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Fixation on last page 18 MARSHAlt LABORATORY LIBRARY C- E0Ia DU FONT PE NEMOURS & COMPANY FABRICS AND FINISHES DEPARTMENT CHEMICAL DIVISION REFERENCE- CPff Mm F@l CllCiifflOi PARIAN LABORATORY CLASS AXXa) RESEARCH REPOST NO, 990 PROJECT NOo J-2023 SUBJECT? EVALUATION OF BCM (RC-SOO) AS A FINISH INGREDIENT DATE ISSUED? June 15, 1950 PERIOD COVERED t JUNE 5* 19*^ TO APRIL 19^9 PREVIOUS REPORTS QN SAME SUBJECTS PARLXN LAB, REPORT NO* 933 BY MESSRS. O.L, HARGIS AND M, MOFFETT NOTEBOOK NOS0 2201, 2261, 22J6 an d 2303 PREPARED BY? CoG. APPROVED BY? CoJ 8 c TABLE OF CONTESTS PAGE % ~ Introduction II * Objectives XII- Summary and Conclusions IV V- VI Action Taken Patents Experimental (A) Study of Topcoats Cl) Application <2) Plasticization (3) Processing (4) Shrinkage C5) Adhesion .16) Stability (1) Cost {$) Catalysts (9) Cold Crack Besi stance CIO) Blue Haze .% 1 1 2 2 3 3 3 5 * 9 10 10 13 13 14 1* m Study of the Components of the Undercoat System 16 Cl) Stain (2) Wash Coat 3) Filler (4) Sealers 16 17 19 19 (5) Glazing Stains and Shading Lacquers CO Competitive Thermosetting Finishes 20 20 21 W Rating Chart (B) Compositions of RC-600 Finishes 21 22 (0) Recommended Built-up Systems 24 4* DUP030001224 PARLXN LABORATORY REPORT NO, 990 PROJECT N0,, J-202'5 SUBJECTS I. 'irn EVALUATION OF BCM (RC-SOO) AS A FINISH INGREDIENT . . . . . . . . . . . . . . . . . . . .. ......... ..............., ,, r.T . ,,n.. ................ ............. .. ......... Tn.. " ... n Wn m* Z. Introduction . V * This report covers the w p St done intermittently from June > 19^ to date on the subject project,, Previous work had Indicated that furniture.finishes with very attractive properties can be formulated with RC-gOO, modified with nitrocellulose and an alkyd resin. Based on the results of previous work three compositions at three levels of RC$QO appeared worthy of fur ther study; viz,* ratios of RC-SOO/nltrocellulOBe/alkyd resin of 55/35/10, %A5/10 ana 95/55/IO, i; - II, Objectives Three main objectives have guided the direction of the work as. covered in this report They area X, 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-gOO containing topqoats but also of each component in the finishing system, from the wood up, through staip, wash coat, filler, sealer, shading lacquer and/or glaze to the top coat! establishment of methods of "application, processing, dry ing times and baking 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 RG-&OO, 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 nltrooellulose and also of plasticizers other than alkyd resin. Considerable attention was given to the possibility of achieving internal plasticization by copolymer!zing Bin situ*35 *of RC-gOO with a mono-functional linear type monomer, suoh as the monomeric alkyl esters of acrylic and methaoryli adds 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 RG-4SOO, SIX. Summary and Conclusions The results of our evaluation of RC-gOO/nitroeellulose/alkyd resin compositions may be summarized as follows? DUP030001225 At the 55$ RC-800 level* maximum: quality Ci,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-800 Is an expensive ingredient and the more there is present* the higher the cost t'/ill be of any given composition. Consequent- - ly* a formula containing 45$ RC-gOO on the solids was selected for* field testing* as representing a good compromise between 00st 2'aad quality* r .? . ili a'small scale field test at the Bassett Superior and Lane Companies, it was demonstrated that the application properties of the 45/45/10 m R0.$0O/NC/EtL<255 formula are satis factory for conveyorized furniture finishing. As anticipated* the man hours reauired for processing were from one and one-half to tfcree times greater than that reouired for furniture "Duoo" . or *W]tfJXa, * . ' % Besides high ingredient and processing costs* RC-&00 formulae ar accompanied by pertain technical difficulties. However* before making additional expenditures to resolve the latter* it seems desirable' to determine Aether the furniture industry is sufficiently interested in RC-800 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 RCMSOO internally were unsuccessful. Copolymeriz ation with low molecular weight polyesters suoh 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 esters and ketones* has not proven feasible to date because of compati bility limitations and the higher conversion temperature <180F, versus 130F) required. Two materials which have appeared on the market* "Phenoplast1* and Bakelite9 s X7-17911* are not likely to offer any serious immediate competition to RC-gOO because of applic ation difficulties and other limitations, Parlln Laboratory Release Letter Ho, 4-39 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-800 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 Parlln Laboratory Release Letter No, 439, DUP030001226 VI,, Experimental The