Document EvO3059nGD0MENoGrqZyeR90g

E. I. DU PONT DE NEMOURS 6* COMPANY PIGMENTS DEPARTMENT 236 VANDERPOOL STREET NEWARK, NEW JERSEY I Uj ' r NEWARK PLANT CHEMICAL DIVISION - COLORS NSW DRIFT TOBB PROCESSING METHODS Priod Covered August 1949 ** Ootobar 1950 DATE: 1/27/53 I .4 A' 4 i V' DUP050069185 Serial No* KN-53-1 Copy So, a Copy tos #1 - Humerical File S * Research Office (223*4) 3 - library File (223,4) 4 - J. N. Mly/A. Siegel 5 - Plant Piles - H, Arnoul 6 - Jackson Laboratory - Orchem 7n ,, 8 - V, H. Chalupskl - Newport 9 - J. H. Cooper - Newark 10 - E, F, Klenke, Jr, ~ Newport 11 - #14 Bldg* File - Newark 12 - Extra 13 - 14 - " NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report Titles HE DRAFT TUBE PROCESSING METHODS Period Covereds August 1949 - October 1950 Charges A-IIC-265 SUBMITTED BY: E. F. KLENKE, JR. APPROVED BY: J, H, COOPER DATE SUBMITTEDs January 15, 1963 DATE ISSUEDs January 27, 1953 DUP050069186 INDEX Introduction Summary and Conclus iona BT-284-D g t -674-d GT-710-D BL-288-D BP-173-D and GP-501-D BT-287-D and GT-689-P Experimental Details GT-674-D and GT-710-D BT-284-D BL-288-D BP-173-D GP-501-D GT-689-P BT-287-P and BT-321-P Design Data Operating Data Quality and Performance Data Summary - Table I BT-284-D GT-674-D GT-710-D - BL-288-D - II III IV * V BP-173-D - " VI - VII GP-501-D - VIII D.T. Capacity- w - IX n - X Filtration - w XI Drying - 55 XII Pulverization- n XIII Plant Formulas and Notes GT-674-D* BM (GT-710*C| Appendix I GT-674-D (D) w II BT-284-D (C) BL-288-D (I) n III n IV Equipment Diagrams Semi-Works Draft Tube Unit - Figure I Plant Draft Tube Unit - * II Reference 1 2 Page 1 1 2 2 2 2 3 3 3 5 6 7 8 9 9 9 12 13 14 16 16 17 18 19 20 21 22 23 24 23 29A 26 30 34 38 39 40 41 DUP050069187 DRAFT TUBE PROCESSING Introduction Draft tube processing, as applied to phthalocyanine pig ments , was first conceived and tried in August 1919, during the development of a process for production of soft texture CPC blue and green toners. In searching for plant equipment to satisfy the requirements of the process for manufacture of GT-674-D, a turbine agitated vat was first selected. Initial results were satisfactory; however, no more than 1/S of the vat capacity could be utilised without causing serious quality degradation, resulting from a decrease in agitation efficiency. Since the success of the process depended upon the uniform dispersion of a water im miscible treating agent In the pigment slurry, it became obvious that the use of special equipment would be required, to permit realization of the economies of large batch size manufacture. It was estimated that an expenditure of approximately $>10,000 would be needed to modify the existing equipment, with no assur ance of success; therefore, other means for obtaining the same results was sought. The use of a draft tube unit ultimately was oonceived and developed as the answer to the equipment problem, A semi-works unit was assembled for trial operation, and the results were sufficiently encouraging to justify consid eration of a plant installation. A pilot scale unit was then improvised in the plant, using the obsolete and unused chrome yellow continuous manufacture unit, to provide scale-up design information and additional quality data. The quality of the pilot unit products confirmed the semi-works results; therefore, a pro ject was submitted and approved for installation of a plant scale draft tube unit, (see Figure II.) Standardization of several CPC codes was accomplished without difficulty in the plant unit, and to date the performance of the unit has been entirely satisfactory. Summary and Conclusions The draft tube unit was developed to meet the need for equipment to produce optimum quality GT-S74-D and BT-284-D at a larger and more economical batch sis than could be made in the then available equipment. The quality of material produced in the semi-works unit exceeded expectations; definite quality improvements were obtained, in addition to the goal of increased batch size. For this reason, the scope of the study was Increased to include draft tube processing of other CPC products, as well as numerous ctaroon pigments. {This report is confined to the CPC work; the .iiaroon study will be covered separately.) The encouraging semi-works results were confirmed In the plant unit. In summarizing the accomplishments to date, it DUP0500691 -2- can be stated that the plant draft tube unit has significantly increased the plant productivity of CPC products of improved qual ity, with resulting savings in raw material and operating costs. This has been accomplished at a relatively low increase in plant investment and has provided the plant with a unit with much needed operating flexibility. An operating unit is now available that can economically provide the benefits of extremely intense agita tion, with no sacrifice in adaptability or limitation of batch size. The following summarizes the individual accomplishments for each of the products that have been draft tube processed to date. {See Table I for tabulation of these data.) 1 - BT-284-P The batch size was increased from 400 lbs. to 1,260 lbs., and a strength increase was obtained, thus permitting dilution with an inexpensive inert extender, (blane fixe*) during draft tube processing to equal standard strength. {See Table II for semi-works and plant quality data.