuxolfl dye stain or an NFL may be used, However, over mahogany with a 27-5000 line filler, gray pores and poor adhesion may develop. If the stain Is applied In heavy coats and la not thoroughly dried (Eel Notebook pages 226l-7$|| 227$1$4 sad 230>*K>), (2) %ah Coat ' , Early in the work on this project considerable pin- holing ms encountered. We were able to show that this was due in the main to the porosity of the wood. To & less extent, how well the wood was filled and how thoroughly the' filler was dried were also shown to have some effect* (Res Notebook Peg 2201-142}o - A study of various means for sealing the wood was therefore undertaken and the following materials examined as possible wash coatsS (a) RK-B760 Furniture DULUX at 12% T.B. When baked 2-1/2 hours at 130F. was definitely superior to 1366 from the standpoint of reducing plnhollng, but it Impaired adhesion (R8 Notebook Page 2201--10$}, lb) 13016 Penetrating Primer at 12# T. Ss P22o0o1r-e1r0$th)e,n 1366 for plnhollng (Ret Notebook page (e) RC-gOO/PX/RL-gSq ($3/33/10) at 12# f,,8. Some Improvement In plnhollng but not as good as WK-5760* Adhesion was poorer than with 1366, (d) Shellac No Improvement in minimizing plnhollng. (Res Note-, book page 2201-10$), (e) Vlnyllte VHCH at T,S, No reduction in plnhollng. Impaired adhesion (Res Notebook Page 2201-139), <r) R0-$OQ at 12% f. 3, Ho decrease in plnhollng. impaired adhesion, (Res . Notebook page 2201-139). DUP030001241 (g) Cellulose Apetate (CA-loS) Slight reduction InpInhoXing. Adhesion was weakened. (Rs Notebook page 2201-139). (h) Ngeaformaldehyde (RCL.721 12% T. 8.) No Improvement In eliminating plnhollng. Adhesion was weakened. (Res Notebook page 2201-139). (1) Phenol Formaldehyde (Xf-17911) Prevented Rd-800 topcoats from converting. (Res Note book page 2201-139). U) 19-580 Sealer at %% T.8. No improvement In eliminating plnhollng. Adhesion weakened. (Re* Notebook page 2201-14-5T. (k) Animal Sin No improvement In eliminating plnhollng. (R* Notebook page 2201-192) (1) Styrenated Alkvds (Styresol teo and 44oo) Styreeol 4-250 showed no redaction in plnhollng. Styresoi WOO shows a slight redaction in plnhollng,, (He* Note^., book page 2161-14). . .' Cm) Butyl Titanate Vv, - , Some Improvement in minimizing plmtaoli&g: was obtained accompanied by indications of Impaired. adhesion (B Notebook page 2281-58). <n) RO-gQO/Ethyl Cellulose This combination gave a very definite redaction in plnhollngg essentially eliminating it and with no sacrifice in scratch resistance. A 50/50 ratio was considered optimum. Medium ethoxy ethyl cellulose was found to b more foolproof from the standpoint of conversion with RG-goo (Re* Notebook pages 22012^5* 252^ 2$2% 2261-48 and 2303-76). DUP030001242 -1% (3) Filler Because earlier work Indicated that under-dried 563line filler was more apt to cause cratering and ridging than 27-5000 line filler, the latter was selected for use in our preferred undercoat system. A detailed study of the drying conditions necessary for 27-5000 line filler showed A hours 130", to he optimum, if the RCMSoo/ethyl cellulose wash coat were used (Be* Notebook pages 2201-133, 156), At this hake, 563*11110 filler also is fairly satis factory, It tends to puff somewhat more hut is definitely superior in freedom from gray pores in a mahogany system with 1366 as the sealer (Re? Notebook page 2303-40), This is true over an NFL stain, hut does not hpla over a "Luxol8 stain. (4) Sealers Earlier work had indicated that 1366 Penetrating Primer was definitely superior to 19380 type sealer in an RC~gOO system and that a sealer was necessary to provide maximum ad hesion, hold out, and foolproofness against surface defects, such as ridging