experimental work undertaken to reach the three objectives listed in the introduction of this report, may be divided into the fallowing two main sections for the purpose of this reports (A) a study of the properties of the topcoat (b) a study of the individuaX 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 t-rark, the fallowing built-up system was employed? Topcoat? Air dried 1/2 hour, baked 2 hrs, 130** Application of the three initially selected basic topcoats over this undercoat system indicated the following? (1) An showed varying degrees of pinhollng, depend ing upon the porosity of the piece of wood over whloh they were applied* (2) The 35/55/10 and 45/45/IO formulations showed fairly good levelling and freedom from surface defects (other than pinhollng). 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 pinhollng to b due to the porosity of the wood, A discussion of the experi ment al work to correct this defect^ will b& found later on in this report under the topi of undercoat system, (1) Application had indioat _ . __ , _____ _______________ __ the levelling of the RC-Soo. topcoat. Experiments were under taken to follow up this lead and to overcome the surface de fects occurring with the 55/35/10 formula, w It was found that the incorporation nif Bantoeel *0* up to 1QJ& on the solids completely eliminated t&@'ridging and orataring of this com position, and also tended to reduce the pinhollng. It liras also found that this was true regardless of whether the Santooe: "G* was ground 15 hours in a laboratory crook or 144 hours. The DUP030001227 only errpo t ; or tn longer grinding cycle was to increase the gloss (References Notebook Pages 2201~l4o 153* loo* 173* -181'$ 2261-4-0), Other pigments and materials examined for this purpose were as followsi (a) Aluminum Stearate (G-217)* This soap also eliminated ridg ing and cratering" but 'did not appear to have any effect on the degree of pinholing and aid not yield as transparent a film as Santooel BCtt (References Notebook pge 2201-157) (h) Linde6 s Coated Silica #30s This pigment also tended to eliminate 'cratering and ridging hut did not seem to have any effect on pinholing. The films also were somewhat gritty. It is believed that this could be otercome by better dispejv sion (Res Notebook Page 2201-161), (c) Blanc Fixe (ff-30)i No apparent effect on blistering^ ridg ing or cratering was noted at the same pigment level as Santooel ttC* but if the amount was increased to three times that of Santooel "Cw on a volume basis, it too eliminated these surface defects (Res Notebook pages 2201-166, 172), (d) Sllex Silica (V7-`!l)s Did not eliminate ridging and. craterlog wSeh used on an eoual weight basis with Santooel ttCB (Res Notebook Page 2201-166), (e) Tamms Gold Bond Silicas Did not eliminate surface defects . when used'"'^"'"'^" 'eauai1 weight;1 basis with Santooel "'O3 (Res Notebo ole Page 2201-166), (f) RBH Dispersions RV-62S Reduced pinholing and eliminated moa^surface 'defects"on' an equal weight basis with Santooel "CB bat did not yield as good clarity (Res Notebook Page 2201-163), .(g) Iron Hydroxide; Did not eliminate surface defects when used on an equaL 'iMghFTSasis as Santooel "C,! (Res Notebook page 2201IgS), (h) Chromium Tetrahydroxldes Did not eliminate surface defects When ttse'd'oh.i-air'eauai" weight basis as Santooel "C15 (Res Notebook Page 2201-194), Prom these results, it appeared that Santooel WG. was effective either because of its high bulking value and large surface area with adsorbed air or that it adsorbed something from the film which causes the ridging and oratering. Experiments were therefore conducted in which Santooel nG\ Blanc Fixe, Nuohar, a low absorbent silioa GRS-44o-52 mioronized asbestine, Sllex silica and Tamms 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 Santocel ``C'1 is probably that of a bulbing velue due to its large surface area* Other materials examined as possible aids in eliminate ing surface defects which would still permit the formulation of a clear were! Cl) calcium ootoate and (2) GE. Silicone &L069, Calcium Octoate inhibited the conversion x-rhile the G,E0 Silicone $1069 had no beneficial effect on ridging and cratering, (Res Notebook Pages 2261-92, 2278-4-, 2261-84, 22?8- 62 and 2303-50, 5h), One additional experiment was conducted using an RC 800 syrup (Re* Notebook Page 2248-136) prepared at the writer's request by Mr, Claus Victories in place of R0-8OO monomer, While cratering and ridging of a 65/25/IO composition were not eliminated entirely they were decreased noticeably (Res Note book Page 2261-92), * Therefore, for the present, it was decided to con fine future work to a clear, at the 4-5/45/10 ratio' and a flat containing 10$ Santocel ,!Ctt on the solids at a $5/40/5 ratio, (2) Plasticization Both of these formulations show good resistance to cold checking. However, they, were felt to be more brittle than is desirable and attempts were