} significant raw material {CPC) savings have resulted, as well as savings in labor, processing and testing, etc. The plant adopted the BT-284-D (0) formula April 22, 1950. ^Subsequently changed to barixsm rosinate, 2 - QT-674-D The batch size was increased from 420 lbs, to 1,260 lbs,, and some improvement in ink mill properties was noted. This product was also diluted with 5% inert extender {blenc fixe) by decision of Sales. {See Table III for semi-works and plant quality data.) Raw material (CPC), labor and related savings have been realized. The plant adopted the (2T-647-B (D) formula May 12, 1950. 3 - OT-710-P (Originally coded GT-674-P* HM) A product equal to the semi-works standard was obtained at the large (1,200 lb.) batch size. {See Table IV for semi-works and plant quality data.) The formula was adopted by the plant May 12, 1950. 4 - BL-288-P Use of the draft tube unit penait ted formula modific ations that resulted in improved dry lump uniformity, freedom from grit, better dispersion in linoleum and plastics (vinyl), and increased strength. An increase in batch size from 1,585 lbs, to 3,170 lbs. was also accomplished. (See Table V for semiworks and plant quality data.) Aside from the benefits of increased DUP050069189 -3- batch size, the chief advantage of the draft tube process has been the elimination of hard undispersed pigment partteles (grit) from the final product. Because of customer insistence on gritfree material, all BL-288-D production has been scheduled for the draft tube unit. The plant adopted the BL-280-D (I) formula June 7, 1950, 5 - BP-173-D & GP-50I-D Draft tube production of these codes was tried primarily to determine whether any strength improvement could be obtained that would permit reduction of the CPC toner content. (The toner content of batch produced as BP-173-D had to be increased from 73.4$ to 76.0$ to meet standard strength.) During the trial study a sim plified formula was introduced, substituting sodium roslnate for the usual separately prepared ammonium rosinate, thus providing a raw material savings ana reducing the fire hazard (during pulveriza tion) due to the presence of free rosin. The results were quite encouraging! (See Tables VI and VII for seml-workn and plant quality data.) standard strength BP173-D was produced at 74,4$ toner content as compared with 76.0$ toner content of batch production, and all other properties were found to be essentially equal. An Insufficient number of OP-501-D draft tube batches were made to do more than establish the fact that standard quality material could be made at a lower (72,6$ as compared with standard 73,6$)toner content. Because the draft tube unit was needed for other pro duct ion, the standardization of these two codes In the unit was not possible. 6 - BT-287-P & GT-689-P Trial of the draft tube unit for production of these codes was limited to one semi-works batch each, to determine if standard quality material could be made. The 4,000 lb, maximum batch size in the Abbe* Lenar*t mixer Justified these trials. Standard quality material was obtained in each case, and a 20,000 lb. batch size forecast for the plant unit. (See Table VIII for quality data.) Due to the priority of other work, plant trial of these codes has not been made. Experimental Details A. - GT-674-P & GT-710-D As previously stated, the draft tube study was started In the semi-works using the GT-674-D (C) formula. The Green used at this time was the solvent milled eutectic type. After the size and relative dimensions of the semi-works draft tube unit DUP050069190 -4- w-5*$established (See Figure X), a variable study was conducted to determine the optimum conditions required to Cl) produce ma terial of standard quality, and (2) obtain additional quality improvements. Listed below are the variables evaluated, together with comments regarding their effectiveness, 1 - A 5$ concentration of pigment in the final slurry was found to give the best results, when the 5$ CCl4 - 2$ TEA-C12 ester emulsion treatment* was used, When only 10$ CC14* was used, a 10$ slurry concentration appeared to be most effective? at higher concentrations the slurry became quite viscous and the recircula tion rate was measurably reduced, making a longer cycle necessary, 2 - Since the use of CC14 and TEA^C^g was already well established, no attempt was made to find other agents. The only variable tried was the use of 10$ C0l4 without the TEA-Cig ester? the ink mill properties remained essentially unchanged, but weak ness in the neighborhood of 5$ was disclosed. When tested in plastics (Vinyl), the CC1* treated material was found to be super ior to the ester emulsion treated products in ease of dispersion? therefore, this treatment was ultimately adopted and coded GT-710-D for sale to the plastic trade, 3 - Addition of the ester emulsion to the pigment slurry circulating through the draft tube at 190 to 195F, with continued recirculation through the draft tube for at least 1 hour, produced optimum quality material. It was found that the treating agent could be added to the slurry in the holding vat provided adequate agitation was provided to disperse it rapidly. Subsequent circula tion through the draft tube was necessary, however, to obtain satisfactory quality, 4 - Heating of the ester emulsion treated slurry at 190-i95F produced material of superior tinctorial and printing ink properties, as compared with material treated at room temper ature, Heat development of the CC14 treated slurry (GT-710-D type material) gave no evidence of quality improvement. 