and crawling. Since 19380 definitely impaired the scratch resistance of the system, 1366 was selected as the sealer in the initial work. A further sealer study was made Cl) to improve adhesion and minimise gray pores, and (2) to reduce the shrinkage in the system, work covering the latter has already been discussed under the heading BShrinkageH in a previous section of this report (see page 13). Th follotdng study of various sealers was made to improve adhesion. is) Nylon flAl m~m This film former was found to give improved ad hesion, more "life1* and better pore definition with a minimum of gray pores0 Over porous woods such as walnut and mahogany* It yielded the greatest improvement in adhesion when used as a wash coat as well as a sealer. However, it had two defeotas Cl) high cost, and (2) the built up system exhibited objection able shrinkage (Res Notebook pages 2261-44, 74 & 22?g-24-g)a (b) Miscellaneous Sealers Various other sealers were evaluated, such as iOp polyvinyl acetate dissolved in butyl acetate, 4$ polyvinyl butyral (G-64-9) in butyl aoetate/alcohol, 10% low molecular weight, solution prooess, polyvinyl butyral (Re* Notebook page 2249-95), 13016 Penetrating Primer mid a penetrating primer based on low molecular weight, solution process polyvinyl butyral. All were either poorer for adhesion or no better for adhesion than 1366 (Re Notebook page 2278-16). DUP030001243 20- Based on these results, 1366 was selected as the best sealer except perhaps on maple where the shrinkage of Nylon $AlBgo Is not of importance* (5) blazing Stains and Shading lacquers Two basic types of glazing stains were evaluated for possible use in the RC~gQO systems viz8 one based upon a drying oil vehicle and coded in the 307 line and the other formulated with castor oil ana carrying a 2$ line code* The latter was found to be definitely better from the standpoint of adhesion than the former (Net Notebook Bag 2303-M-2), The 266 line shading lacouers based on blends of 259 line "Dueo* were found to be satisfactory for use in the RC-SOO system (Res Notebook page 23Q3~4k8 *t-6>* (C) Oompetitive Thermosetting Finishes Two oompetitive finishes ware evaluated versus the RC-SOO system. They were the finishes offered under the trade name wPhenoplastM and Bakelite Corporation s. X7-17911* The latter lea phenolforffialdefcyde type which Bakelite offered to manufacturers of wood finishes* Our evaluation indicated that ^Phenolplast" when properly cured, and over a suitable primer, provided a tough, mar, solvent resistant finish equal to our proposed RC-gOO type finish (^5/45/10K Although it sprayed or brushed fairly well, it tends to crater and crawl in the same manner as some of the earlier RC-800 type formulas containing high amounts of RC-goo* Also its,dolor retention was inferior to our RCgoo finish* Vm From fits general appearance and physical character- istics, HPhnolplastis apparently very similar to XF-179H, Bakelite a low temperature baking finish for wood,- The latter is characterized by the same advantages and disadvantages* It is not believed that `'Phenolplast^ as now formulated is a serious immediate competitor in the field in which we contemplate exploiting RO-SOO finishes (Ri Notebook pages 227&23, 25 thru -333* _____ _ DUP030001244 APPENDIX TENTATIVE BATING- CHART FURNITURE FINISHING SYSTEMS WITH BCWgQQ TOPCOAT Properties 1. Cola Check 2* durability 3. . Humidity 4, Water Resistance $. Alcohol Resistance 60 Solvent Resistance 7* Heat Resistance (212P} 6. Scratch Heal stance 9. Mar Resistance 10* Resistance to discoloration 11* Print Resistance 12o Clarity 13. * Sanding L 14. Rubbing 15. High Polish 16* Shrinkage 17* Spraying Solids Type A romx 6 c* 3 9 9 5 '9 $ 6 9 &-X/2 6-1/2 @ 5 5 7 Type H "51160 9 9 10 6 5-1/2 0 4 g 6 6-1/2 6 6-1/2 7-1/2 6 6-1/2 g 20 RC..600 Clear 10 10 10 10 10 10 10 9-1/2 9 6 104* 9 4 5 6*1/29 32^ DUP030001245 Compositions of the clear and flat RC-600 topcoats and the ethyl cellulose/RG-600 wesh coat are as follows at spraying viscosity? Ca) Clear (45/45/10) ?3U?555 (Ary) H-X-d H~X HB--6 HA-136 B-12 HL-255 &G-4121 KG-4122 SE-4120 h u 47 Theo? To So 32. 