made to improve their flexibility by the use of (1) external plasticizers, and (2) internal plasticization through copolymerization. It was felt that the latter might also increase the thermoplasticity of the film , and therefore reduce the labor needed in processing, j, ' Earlier work In which a large number f plasticizers were evaluatedlsaS. Indicated that RL-255e a castor oil modified alkyd resin, was the most satisfactory plasticizer for RC-800/ nitrocellulose. Most of our efforts were therefore confined to attempts at internal plasticization. - The following materials were examined? la) Butyl Cello golye Methacrylate Monomer (BCMa) (1) Castings made in an attempt to copolymerise RC-goo with BCMa showed only a slight flxiMlizing action blow 25$ BCMa - above this percentage, cheealness, rather than toughening, was apparent. The joint polymerization rate of BCMa/RGg00 decreased as the amount of RC-800 decreased, , DUP030001229 (2) In films* only a slight plasticizing action could he noted* "being more apparent x-jith ethyl cellulose as the bodying agent than with nitrocellulose, (Re* Notebook Pages 2201-104* 196* 196* 200* 212* 226* 2261-26* 34), (b) Normal Butyl Methacrylate Monomer (n-BMa)s {1) Castings made in an attempt to eopolyiaerlze n-BMa with RC-600 showed only a slight flexibilization* less than With BCMa and again cheesiness rather than toughness developed as the amount of n-BMa monomer was increased, The joint polymerization rate of n BMa and RC-600 also decreased as the amount of n-BMa increased. (2) Films showed only a slight plasticization ('Res Notebook Pages 2201-206, 224j 2261-36), (c) hauryl Methacrylate Monomer (Ufa) (1) Castings made in an attempt to copolymerize LMa with RC-600 showed only a slight flexibili zing action* less than with BCMa and again heeslnees rather than toughness developed when the IMa ratio was Increased, Again the joint polymerization rate of LMa and RC-600 was decreased as the ratio of Ufa increased. (2) Films showed only a slight plasticization (Res Notebook Pages 2201-203* 222), (d) 2-Ethvl Hexyl Acrylate (2ERA) Castings made in an attempt to copolymer!ze H-EHA with RC-Soo showed only a slight flesibiXization* developing cheesiness rather than toughness as the amount of 2-EHA to RC-60Q was increased (Reg Notebook Pages 2201-260). () Allyloxy Ethyl Acrylate (7090-164) (AOEA) (1) In thin films with RC-600 it tira.s too volatile at I30 F (2) By itself* when catalyzed with oobalt nitrate hexahydrate and benzoyl peroxide* in a testHtube it would not convert in 65 hours at (*Vj Notebook Page 2201-246). DUP030001230 -7if) 1,4 aiallyloxy-2-butehe <1.4 DAB) Cl) Did not polymerize "en masse" when catalyzed with cobalt nitrate hexahydrate and benzoyl peroxide in 66 hours at 4oC. Incompatible with RC-80O at ratios higher than 50?a* 1*4 DAB, At this ratio it did not appear to speed up the Joint polymerization with RC-600. (2) In thin films It volatilizes from the film at I30*Fo (Rea Notebook Pages 2201-116, 246, 250), Cg) Dlallyl phthalate and Dlallyl Glvoolate (DAP & DAO) Did not appear to convert in RC~60Q system at 130*', Acted more like a non-drying oil alkyd Ces Notebook Pages 2201-146, 214, 215) (b) 60/40 Allyl Acrylate/Styrene (PRCR-7176) Incompatible with HC-600. Converted with cobalt catalyst in 2 hours at 130F,, to a non-tacky, soft film (Res Notebook P?ges 2201-236, 248). (l) 50/30 Allyloxy Ethyl Acrylate/styrene (PRCP-7166) Incompatible with RC-600 yielding a hard brittle film of low strength (Res Notebook Page 2201-191), (3) PRQP~61522 (a straight glycerol allyl ether phthalate resin) (.1) When used as a plasticizer in the RC-600 system, tended to embrittle the film, (2) By itself with oobalt catalyst, it converted in 16 hours 150P, to a fairly tough film, (Res Notbook pages 2201-116, and 2261-66) (k) PROP-92135 (a glycerol allyl ether phthalate modified dehydrated pastor oil alkyd) _____ , , . . r_.' (1) When used as a plasticizer in the RC-600 system it tended to embrittle the film, (2) By Itself with oobalt catalyst it converted in 16 hours 150to a somewhat soft but fairly tough film. (Res Notebook pages 2201-116 and 2261-66} (l) Propylene GjLyeol Maleate/Adlpate (PMA) Cl) Incompatible with RC-600 when polymerized "en masse" at ratios of 25/75. to 75/25, Addition of monomeric styrene to RO-SOO/PMA 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 onreacted styrene monomer. DUP030001231 < 2> Thin films of RC60Q/P2IA/etyrene in which nitrocellulose was used as the bodying agent showed ex cessive cratering and crawling (Re 8 Notebook Pages 2201-254-, 256* 26j 2261-4-2). Cm) Polyethylene Glycol Maleate/Aaimte (PG-MA) Incompatible with RC-600. When catalyzed with cobalt nitrate and benzoyl peroxide, converted to a cheesy film In 2 hours 130, which crawled and cratered on both glass and wood. (n) Ploctyl Phthalate (POP) This plasticizer was tried as a replacement for HU-255 but when freshly prepared, the highest ratio of POP that coaid be used without spewing out was RC-gOO/PX/pQP * 55/40/5 On agiisg several months, even ttii% composition showed some spewing (Mes Notebook Page 220ll62), O) Crocessing As can be seen from the attached properties hart (see page &<?) the RCMSOO formulations are much more difficult to process; than either HDucos or KDULUXn. This was found to be true in the laboratory and was substantiated in a small-scale field test conducted at the Bassett Superior and the Lane Companies,, The following studies were made to reduce the work red&lred in processing. (a) . Methods 1* Sgy^Sanding - Mo improvement (Eel Notebook Page 2. Camphor In Octyl Alcohol as Lubricant - Ho improve.lent (HeV HotefakPage 227.6-57}',, 3<> Silicon_ Oil ..