5 - Since pan loading the GT-874-D slurry (5$ solids) would require an excessive number of dryer cars, the material was pressed (but not washed) before loading onto dryer care. There were some indications that this filtration step gave a slight improvement in tinctorial properties (strength and inten sity), Adjustment of the slurry pH from approximately 8-10 to 5,0-6.0 prior to treatment gave some evidence of improving the pressing characteristics, and possibly causing some improvement in tinctorial properties (See Reference 1.), *$ calculated on a dry pigment basis. DUP050069191 6 - When using the 10% CC14 treatment of a 10% pigment slurry (GT-710-D formula), it was found necessary to add the CC14 into the vortex of the draft tube during circulation of the pigment slurry at roan termperature. Heat development at 190-195F gave no quality improvement, and addition of the CC14 to the holding vat caused a noticeable quality degradation. The final slurry was heavy enough to permit pan loading, which was also preferable for optimum quality, 7 - Comparison of.the draft tube processed material with products made in the Ai>b& Lenart mixer disclosed a 5% strength advantage for the draft tube products. To compensate for this strength increase blanc fixe was added as an inert extender. Addition of the extender to the holding vat, following the emulsion treatment and recirculation period,was found to be satisfactory provided the agitation was adequate to prevent settling before it became dispersed (satisfactory in the plant D.T. unit). 8 - High speed (instead of regular speed) pulverisation of the CC14 treated produced for use in Vinyl, measurably improved properties such as ease of dispersion, strength, texture, etc* Standardization of GT-674-D and GT-710-D (coded GT-674-B* HM at the time, to identify it as material for use in plastics) in the plant draft tube unit was started on April 4, 1950, and accomplished without difficulty. Twelve consecutive 1,250 lb* batches of GT-S74-D were made (previous maximum batch size was 4.0 lbs,), all containing the 5% inert extender; the average quality was slightly superior to standard (See Table Hi for a tabulation of the results,), thus exceeding expectations, (See Reference 2,) Excellent duplicability of results and the absence of any operating problems prompted the plant to accept the GT-674-D (D) as standard on May 12, 1950, (See Appendix II for formula and notes,) The process for draft tube manufacture of GT-674-D* HM (see above) was also accepted by the plant on May 12, 1950, (See Appendix I for formula note) Despite the fact that prior draft tube development work was limited to one semi-works run and complete operating data v/er not available, the first plant batch was fully equal to standard in all properties, as were all subsequent batches; no operating problems were encoun tered, (See tables III and IV for results,) D. - BT-2B4-D 4 The semi-works draft tube wit developed for GT-674-D was used for the development of a process for BT-284-D, using the (B) formula. Since this basic formula was quite simple the variable study was quite limited; investigations were restricted to finding the optimum operating oondit'ons. The following summa^ rlzes the variables tried and the respective effects. DUP050069192 1 - A 10# solids content slurry was found to be optimum; slurries of higher concentration required longer recirculation times and were difficult to pump, 2 -As in the case of GT-710-D, the addition of the COI4 other than into the vortex of the draft tube during clrcu~ lation of the pigment slurry, caused some quality degradation (poor ink mill texture and "separation" on the rolls), 5 - The use of TEA-Cig ester with the 0014 (as for GT-674-D) gave no quality improvement, 4 -A comparison of pressed and panned material dis closed some evidence of a strength loss (2-3#) attributable to pressing; therefore, direct pan loading was adopted, $ - in the plant unit the batch size was increased from 1,260 lbs, (400 lbs. was the maximum batch size in the Abbe8 Lenart mixer) to 2,520 lbs,, and the treating agent (OCI4) reduced from 10# to 5# (of the pigment weight) with no discernible loss of qual ity. The only operating problem encountered at this larger batch size was the excessive demand on dryer cars; therefore, the 1,260 lb. batch size was adopted as standard, 6 - Evaluation of the draft tube processed material disclosed it to be at least 5# stronger than Abbe* Lenart products {.Lot 71505 vs 71457 and Lot 15712 vs 15644) and BT-284-D standard; therefore, 5# inert extender (blanc fixe) was added to reduce the strength to standard. The addition of the