7/8 Gal. Height .* 6.01# Via. 7 cap 45-55 x 4.3o 7.70 9.00 16.10 6.4o 2.50 5.?o O.45 P. 14. 1 ,1/6 seo. Hercules Hitreeo tton) alcohol of drhydratlon) 'ethyl alcohol) iiWbutyl acetate) ! ethyl acetate) n-butyl alcohol) 50$ castor oil alkyfi) cobalt nitrate hexahydrate) benzoin) |HC-600 monomer) 'toluene) PX-7555 (dry) B-l-d E~X HB-6 HA-136 H12 HL-255 I KG-4-121 KG4l22 mil Base KS-4120 EU4j Then* T.S. Gal. Height Vise. 7 P Sheen *mil Base IST HB--6 HA-I36 Bl-255 G-222 H47 ^Clear Base 1/6 seo* Hercules Hi tsro cotton) alcohol of dehydration) I ethyl alcohol) n-butyl acetate) Cethyl acetate) fn-butyl alcohol) |50$ castor oil alkyd) (cobalt ni trate hexahydrate) (benzoin) (see below) |RC-600 monomer) (toluene) DUP030001246 ^Clear Base X. -2> PX.7555 <di?y) Bl-d H-4? HB-6 HA-136 B-12' t-) Wash Coat C Thermo setting) *8-4123 KH4l20 E47 B~X2 5-5*3 121 5*0$ 5*0 (7 ope* raed. ethoxy Ethooel) (ECLSO0 monomer) (ethyl alcohol) C toluene) Cn-fcatyl alcohol) (xylene) Cmethyl ethyl ketone) Coohalt nitrate hexahy&rate) DUP030001247 ' 1 -I'-.f ' 1 ' ' ...... ...... " " '............ RECOMMENDED SYSTEMS FOR USING Rg~gOQ TOPCOATS Operation Open Grain Wood {Mahogany & Walnut) Close Grain Wood (Maple and Birch lo Stain Dry NFL for walnut and Luxol for mahogany to minimize gray porea* 15 to 30 minutes at room temperature,, 307 line (oil type) 16 hr80 or longer at room temperatures of 60F. or higher 20 Mash Coat Dry 1366 for good ouality None veneer JRK-A10336 for poorer quality grades of veneer 1366 should be flashed 1 hour J-RK-X-10336, If baited simultaneously with the filler, should be flashed one hour. Otherwise bake J-RK-X.10336 for 2, hours or longer at 130-l4oF. 3c Filler 27-5000 line None or 27-5000 line Dry Filler, or filler plus wash Filler If used to be coat, are baited 4 hra. at baked 4 hrs. at 130-11(0 F0 130-140F,, 4. Sealer 1366 1366 Dry 3and One hour at room temper ature (6o'*\ or higher) Scuff lightly with #360 paper One hour at room temperature (60'F. or higher) Scuff lightly with #360 paper. 5c Glaze Dry Optional. 28 line as represented by the com position of F*2g-R~555674. Flash off solvents which should not require more than 1 hour Optional. 28 line as represented by the composition of r*8SR"55674. Flash off solvents which should not require more than 1 hour. DUP030001248 Operation 6. Shading Laoaaer Pry 7 S8riJ3a2i Bake ~25* Open Grain Wbok (mhDzmy & Walnut) Close Grain Wood Optional,, 266 line- Optional. 266 line 1 hour at room temper 1 hour at room temper* atop (60F,,or higher) attire (6oF, or higher; For maximum quality apply 2 ooatse flashing 30 minutes between ooats and 60 minutes prion to hav> _ing. 2 hours at 130~l4o&S\ and 35$ R0H. Cannot he air dried. For maximum quality apply 2 ooats, flash ing 30 minutes hetween coats and 60 minutes prior to baking. 2 hrs. I30-l4oF0 and 25$ R,H. Cannot he air dried. COM 8MON DUP030001249 stsssasa f ^ Br* ,R.B. Pavla* Flint Thomas* Newburgh Mr. J, W. XUff* - -PhiXa, Lab, t Br0 Go Do Graves* Boom D-TOl^MLln. )Zn Pr* J.P. MeBurneyy Wilm. Mr, J.B. Bullitt-* Wilts. )tum Sir, Matt Penning* Wilts. Mr, H.J. Haon* tom. Mr, P.B. Cochran* $&lm. Hr* J,P, Shiela, Wilm. Pr. PoGo Wise* Exp .Station* Wilm, Mr* A0K, Bar&e* rcLlm. Mr. H.L, Friday* Parlln REPORT MO, 975 DUP030001250