(.go E*,, 61069? in Film - Ho improvement fins Notebook Page 27S62). (b) .Two-Stage Conversion Experiments had indicated that the labor of pro cessing the RC-600 finishes can be materially reduced, approach ing that of HDucott, if the finish is partially converted to an *A* stage, processed, and then the conversion completed to the B" stage* Conversion to ths "A** stage was accomplished by overnight drying at ?0F* or a short force dry such as, one hour at 110F,, However, unless a thermosetting sealer was used, objectionable shrinkage occurred* (Res Notebook Pages 2261,90j 2276-12, 76, 60, m and 90)* . DUP030001232 -9(4) Shrinkage As stated above, when the topcoat bait was spilt to allow easier processing, objectionable shrinkage occurred when the film was completely converted to the final or ,fB" stage* The follotdng factors were investigated in an effort to contra shrinkage? (a) Some improvement (b) Measure of volume change of film at various ages of owreriSon Borne "decrease""in volume. 0.l^ocorredTM between "air-drying overnight and 2 hoars 180F,, 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 (Res Notebook Page 2278-64)* (c) Effect of Filler 1* Length of Filler Dry ~ No effect on shrinkage* (Res Notebook Page 2278-65). 2* Flash Dry vs* 27*5000 line Filler - No effect (Res Notebook Page 2278-70) 3. Double Filling * No effect (Res Notebook Page 2278-70). 4* D.F. Modified 27-5000 line Filler - No effect (es Notebook page 227&-72, 7^)9 '(d) Effect of Sealer 1, 1366 vs. nylon sealer - Nylon sealer was poorer* (Res Notebook page 2278-82) 2, RG-600/PVB Sealer - reouired a high baking temper ature or overnight at 120F. but essentially . eliminated shrinkage (Res Notebook Pag 2278-84). '3 RC-80C/7MGH Sealer - Required a high baking temper; - ature or overnight at 120*F. but minimized shrink age. Res Notebook Page 2278-96). 4. Increasing dry of 1366 and/or nylon sealer - No improvement (Res Notebook Page No. 2278-98). 5. RC-800/ViCG Sealer - Required a high baking temper ature or overnight at. 120F, but practically eliminated shrinkage (Res Notebook Page 2278-102). DUP030001233 6* Nylon Sealer plus catalyst to crosslink - No improve ment when nylon plus citric or maleic acid as catalysts to crosslink nylon# were used (Res Notebook page 22JS- 104), ,- ' To Topcoat as Sealer - Eliminated shrinkage essentially on hundred percent (Res Notebook page 2278-106) \ *v The above results indicated that in order to reduce shrink age# which occurs when RC-&00 finishes are processed to an #AB stage and subsequently concerted to a ffBw stage# it is necessary to use a theraraset ting sealer or one unaffected by the solvents of the topcoat# She,; extra cost of baiting 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 adheibn of the RC-800 topcoat to the 1366 Sealer was encountered# It was investigated as follows* 9 (a) Effect of. Dry of 1366 - None (ReS Notebook page 2278-165) (b) Effect of Film Thickness of 1366 - Adhesion increased slightlyvdth increased build (Res Notebook Rage (c) Effect of Moisture Condensed on Sealer (1366) SurfaceNone (Re* Notebook Page 2276-168) (d) Effect of Poor Drying Conditions During Entire Finish lag Schedule - Promotes poor adhesion (Re* Notebook Page 2276-176)o (&) Effect of Heavy Coats of Stain - Promotes poor adhesion# particularly if not thoroughly dried (Qes Notebook Page 2276-178)o (6) Stability Initial tests indicated that the shelf life of the 45/45/10 formula x^ithout catalyst# at room temper?tore# in partially full glass containers is approximately on month and in partially full tin containers it Is approximately 3 weeks* ,(**? Notebook Page 2261-68) o The 55/40/5 formula containing 10$ Santocel 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 12s** months versus six weeks. A further study of containers (Res Notebook Page 2261-94-) with storage at 105110F. indicated the following for the 45/45/10 eompoeition. DUP030001234  Glass Iron Tin 7 Says 40 hours 4- days Res Notebook Page 2Z1M Glass Aluminum Stainless Steel Galvanized Iron Tin 7 days 7 days 4 days 4 days 4 days Rea Notebook Page 227S-39 This indicated that the best commercial container Is either tin for small quantities or phenolic-lined, for larger