blanc fixe to the holding vat, following the CGI* treatment and recirculation period, was allowable provided the agitation was adequate to disperse it (satisfactory in the plant D.T. unit). Addition of the extender through the draft tube was found to be undesirable because it had to be added slowly to prevent excessive settling in the low velocity zones outside the tube. Pinal standardization of BT-284-D in the plant draft tube unit was started April 22, 1950, and on May 12, 1950, the plant accepted the process as BT-234-B (C). (See Appendix III for formula and notes,) Luring the plant development period more than a dozen batches were mads with excellent duplicability of results; the average quality (with the extender included) was slightly better than standard In strength, us well as in printing ink properties, (See Table II for tabulation of results.) C, - BL-283-D . Development of a draft tube process for manufacture of BL-28S-D was prompted by (1) the possibility of improving qual ity (strength improvement such as obtained for BT-284-D), or re ducing the toner content, (2) the hope of increasing the batch size, with resulting labor savings,.and (3) the unique provisions of the draft tube unit for screening the K-623 and the final prod DUP050069193 -7 - uct (see Figure II). I tan (5) was most important because of cus tomer complaints of streaking--probably attributable to dry lunp non-uniformity, due to the presence of hard uadispersed granules of pigment. Snail scale development work was restricted by equipment limitationsj therefore, after a few semi-works runs to confirm the feasibility of the process, the development work was continued in the plant unit starting May 3, 1950, The following variables were evaluated, using the basic (H) formula, 1 - Since the draft tube unit had the facilities for heating the slurries being processed, the effect of heat devel opment was investigated. Heat development at 185- 195F, fol lowing the addition of Resinous Oil X-l and a subsequent recir culation cycle, was found to improve the dry lump uniformity as well as strength. The heat treated material contained no undlsparsed extender {Abbe' product was full of white particles) and was 5-5$ stronger than the cold samples (See S.V/. lot 2099 and plant lot 71366), 2 - A comparison of pan loading vs. pressing was made, and the pan loaded material (from the same D.T. batch) was found to be 5$ stronger and more intense than the pressed portion. Be cause of the excessive demand on dryer cars, however, pan loading was not adopted* 3 - The batch size was increased from 1,585# to 3,170# (twice the Abbe* batch size) with no evidence of any quality loss, and no operating problems were encountered. Following this rather limited development study, during which it had been demonstrated that excellent quality material could be produced by the draft tube process (See Table V for a tabulation of results), the plant Quality Control Group accepted the problem. On June 7, 1950, the plant adopted the draft tube process as BL-288-D (I). (See Appendix IV for formula and notes.) Subsequent to adoption of the (I) formula, the Sales Department requested that all BL-288-D be made in the draft tube to insure minimum "grit*1 in the product, D. - BP-173-D A draft tube process for BP-173-D was developed in an attempt to meet standard strength using less CPC toner than the batch process. Plant batch production required the use of approximately 76$ toner as compared with 73.4$ for standard. The development study was started In the serai-works using the (D) formula (lots 2227, 2228). The experience gained prompted the use of a sodium rosinate solution to replace the DUP050069194 8 separately prepared ammonium rosinate, Mid this ''simplified for mula" was tried (lot 8229) with success. Since the (D) formula products were weaker than standard, further trials were made at increased toner content (lots 2232. 2233, 2267). The results of the semi-works study indicated (l) the draft tube products to he slightly stronger at equal toner content, and at least equal in all other properties to hatch products prepared as controls, and (2) standard quality was reached using the simplified formula with 74.6# toner; therefore, a plant study was started. Six plant hatches were made in the new draft tube unit, and portions of each were set aside for a new standard (see Tables VI and VII for detailed data). The proposed standard (NS-865) was ultimately rejected because of weakness (See letter JCN to FEB, 4/3/51). During the semi-works and plant studies the following variables were evaluated;- 1 - A 5# increase in toner content gave a 5# strength increase. 2 - Praft tube processed material sampled before heat development was fully equal to the final (heated) product. The "cold process" was con sidered more desirable because it reduced oper ating time and permitted slightly larger batch sizes to be processed. 