quantities*. A. study was then made of other methods of splitting the fomula and of inhibitors (stability at lO^llo^F), (a) Split Packaging (Re8 Notebook Page 230>134) V/;" System I - Clear topcoat minus catalysts at 41'i 4^ TVS. .1 week ' Catalyst solution (cobalt nitrate 4 benzoin)- No apparent deterioration. System II * RC-gOO - 1 week Clear topcoat minus RC-gOO but with Catalysts, present. No apparent deterioration. Catalyst, solution - No apparent deterioration. Gystem III - RC-gOD ** 1 week Clear topcoat minus RG-goo but with catalysts present. No apparent deterioration. System XV - RC~goo/PX at 57.2$ T.S, - 1 week . RL-255 4 catalyst solution - No apparent deterioration. System V - RC~gOO/RL"255 at g?,l$ T,S. ~ 3 weeks PX * catalyst solution. No apparent deterior ation. System VI System X with 10$ nitrobenzene on RC-SOO g weeks. This indicates that nitrocellulose does not improve the stability of RC-gOO but that RL-255 does, and that nitro benzene is a stabilizer for RC-Soo, DUP030001235 (b) Effect of Various Stabilizers CD 10$ nitrobenzene on the RC-600 In 45/45/10 formula Increased the shelf life at 105F,, in tin, from one to five weeks (Re* Notebook page 2303*56), (2) 50$ nitroethane on the RO-gOO In 45/45/10 formula increased the shelf life at 105^,* In tin, from one to two weeks, (Res Notebook page 2303*62), <3) Toluene In an amount equal to that in the final formula, added to RC-SOO increased the shelf life of RG-600 from 10 days to 12 weeks wlas. In tin at 105^0 Notebook Page 2303*64), (4) 20$ nitrobenzene or nitroethane on the RC-600 In a 45/iO combination of RC-600 and RL-255 at 45$ TS, In toluene Increased the shelf Ilfe from . three weeks to twelve weeks plus In tin at 105?** (Res Notebook page 2303-?0), ^ ii ' (5) 30$ Terpen B on the Ro-goo in R<4=gOO/RL~255 45/10 reduced to 45$ TS, with toluene, increased the shelf life from three weeks to six weeks plus In tin at 105F, (Res Notebook page 2303-114}, (6) From 60-170 ppm, anhydrous NH3 on the RC^SOC in creased the shelf life of RO-gOO, In tin, at 105F. from one week to four weeks plus (Res Notebook page 230>12g), () Relative Stability of Various hots of RCL.60Q Lot 22 (received 5/9/49) * 10 months at RT, In phenolic-lined containers Lot 46 (received 10/5/49)- 1 month in R,T, in phenoliclined containers, iU.1 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-600 monomer is to reduce It with all of the toluene in the formula and/or add Terpene B, The best split system for shipping to the customer Is that of packaging the RC4>6oo/RL255 at 45$ T, s. in a toIaene/Terpene B mixture in one container (partially full and phenolic lined) with the nitrocellulose, nitrocellulose solvents and the catalysts In the second package. Tin-lined containers can b used for batches of a gallon or less. DUP030001236 (7) Reduction In Coat; 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 eannot be obtained in 2 hrs, at 130F, with cobalt nitrate and benzoin as catalysts# Temper** atures of 16019O*F, are required. No low cost third modifier, compatible with MMa and/or RCU60Q was uncovered# Hence an appreciable decrease In cost at the 45$ Isrel of RC-600 was not possible, (Re* Notebook Pages 230>26, 66, 94, 102, log, 110, 116, 122, 124),, (b) Ethyl Cellulose Satisfactory conversion is not obtained in 2 hours at X30F, with cobalt nitrate and benzoin as catalysts. Temperatures of X60-190Fo or a longer bake at 120F, than 2 hours, are required. No low cost third modifier compatible with ethyl cellulose and/or BGM was uncovered, preventing an appreciable decrease In cost at the 45$, level of RC-goo. Also poor adhesion on aging, to 1366 Sealer, was obtained, (Re* Notebook Pages 2303*72* 74, 60, 66, 92, 112, 116, 120 - 2261-24), <) Satisfactory conversion is not obtained in 2 hours at 130F, with cobalt nitrate and benzoin as catalysts# Temper* atures of 160*190F,, are required (Res Notebook page 2303~6S), An appreciable reduction in coat per gallon (approsimately 20 cents) Is indicated in the R0600/^C<mL255 %/45/XO formula, by changing the catalysts from cobalt nitrate and benzoin to cobalt naphthenate. An equivalent degree of conversion was ob tained at an equal metallic cobalt content (Res Notebook pages 2303-56, 64), (6) Catalysts A high investigation^ of the catalyst reouire* ments for the RS-8OO/PX/RL.255 (45/45/lof formula indicated* (a) A minimum metallic cobalt content on the RC-600 of 0,2$ (Re# Notebook page 2261-33) (b) Benzoyl Peroxide tdthout cobalt nitrate is in effective as a catalyst at 130F, (Res Notebook Page 2276-16)o DUP030001237 (o) In the presence of cobalt nitrate and benzoin the RC-gQO/PX/KL~255 formula can be converted. In one hour under UY (veatherometer) bivalent to 2 hrs. at 130F, (Re? Notebook Page 227S-36K (9) Cold Crack Resistance Cold orach data indicate that the check resistance of the BO-0CO/P%/raU255 formulae, either at W45/IO or 55/W5 plus 10J8 Santooel *f0H, is very good even when 