3 - The use of sodium rosinate instead of separately prepared ammonium rosinate was found to simplify the operation and produce material superior in paint properties and fully equal in all others, (See Tables VI and VII.) 4 - The standard solution and slurry concentrations were considered optimum for good draft tube performance* E. - GP-501-P The experience gained during the draft tube processing of BP-173-D was applied to GP-501-D to determine whether 1) a reduction of tcnsr content would be possible,and 2) if formula improvements (increased batch size, reduced cycle, etc.) could be realized. Only twc semi-works batches (2269, 2270) and one plant draft tube batch (18857) were made, and the foiloiling conclusions were reached;1 1 - As in BP-173-P, the "cold'' material was fully eq*?salio the heat developed (std. ) material. DUP050069195 9 Use of th ''cold1* formula simplified the pro cess (3 hour shorter cycle) and permitted us of larger (+ 1,500 lbs. vs 1,180 lbs.) batches 2 - Th simplified formula (sodium rosinate Instead of ammonium rosinate) gave material fully equal to standard at slightly lower toner content (72.4$ vs 73,2$; see Table VIII). 3 - The hue of standard'could be rntched by adding a small quantity of S'-623 (Blue LB) to the N-624 (CPC Green) before processing. Following the above brief study, GP-501-D was considered ready for restandardization in the draft tube unit;however, the work was deferred until standard quality N-624 could be spared for this purpose. P. - GT-689-P The semi-works draft tube unit was used to prepare one batch of GT-689-P to determine if any strength improvement could be gained and/or the process simplified. The results of the single batch (2105) indicated that material at least equal to standard could be produced at a greatly increased (20,000 lbs.) batch size* Nothing more has been done, G, * BT-287-P(and BT-321-P) A single draft tub batch (2111) was made and evaluated. A product fully equal to standard was obtained and, in the plant unit, a considerable increase (to 20,000 lbs,) in batch size should he possible. Nothing more has been dene. DESIGN DATA The #6 building (Newark) draft tube unit v/as primarily designed around the available 3 ET.P, variable speed D.C, motor, (used in the draft tube) and the 3000 gal, turbine agitated vat 240; however, the following basic relationships (developed In the semi-works) were kept in mind and followed as closely as pos sible: 1. Turbine agitation was considered most suitable for the holding vat. 2. The capacity of the holding vat is largely dependent upon the capacity of subsequent processing equipment. For sample, if pressing capacity is limited to 1,200 lbs, of color, there would be no advantage in designing a D.T, unit to process 3,000 lbs. Therefore, the pressing and drying requirements must first be estab lished and capacity determined, then the holding vat designed to fit into the production pattern. DUP050069196 - 10 - 3, Having determined the volume of the holding vat, conventional design data may be used to calculate the turbine size, etc. Selection of the circulating pump Is the next item. Semi-works and plant exper ience has emphasized the desirability of using a positive displacement pump for circulation (prefer ably a piston pump) because pf the heavy consistency of the slurry during treatment of the pigment. The centrifugal pump used with the plant unit performed satisfactorily with CPC products, but was incapable of handling some pf the `^roon slurries. The minimum pumping rate can be calculated as follows? (1) Batch size (gallons) x 3 - Hate (gal./nin.) Troces s in g c^le"XmiriutesT (2) (1) The factor 3 was empirically established in the semi-works unit as the required number of times the entire contents of the holding vat should be pumped through the draft tube to insure at least one passage of each particle through the intense agitation zone, (2) The processing cycle referred to is the total time required to add the treating agent (also equal to the time required to insure homogeneity of the material after treatment). In general, this figure will be arbitrarily established; for example, if available equipment time is limited to 4-1/2 hours, and if loading and other preparations take 3 hours, then 1-1/2 hours is left for treatment and subsequent agitation for uniformity, or 3/4 of an hour for the processing cycle. 4. The capacity of the draft tube vat may be determined as follows; gal. /min. minimum pumping rat (see above) x 2, min. - Capacity (gals.) The usual ratio of diameter to height may be used. (1:1,2 was used in semi-works and plant.) '(3) The 2 min. figure was established in the semiworks as the desirable retention time of an average particle in the draft tube vat. 5. Design of the draft tube itself plus specification of the propeller size and locations within the tube is probably the most controversial item to be con- DUP050069197 sideredj however, reference to engineering design data (DG-3.1E, etc,) plus the following should per mit fairly accurate specification of these pieces of equipment. In the plant unit two .5" diameter marine pitch propel lers rotating at 2000 RPM In a 101' diameter tube situated in a 38* diameter tank, satisfactorily agitated and circulated (within the tank itself), fairly thick (4) pigment slurries being pumped into the draft tube at approximatly $0 5PM. (For actual relative dimensions refer to the appended drawing #1.) (4) Some of the slurries (BT-284-P, BP-173-D, BL288-d ) attain a consistency of heavy cream. No accurate or significant viscosity data have been accumulated to date. The following modifications are recommended for future draft tube unit installations: 1, Future instalrations should include two agitated steel tanks, approximately 400 gal, capacity, equipped with steam and water lines. These tanks to be used for preparation of the treating agent, etc,, and the discharge lines should discharge, through rota meters, into the draft tube, 2, The discharge line from the draft tube tank into the holding tank should be as short as possible (space must be allowed for the control valve) and preferably vertical. These provisions will facll- ' Itate flow of heavy consistency slurries and min imize clean-out problems, 3, All controls (rotameters, agitators, switehee, etc,) should be mounted on a panel close to the draft tube vat to permit most efficient operation of the unit* 4, Two screens in parallel should be provided in the pump discharge line, to permit clean-out of one while the other is in use. This will eliminate delays due to screen plugging, $, With regard to approximate unit size, calculations based upon the #4 (1930) sales forecast indicate that a unit the size of the present one in #6 building (Newark plant) would be adequate. Although 90$ of the #6 building unit time is currently being sched uled for only four of the eight codes {.BT-284-D, BP-173-D, BL-288-D, and GT-674-D), the fact that at least 1/3 to 1/2 of the making time for each batch DUP050069198 12 -- Is devoted to dumping 1-623 or N-624 from drums into the unit would seem .to indicate ample processing is available, provided the loading step could be simplified. Installation of a draft tube unit at Newport would accomplish this simplification, since slurry could be pumped directly to a storage tank and thence to the D.T. unit as needed, thereby elimin ating all drum loading or unloading, OPERATING DATA Operation of this type of unit has been found to be relatively simple, and excellent quality material has been con sistently produced when the following basic principles were fol lowed % 1, The level of slurry in the draft tube tank must never drop below the upper edge of the draft tube .and.''1'' for maximum efficiency, should be maintained (1) sufficiently higher (+ 3 inches) than the critical level to cause the slurry to flow into the draft tube from the annular space. The slurry level at which this flow into the draft tube is at a maximum is almost independent of the range of viscosity en countered thus far, and does not vary significantly between codes, 2, Ingredients (or treating agents, etc.) specified to be added to the draft tube must be introduced into the draft tube itself and^no^ merely into the vat; otherwise, standard quality material cannot be produced, 3, Best results have been obtained when the rate of addition of material into the draft tube (during circulation) did not exceed two times the ultimate percentage of the ingredient in the final batch. For example, if CCX4 is to be added to a batch of color to give a ultimate treatment, and the pimping (circulation) rate is approximately 50 GPM into the draft tube, the CC14 should be added into the draft tube at a rate not exceeding 5 GPM. (2 x 0.05 x 50 - 5 g./min,) The following tables (IX to XIII, Incl.) contain a tab ulation of the operating data collected to date for each code processed in the plant draft tube unit. (1) Liquid level in the draft tube tank is controlled by ooeration of the valve on the outlet line from the draft tube tank Into the holding vat. Generally this valve needs little or no attention once the proper level has been established. DUP050069199 IH 10 w HA x> a \ 0 & \ P > 4C--O4 V^ CO p tc P 8 5 p0 cr a a 0oC >9 P o 14 2 s 00 ft % \ > \ \ > \ to p c ft p 0Q o o a 0 CH O> Eh r. ^5lft <c Eh 14 PQ s CO m w o a <c >s P 43 o HH H> Pc 0 Cj? 14 jft s w cu M &< P Eh M fi M 0 g3 ft n CO P Po P T* o> p ft < 0 14 ft O Eh <0 <H Q-t 0 O a p 0 S ft O H > P 0 0 H ft i uo 03 0 o o H P 0* tO --4 *o 01,10 + }u 0* fr1> w 01 H t>>-. o o o o HH O o H to >-> 0*4^' <0 01,10 + ft l> tO 4_Cf- o JCO4 .H44-- . tO 4-4. 01 . to P i- >-- + w W VI. * 0 r 0* p 41 w < P oo * o X) pp CO CO ' S P cO to a p CO pp CO CO 9 .O xf x3 PP CO W O'"* o~ o-- OH OH OH 01-' 01 w Cl > * HH H tH to o --' 0--4 o -- 01 to QO 4--' - QH OH o H QH H 01 CVl4^ '--' CO 01 OP O 0* 0* 0 O }S to O Q 0 C~ CQ tO CO H H HH 4-:.* Oft O O- O H OH PPOP <efl ft Hi* p --< a 0 N CQ N rl 0 H 0 0 ^0 P O G P P rl P 00 PP P P `d tc >o 0 w m 0 14 0 P 0m ?0 o 0^ 0 H IP H n * 0 P <P P 0 0 0 0 0 CO o. O O H p HP G ffl 0 o. 0 H , P 0 0 O PCS 0O 0 N 4pH 0 o o OOP 0 . ( *r\ P ft 0 ft 0 0 P 0 rl H ffl o o P H 0 H 0 tt, p St 0 ft O ft O 0 0 1 P ap SP o P H H0 s ffl o 00 0 < 0 00 0 P O & W 0 ,, 0 O wO^ 0 P *0 H HP O0 P0 0P 0 O S3 OO 0 XS O' p o 00 00 p 0 !S O w ft 0 ft 0 P H H P O P 0 P *o w 0 ffl 0 o 0 w aA i .1 0 co " Cl P O i 1 O P Eh CO El O A i O H CJ Eh P A AA 1 tl CO to H 00 J> O Cl H in 1 1i A CL, ft CO A ft ft 11 > 03 A a <8 Eh Eh A 0) ft P p a S1*0 % p O 00 f0c-fl O -PPi 0 0 P 0 OW 0 0 0 14 0 ffl 'Cl ffl O 0. 0 0 0 t? O 0 o , . P 0 <0 G _ ,, H 0H P *te p 6 P P P t>0 twopta pbo a H GH G 0 O Pi 0 3 p, Pm p pm type v^. fOfl Vi. o^ti.