1/6" nitrocotton Is used. However when extra thick films are applied and for the highest quality finish* 1/4" nltrocotton must be used0 This reduces the total solids at spraying viscosity for these formulae from J2% to approximately 2627/& (Res Notebook Page 2303-68)0 (10) Blue Haze From time to time various difficulties In the applic ation and formulation of the HC-80Q 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 tfblch arises as the panel ages, Xt will occur in the dark, but heat or light accelerates it. The following experiments were undertaken to deter mine the cause of the difficulty, with negative results. They are being recorded here for reference purposes only,' Ail systems were exposed either to carbon arc or to ultra violet, (a) Effect of Catalysts? None, cobalt nitrate plus.benzoyl peroxide, oobaStlSTrate plus benzoin and straight cobalt nitrate - baked 2 hrs, at 250F, No blue haze, (b) Same as (a) except bakea 2 hrs, 130F, Where no catalyst was employed finish was baked 2 hrs, @ 250F, No blue haze, (R Notebook page 2276-155), Co) Type of Stains No stain, NF&, Luxol and oil stain - no blue haze l ues* Notebook Page 2278-153) ,, .'i Cd) Effect of (a) Sealer? None, 1366, 1366 stain, nylon primer (Reg Notebook Page 2276-163). Cb) Stains Normal and 5 times normal amount, n o haze in either case (Res Notebook page 2276-163). DUP030001238 -X5-' () Effect of light and heavy ooais sealer 1*566 - Ho blue ttflze (iles foteixsote pagfi '"`2'SfCT557* 4'"" if) Effect; ooff_1_166 vs. RC-gOO/ethvyl cellulose was!h coat In a systemmeSIoH^atneCTosetHng^eaIeF~^Sa*~' blue haze (Eel Notebook page 2276-167). <S) Effect of mol stupe oh..sealers 1366, 1366 4- water, no sealer, and water on filler surface before 1366 was applied No blue haze (Ess Notebook page 2276-168) (h) at .130%,5* &mh under 1366 and J-X3OC-5C10362, (1366 made with FW of our own manufacture!- No blue haze (Res Notebook Page No. 2278-178). U1 Formers to the gtaln* Polyvinyl ce, ose - N6 blue'haze (Res Notebook page 227r88--318o (k) Effgot of Slow Solvents In 1366s Butyl lactate, ethyl lactate, Oelloiolv'e'1 and '0Hos5Tve acetate - No blue haze (Bes Notebook page 2278-183). (l) imparl eon of Oil Type, NFL and Loxol Stains - Applied in formal ana In Stra Eeaw""Boats' wo 'blue haz <H8 Notebook Page 22?8-l83). Cm) Influence of Each Element in System with normal and 5 times normal amotint of stain - No Blue haz (Rs Note book page 2276-l8k). <n) Mash Coatt 5# T.S. RG-800/E.C. up to 25# RC-SOO/E.C. ind X5#fT8o RG-600/N.C. - No blue haz (Res Notebook page 2276-190). ,<o) <P> -1J- ~ H bl"S ^ (<l) Effect of Pry of Nash Coat No blue haze (Res NoteboWpag^T30P3T: <*) Effect of high aleohol 1366 vs. StTblue haze lRi"^oteKoS' p age. DUP030001239 (s) Effect of 1166 vs. 1366 + 50 ethyl butyral - Over nomal and heavy stain a Ho blue haze (Rei Notebook page 2303-7). (t) Effect of speeding up the dry of the system - No blu Haze (Res'`Notebook page 2303-10)...... (u) Effect of normal and extra heavy_wet goats of topcoat ^'biWliazVr 'WeT'I^TebooS: page. 23o3"iw . . (v) Effect of^l366 in Topcoat No blue haze (Ret Notebook (w) Effect of a tain In topcoat (NFL and Xwcol) Ifp blue haze.' '(ReT NpV^ooFpage 2303-20) (x) Effect of temperature of oonversicmof topcoat ~ No Wue haze (Rei Notebook page' 2303-22$ (y) Effect of age of topcoats before application - No blue SsTzC"'TKeratebook pages '2303-2k> 28) ''r "!' " (z) Effect of excess phosphoric acid In filler - No bln Sazin!^iiFWteW6Kpage^3o^36Tr^ (aa) Effect of inhibitor In filler - No blue haze - (Res rairorpag'',23^^w:"... * ' '%, (bb) Benzaldehydg as a Contaminant - No blue haze (Rr Note BboW page 2303-52 i (co) Effect of Urea as a Contaminant - No blue haze (Ra$ WS^Smok. page 2303^0)T B. .Study of the Components of the iladercioat System Th recommended undercoat system for the preferred top coats consists of.the followings (a) Stain (b) Nash coat (e) Filler Sealer e Glazing Stain Glazing Lacoaer needed -%y systPffi 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 maple, oil type stain has been found to be satisfactory if drlted overnight or its equivalent (Be: Notebook page 2878-62) ..: . . DUP030001240 :< ' f=-. ' (b) Over porous woods such as walnut or mahogany, either a ttlxola dye stain os* an NFh 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 eoats and is not thoroughly dried (Res Hotebook pages 2261-78I 22?0-10^ and 230>lK>), (2) ash Coat I _. , Early in thl work on this project considerable pinholing was encountered* W were able to show that this was due in the main to the porosity of the wood* To a less extent, how well the wood was filled and how thoroughly the' filler was dried were also shorn to have some effect, (Res notebook Page 2201Xk2h A study of various means for sealing the wood was therefore undertaken and the following materials examined as possible wadi coats* (a) BR~576o Furniture "PHLOX" at 12# T,S When baked 2-1/2 hours at 130F,, was definitely