^<-3 p to PlO H0 II II rl 0 PH :> o 0 0 H 0P P P .0 xs 0 0 0 0 40 O P0 ft4 0 OH OPf o 0 <s o H P 0 o 0 OS* * 0 o JS p 0C1O .a0 \ttoV0oc OS' fltf c S ffi -p pi _ 01 3 S' 0 ca fd SH !0 K Pj *0 to H o 5* jg I 0 (fit fA0tf0t 0g 0 O0 0 ffl rt 0 vl OH Hp 0 p o cr 0 0H >0u0 p ffl $C4 OPH 00 0EH0 O P *_0 ffftl 0 p SA 0a 0 0s J 0 0'O 43 % p ,~ *rt p n hH O O 0 0 {4 C> 0 P ft HH ^ 0P 0 poP pa 0p, a3 0 SPH ft 0 O 0 <0 t S2 to as.g n p o p 0 p f0t p0 H0 0 <f4t P P ft 0 00 0 p P . O sa H g$g `O 0 P 0 H0 14 O p ft <S G PGU_ ffl POO X >P0 00 14 O 'OP P G 0P P 0 ft , Uo 0 O g 0s H'O H tl . *$ig .**8 . tO P 0 tj H 1> 0 0 0 0 0 0H SS O 0 0 0 0 H0 T0J 14 OP ftH 0 p- -0 80403 P0 p90 X2a. 0 HO P 0 p G ffl > O H *> P 0H 00 O 403f0/tliHfrt4 f0Ot "2 Sj'fg^Sl lfiii^ HH 4> > Ofe 3 o p 0 a _ 0 0 0 p p F SPSS'S"" O 0 8 0 O __ 0 14 *0 C P ffl 0 0 P 0cpGoHgiioais P 0*0 g t0a,, i-< 00 p 8G ftpWTfeS. 00 ft 1 O 0 0 0 P to O ft * ft a 0ft *H O 1> H P0-1 ,, p 0 ft fpt H ffi 1 3< CJ H -0 H 03 *0 U) <0 CD DUP050069200 1S-A I * 8 I Oo rH 3 .s DUP050069201 14 - TABLE II BT-284-D DRAFT TUBE BATCHES 1 Sib Out 1 Texture Lot Type ! MT str. Tint | 3L 5X L5644 400# - Abbe * Lt. 101 vs dull tm 15712 (1) 1200# D.T.(5) 3. dk. & int. 95 vs grn. - 15772 40# from 15712 15757 (2) 1236# (6) vvs dk. 99 int. 15795 (2) 1236# S) S* X'b* OK vs int. 14-- 18 14 17+ 15862 (2j 1648# (5) s. It. OK vs red 14 17+ 14 17+ 16013 (2) 1236# ws it. 101 vs red . . <M 15831 (2) 1236# (5) It., red OK s int. 14* 1814 17+ 15996 (2, 1236# CK, s red 99 vvs red - - 15997 (2! 1236# vvs It. 99 vs int. m 15998 (2; 1236# It, 101 vs dull - 16305 (3; 1260# OK, s int. 98-99 vs int. - 17305 (Si 2520# s dk., int. 97 int. - 16+ 71505 4; 170# 6 Bldg. 2005 Cont.Yel.TJhit S.W, - CC1* OK 94 s int. 17+ mtt Mi jw .- 2006 S.W, - CC14 t e a -c 12 '- M - :w - 2044 S.W. - cci4 Cont. adc OK 95 s int . M 17+ 2045 S.W, - CC14 Batch add OK 93 s int. m 17+ Cl) Contains no extender {see page 2) j same H-623 as lot 15644, (2) Contains 3# blanc fixe (see page 2)* (5) Contains 5% blanc fixe (see page 2)j also only half the standard ^ amount of CC14. (4) 5-8$ stronger than Abbe* batch 71457, (5) Average gd. yield for the 5 D,T. batches -was 99,4$. DUP050069202 i to a -t A i> W L W JfiH I--1 + + HH HH .X? X rl P-l? x? x* \s HH a P1 1 B <a P1 W1 i* 03 HH 03 01 HH x? X H fi- fc- 03 x? XX rH rH toco II 1 1 1 Hf '* Js.fiHH cooHH 4* H03 HH 1 to 03 HH x? a* H rl fi-fi* ` xj* X IH 00 6- ccH *& SsXs HH C0 to 03 x? XX HH to tO II 1 t II * i 1 II 1 t II ( +l COG C> CQ H H rl H ++ + 03 03 to 03 H H rl H 3 g o 9' tCx-O?#Hco Eoh Ofrt &* o 2 0 ffO 1 o^ M U5 o o> ,^o 4p T4.1 ji> --.w oc . K art i f tO lO cn 0> H pPe i art I >to C6K-'<M(H3 . a--ax-a I 00>> C0>O rl 49 >c ; w> a i, art 1 I 60> oG mM t> Eo> 0 pp cc H H3 & H CQ o X02a VCrSf* H Bo s ^ HH H H99 p pH r-t M p pa p c *c& *c H COCO H > 0 H rl {H 1 as 1 P * rl tH 5 H I^ P P H8 P Hc r-t I 1 a. M Cl VP P p p I >4 P ** * i H tO ca fi at CO C> s I 3 I o H tOi. o03 C* xH to H H H to O o qo O O O H H H H rl H $<0 to 03 ' 03 03 as? 03 CO 1 58 I 03 *0 to rH CO 03 00 03 W t 1 U3 to I tp rl 03 & o> 03 t-t03 03 03 0 03 pH: rl H H H H H rl H co w to i tO 03 I I CO E03 i t to to to g 'SJ 03 CO 03 H c- 03 03 (O x? fiO tO 6- 6- (0 tO 03 03 03 03 HH H H HH H H N H W * to 03 H Xf P V) o G 03 H UP to o to 03 H <o P w 03 * 03 '0 to P cO oto 03 H O to Oto Oto O to 03 03 03 03 03 H HH H H =tel rCOl + 03 O ltO--I H to xH 03 to 03 tO H H IO ttoo to. H to X? to H X?H to lO tOx? lO H to 0 o to H CD x? H to H O ctP H CraQ <io0 6- CD to CD HH to (0 !> 03 03 .rfct- TABLE I I I -u-All c o n ta in b% e x te n d e r (see page 2 ) DUP050069203 GT-710-D QUALITY DATA *>i| 4'"'P4*K E*! w ft 81 | 111 S^*9^-I1 43 a toI <0 CO 1^ ' !i 1 01 \ H IH !i I 10 1 <h a Mo CO & I !> + 00 c ffl p H M 1 e B taIi i w| i Wn>*W ca X K"S Sfe: QH <0 H (O 43| * O w IO Ml CM CM o 43 to % Cr-t 10 H \ DUP050069204  Cl 03 fr-5? tO tO 03 CO CO CO 8* CO o 44) 43 to H to 01 tO O o to to 01 CO "S' 1-1 00 coco CO <0 CO CO to oa n * *v w > g 0tp3 to COCO rjOOS I to o rl CO 01 to ^ 03 fe! I 0- CO CO CO CO Js; tot c rrati fot Uft*= *o fit c s E 0 Ot a. PU CO 8 j+a>- & Off <D s01OMKiOH WM.. t0O5 c- a ft H O O rl O O II 43 rl CO c E-i * d 3j! I ft b? C HO St fH I> 03 O) 'St tO O 0 H tO 10 CO lO a* h * tO h i tO to 03 03 CM 03 W 01 <a ;a CC pH 3 ?H 43 to W SiS 03 O 03 H ^ O "S' tO H C- CO n P rH 0310 to to to W CO 10 H H rl o 5s to c s a to H - e< E E R XI .<O5 S E E E-< R & IOQ05H CO CO 03 tO tOxpsPCO W 0> H tO tO tO H tO tO CO tO 1--I co o> o 03 o o h h CU iH r4 03 i--1 rl rl t- t* a 3-5$ samples were c o ld and a fte r heat development j the rubout and linoleum e va lu a tio n * re by XI 43 xi 43 43 ft tJ XJ 43 43 ft rl C0&, ra ft toe- T H toe- ca oc as a o H 43 ft 43 g O c 0 H o o c r-l ft xi rl gC a' 1 * 43 E4 64 * RR % COR Q 0> 05 O OOrl 0103 03 ft 0 * 43 rl 0 S h P H t 1 01 to to H tO to 00 r-l : * <g to to -tH $ 03 03 03 li II II * 43 Sft X> x> 3 43 <0 x gi g ^43 $X^ a c o ft 4paR 4 CftO 5 befo ples ken sam tla wf iernea les the ^Samp than DUP050069205 cQw O ^M COO* CHO (^0 tIfr II<0>* C* !