superior to 1366 from the standpoint of reducing pinhollng, but it impaired adhesion (Re* Notebook Page 2201-100} (b) 13016 Penetrating Primer at 12# T, S* Poorer than 1366 for pinhollng (Res Notebook page 2201--100)* (c) RC-0OO/PX/RL-253 (63/30/10) at IS# T.S. Some improvement in pinhollng but not as good as R&=>5760 Adhesion was poorer than with 1366* Id) Shellac No improvement in minimising pinhollng, (He* Note-, book page 2201-100) (e? Vlnylite VMCH at &% T0 S9 No reduction la pinhollng* Impaired adhesion (Hs Notebook Page 2201-139), <f) RC-000 at 12# t. 8, U decrease In pinhollng, Impaired adhesion, (Res Notebook page 2201-139), DUP030001241 Cg) Cellulose Acetate (OA^lOgU Slight reduction in plnhollng, Adhesion was weakened, (Re* Notebook page 2201-139). <h) Ureaformaldehyde (BCU721 9 12% T..S,) No Improvement in eliminating plnhollng. Adhesion was weakened, (Res Notebook page 2201-139), (i) Phenol Formaldehyde (Xff-l?911) Prevented R0-600 topcoats from converting. (Res Note book page 2201-1395, <45 19360 Sealer at gg T,,a. No improvement in eliminating plnhollng. Adhesion weakened*, (Re* Notebook page 2201-1457, (k) Animal Glue No Improvement in eliminating plnhollng, (Ret Notebook page 2201-192) (l) Styrenated Alkvds (Styreaol 4250 and 44oo) Styreeol 4250 showed no reduction in plnhollng. Styresoi 4400 shows a slight reduction in pinholing. (Res Note-.. book page 2l6l-14), (... (m) Butyl Tltanate V/ Some improvement In minimizing pis^holing was obtained accompanied by indications of iijppired 'adhesion (Res Notebook page 2261-56), <) RC-Soo/Sthyl Cellulose fhis combination gave a very definite reduction in pinholing* 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 RO-gOO (Res Notebook pages 2201245* 252* 2621 2261-1$ and 2303-76), DUP030001242 -19* C3) Filler Because earlier work Indicated that under-dried 563 line 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 4 hours 130ftF* t be optimum, If the RCMoo/ethyi cellulose wash coat were used (Res Notebook pages 2201-133, 1565, At this bake, 563-1113,0 filler also is fairly satis factory. It tends to puff somewhat more but la definitely superior in freedom from gray pores In a mahogany system with 1366 as the sealer {Res notebook page 2303-40;, This Is true over an NFL stain, but does not hold over a aLu35ol stain, (4-5 Sealers Earlier work had indicated that 1366 Penetrating Primer was definitely superior to 19380 type sealer in an R0-600 system and that a sealer was necessary to provide maximum ad hesion, hold out, and fooiproofness against surface defects, such as ridging and crawling. Since 19380 definitely Impaired the scratch resistance of the system, 1366 w&s selected as the sealer in the Initial work. A further sealer study was made Cl) to improve adhesion ana minimize gray pores, and (2) to reduce the shrinkage in the system. Work covering the latter has already been dlsougsed under the heading "Shrinkagein a previous section of this report {see page Ij), The following study of various sealers was made to Improve adhesion, (&) Nylon 8A1 PV~gQ BUs film former was found to give Improved ad* hesion, more "life1* and better pore definition with a minimum of gray pores. Over porous woods such as walnut ana mahogany It yielded the greatest improvement in adhesion whan used as a wash coat as well as a sealer. However, It had two defects? Cl) high cost, and (2) the built up system exhibited objection able shrinkage {Re* Notebook pages 2261-44, j4 & 2276-24-98), (b) Miscellaneous Sealers Various other sealers were evaluated, such as 10/5 polyvinyl acetate dissolved in butyl acetate, 4# polyvinyl butyral (0-649) in butyl acetate/alcohol, 10# low molecular weight, solution process, polyvinyl butyral (Re* Notebook page 2249*95 5# 13016 Penetrating Primer and 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 <Rs Notebook page 2276-16), DUP030001243 *20- Based on these results# 1366 was selected as the best sealer except perhaps on staple where the shrinkage of Nylon 8AlDgo is not of importane, (5) glazing Stains and Shading Lacquers Two basic types of glazing stains were evaluated for possible use In the RC-800 system} vizs one based upon a drying oil vehicle and coded in the JOJ line and the other formulated with castor oil and carrying a 28 line code. The latter was found to be definitely 'tetter from the standpoint of adhesion than the former (Res Notebook Pag 2303-42}, The 266 line shading lacouers based on blends of 259 line "Dueo" ware found to be satisfactory for use in the RCU800 system (Res Notebook page 2303-44, 46), (0) Competitive Thermosetting Finishes Two competitive finishes wpre evaluated versus the RC-SOO system. They were the finishes offered under the trade name "RhenoplastH and Bakelite Corporation8 s 3C?1?911 The latter is a phenoXformal&ehyde type which Bakelite offered to manufacturers of wood finishes. Our evaluation indicated that ^Phenolplast8 when properly cured, and over a suitable primer, provided a tough, roar, solvent resistant finish equal to our proposed ECS-800 type finish (45/45/10), Although it sprayed or brushed fairly well, it tends to crater and orawl in the same manner as some of the earlier RG-800 type formulas containing high amounts of RGU800, Also itsjtolor retention was inferior to our RC-800 finish, i From fits general appearance and physical character istics, ^Phenolplast8 is apparently very similar to XV-17911, Bakelite0 s low temperature baking finish for wood,- The latter is characterized by the same advantages and disadvantages. It is not believed that 8PhenoXpXast:! as now formulated is a serious immediate competitor in the field in which we contemplate exploiting RG-800 finishes (Res Notebook pages 2278-23, 25 thru -33), * mrntmA . DUP030001244 appen d ix TENTATIVE RATING CHART FURNITURE FINISHING SYSTEMS WITH R&.goo TOPCOAT Properties le Cola Cheek 2. Durability 3. . Haaaaity 4-, Wat er Resistance 5* Alcohol Resistance 6. Solvent Resistance 7, Heat Resistance (212F) 8 ,, Scratch Heel s tanoe $o Mar Heslstanoe 10, Resistance to Discoloration 11, Print Resistance 12, Clarity 13, Sanding L Ik. Rt*hfcing 15. High Polish 16, Shrinkage 17? Spraying Solids Type A mihUX* 6; 3 9 9 3 9 $ $ 9 8-1/2 6-1/2 8 5 5 7 Type H "Dueo* 9 9 10 8 5*1/2 0 4 8 6 8*1/2 8 8-1/2 7*1/2 8 8-1/2 8 26$ R0.800 Clear 10 10 10 10 10 10 10 9-1/2 9 6 ic mj * 9 4 5 8--1/2 9 32$ DUP030001245 <=23= (B) Compositions of the clear and flat RC-000 topcoats and tlie ethyl cel1ulose/RQk000 wash coat are as follows at spraying viscosity? Ca) Clear (45/45/10) PX-7555 (dry) H-X-& B~X HUMS HA-136 B-12 b l -255 KJ-4121 IE-4120 -e ~47 14.30# 7.70 9.00 10.10 0.40 2.50 5.40 0.45 0.45 l4.io 19J0 (1/0 sec, Hercules Hltroco tton) 'alcohol of drhydratlon) ethyl alcohol) n^butyl acetate) ethyl acetate) n-butyl alcohol) 50# oaetor oil alkyd) .cobalt nitrate hexahydrate) "benzoin) RC--000 monomer) (toluene) 3?heo? To So 32.1% Sal. Weight 0.01# TlsOo 7 oup m 45-55* frat. (45/lgAo) HC-7555 <4iy> B-X--d B-l HB-6 HA-136 H12 10-4X22 Mill Base KS-4X20 EU47 1/0 sec, Hercules Nitrocotton) alcohol of dehydration) ethyl aloohol) n-butyl acetate) ethyl acetate) n-hutyl alcohol) 50$> castor oil alkyd) ,cobalt trate hexahydrate) 'benzoin) see below) .RC-000 monomer) toluene) Theo* To S# Sal. Weight Vise. 7 up Sheen Hill Base --Ti=r~ H-47 HB-6 HA-136 Rl-255 0-222 E.47 Clear Base DUP030001246 ^Olear Baaa X.. PX-7555 (dxy) E.ia H-% .HA-136 H~12 350% t) flash Goat (Thermosetting! m4l23 K04X2O 1? H-12 E5S3 121 50# 5oO (7 ops* raed, ethoxy Ethooel) (HCUSOO monomer) (ethyl alcohol) C toluene) (nbatyl alcohol) (xylene) Cmethyl ethyl hetone) Coohalt nitrate hexahydrate) DUP030001247 RECOMMENDED SYSTEMS FOR USING RC-SOO TOPCOATS rt ifn ii n n> --n m>w w -- < m tmj ' n mum m' Operation en Grain Wood ahoEany & Walnut) Close Grain Wood (Maple and Birch 1* Stain Dry NFL for walnut ana Luxol for mahogany to minimize gray pores* 15 to 30 minutes at room temperature* 3$7 line (oil type) 16 hrs or longer at room temperatures of 60F. or higher 2c Uash Coat Dry 1366 for good ouality None veneer JRK-A10336 for poorer * - quality grades of veneer 1366 should he flashed 1 * hour J-RK-X-10336, if baited simultaneously with the filler, should be flashed one hour. Otherwise bake J-RK-X-10336 for 2 hours or longer at 130~llJOF. 3 Filler ~ X" Ul um iltli J Dry 27-5000 line None or 27-5000 line Filler, or filler plus wash Filler If used to be coat, are baked 4 hrs* at baited 4 hrs. at 130-1^0 F* 130-140 F. 4, Sealer 1366 1366 Dry 3and One hour at room temper ature (60*F. or higher) Scuff lightly 'with #360 paper One hour at room temperature (60'^, or higher) Scuff lightly with #360 paper* 5. ^aze Dry Optional. 26 line as represented by the com position of P-26-R-555674. Flash off solvents which should not recuire more than 1 hour Optional. 26 line as represented by the composition of 1*26 R-55674. Flash off solvents which should not require more than 1 hour. DUP030001248 Operation 6. Shading Laooaer Dry 7. SSsgg^Josgoa^ Bake -25 Open Grain Wood (Mahogany & Walnut) Close Grain Wood Optional. 266 line Optional. 266 line 1 hour at room temper 1 hour at room temper attire (60*Feor higher), ature (6oF. or higher' For maximum quality apply 2 coats, flashing 30 minutes between scats and 60 minutes prior to having. \ 2 hoars, at 130-*X4oF, and 35$ R.H. Cannot be air dried. For maximum quality apply 2 coats, flash ing 30 minutes between coats and 6o minutes prior to baking. 2 hrs. @ 130-140 F. and 25$ Cannot be sir dried. .camMGM DUP030001249 d is t r ibu t io n ** Br. _R,,B. Davis* Flint Mr/B*E Thomas* Newburgh Mr, M0XUf*Phila. Lab. Dr, CUD, Qravasi '%om )In Dr, J,,D, MeBuraey^ Nilm, 1 Mr, U.B. Bullitt* Kliau ' )tam Mr, Matt Denning* 10.1m. Mr, H.J. Haon* Wm. Mr, P.B. Cochran'* |OLlm. Mr, j.D, Sfclels* Wilm, Dr. L0G, Wise* Exp, Station* Wllm, Mr, A,K. Br3ce8 Wllnu Mr, H,D, maay* Parlln r e p o r t w o , 975 DUP030001250