> 1> tH t* &* Vi o CO H & C*O'sHf^t ">I> lO COW ft o CJMMCMMtSO jd to bp0<o0> a0 mi uP + co OlOiOHOJOHn OOOOO ooo H rl H H H H H Ho to 3 CO Of OO cr4 H U 49 rlHO OOO rlHH < EH >P GO H 1 fQ *0 < Eh 5 I 1^ cs--' j H1 <8 a Hg 3|p 3* H r-4 P' p Jr s JS o <M o P ft EjS r |B B to Is -1 ip to w <2^8 ftop *** CflOv 0 49 * EH Eh o P& E*HXC+JmJiHS.I 4 Eh Eh Eh h Eh Eh PAflflflflfl iitIii H JO1 oi pT I I i ^ 49 p s S r c = r pH S P P B B Ph to Hi d lO 49 ri* fi- a U o xs P 49 SI 0W Ho 49 49 ca H 49 S0 0 10 OBJ- to rff CJJ OJ JS "- **0 OJ OJ BC- > CO CM IO OJOJ OJ e-t-f* ftt At Mi CM CM tO OJtOOJ !> 6" t* ItI \CxOtCzOtstot 1II *o r> oo co c m t> io 49 OJ CM CM tO tO to S< COCMCMCMCMCMCMtQ CM CM CM CM OM CM tO I CO to CM CM tO -<# 09 CD OJ OJ 0> B- B-B- !> fc* 88CoOj % woo co 5 ttoo toI toI 53 53 .Wv^ HH OOJ II CO tO BB COiO CO H OJ O OJ CO OO OJ OO rH H rl rl rt CM CM CM CM 1u *H xi C OO cO Eh *$ t?ID <HHS S DUP050069206 o o o rH ft. t a ft ft CQ -d ft CQ ft ft ft ft . CJ ft II II U ifl ra to ft *fO0cOOfOtftH*ffb0Htt1O gt if?! ft E tfinJt II II II II (I o M > * a <5 OJ pH s s, ea; 0 frt * vfcsot .ft .l.l p*ra f*ct*o II ll4 II ll4j CO i> pH1 fCeQ CM ftCtof*t pH rH HH Ji6O-|| coco co co coco H 1 to 0 CO to 00I fat *f0t a oi*! Sbftll ft E-< < H It o-co co to co co JCMCM.pJ,CMHi 'O'O ft ft ra ra^i ft ff<tt3 >ft o oo ooo 1*1 1 * 1 to tO O* ft- to ft. to t- ft* & H rt rl * tO ft* CO 0> CM CO *0 3 *CM CM CM tO tO to CM CM CM CM CM CQ CM OJ OJ 01 CM o <o0> c5o3 tO pH Hto HCO S * & ra tO tO ft so to 0 CO <5> T3 A VS *SH3 -CfOt o o0> &01 t 0J ft ffott tO CO w * fdt <0 <H fartl rt f0t, o 0 <ft V) ft M o a HSi g 0o ft* JO ft 4 VI sft to *c3a HH OO > CM <* o to ft os dffl 0$> ft # H0_ H t? ft ft O A4 1* VI a poH H c 3*<> fOt op H ft e-no ft *C0 0 mffl PH2 ft t0O* Ha tOOJ to 0> rt ft. * tft tCoQ ft 0.0(01 t ft KO K QCQ S H HSOHM rl JW * nt * "* 0e H ft DUP050069207 GP-501-D Data B(i b (i C PP P CO CO CO CO 15(3 49 P (I II II co 4 II II om on w Tpj C- to U3 COW CO 09 o> o> 0 09 p CO cou o CO ( to l to I1 iO l> 03 ^ to 01 C*. Cv IV aS H<a g :5s * PSP- CO to CO CD 0> O d ffl t* P03 03 03 to 03 03 01 rt *> 1co0 t5Q5 CO CO H r-t DUP050069208 DRAFT TUBE CHIT CAPACITY DATA (5 ) 75% o f th e tr a it tim e a v a ila b le in a 500 day year to H Om -HP! B OO^.OIU' 0> CO t> 0 H sit o to t* oto too oo*oto cHm to to P f* a A i--t P H> o 01 S 10ft to Mi tO tli $< J> tO to to to to to tO to Os tO to H PfOrt *d a u 4$ CrP to tO ^ CO tO sji H ,H tO 0) rlNrirl OtO^tO HOrlH 0J H ra ^rl CM--' > fOcWHN HXOI P tf OifO 888888 1CMM< J> i-J tO H A to o to O CO to to M* M* HrI to -wp e& lO tOntOCM tO> <M rl Ml HJ> OS CO 0to* OS Ol J> H r-t tO i--I i--t & } ^ CO t0 01 OH Oodfll C0C0t> 00 01 CM 01 01 H 01 01 tO IIIIII H Ci t-1 J--I E-t CQ CO CQ CO CO PQ 0005 sjtt*c0 co to eo to Hjgfc-tD to 01 to tO 01 H sit ?? ts~jt HO sit to os 00 tfrott to tCOI 0 to to II S080-i ft d P ft P H P XI H H d HH OP o <M 4 to XJ co rl p O Q o p & oH H P< ]i c XI cO P p H O' to H OS H pO 3 o2 u d X! <WI S p a p PI H C Pp fc o e-t P4 * 0Q l o d XI p <1-1 2 o XI p d co p < o P. H p o P H ftl p p o Pp *3 O2 3 P Vt oH d Xl O P o Pa CQ p > td H Pi P O Oa di o rl rl' fc* i P E-* H 0 p d BP rl H PO : H rl P P O t <c Irt #--<* 1--. H CO to Sf \ DUP050069209 0) <P 13 Htc 0O CO to to CO CO P-0Orct lOOOrJNlS * O OO*tO tO tO *2* fr- 60 CO CO to to c h q *oH SH P0 Pu H0 td ft * 0 & HC0 0 to to*to*tooo to to o* o 02 tO tO tO '# 02 ^^5H02 wt -p Uft f0t a- &H o ft 0 H Hu u P tp o fl H0 o H Oc s" aE-t s |p Ho E* U3 tOa CO 02 tO 02 H H O CO H tO lO O tO * .* HHHH & >.* NU H ft >* bO _C &te5 u ft Xi v,0t , M P bQ 02 X CO X0i H WS 1o 02 0 02 CQ 03 * to tO < ft Eh 1W e to u ft ^ 02 02 CO tO 10 9QO0t2 O0.jo2 OO*otj< OO2o> ObOo rltO H 02 02 CO tO Si--t O0o(--2t Oo0to2OoCO00 S ^ * ftH foc,ft p H 1 < fbt ca rl ftl o ft 0P p * o co 02 XI o p cd 03 ootOo o0tQo2 otOHji oOe-oOOooOo<4* o8 02 02 0 Q HHOO rl %" PO 0O P H M O 3 & bcO H 0 0 p bO a a: 02 02 02 02 `I p ap 0 t> ft s r-l & aJr '*'>88SZ o^o oCoD ottoo o0r*5loOtoooO'i* oooo oooo 00 bp 0 SCO <H H W Prl|) ft f{t? fkt o <b s p -p p 3 C H eX*Ix0s O H H s6 3 c=2^ft I tO 02 O H "2t H "tf1 CB C3| CD GOt-CO 02 02 c-otoco Ol ol 02 02 H 02 02 tO I pd fp1dt Cfrat ftoIt fIt pq I m CDttoitlo lCO E0-i f0t 0JS E0-i 02 tO 4* (6 ) Based- upon s in g le sem i-w orks d r a f t tube b a tch * (6) Based e n tire ly upon batch data* Never trie d in d r a ft tube u n it (7) Includes GT-710-D. DUP050069210  1r+l3: Em p CO cuu Et CM lara & t ,n* nt* 01 H H O 0101 *j i HH O OJ & 0 sH rl H tO H 1 < <Ehrl p tOoJ w cECHO Eh <s O +3|tPO O 0> t0* OJ to to to O lO to p rwa ffet: ata & a aa , A "" i tEo5 i to *w 0 d h CO & UA 0o 0 Ei P PM 03 Qw ,0 c c H OOP QOO 01 <!l> CO H . CO JO H 88 W 01 H pH r~4 ooa 99 00W00 H^IOK0J0 99 <I> HO CEIOH ftOtI P P 0o TC<h ra A P tCaO P S P a 0m Sai. H> pc M fFtt U0 P no i--I H o Ppt +3 P *0 c T3 5fl THoO no o ft t>> pH g mH *b H P ft GP A p n3 EH c o O -P p co ** % r-4 oa. to DUP050069211 03 A "H o (3 -p K to to tO N HHciWlOW <0 rt <0 00 01-*# W ft ft sr H 8) o CO H CO to to o w 0> CO *# 01 0) 015? HH 8 ft Eh >>{>>>> > * * >>!>!> ta w p ra w w to W WWW 3, <; tf -P poi ooi o35 o*H o*t*oto 00 03 H HHH qco 01 8 000 01 "si* WWrIH Eh a & C: P B P tt ta g S Aw H a tO tP OOIO to 01 to<st> H C- N CO Ol e' to E-tO ^i H W rt W en pH r-t 03 fcx. a o " "t}* to to to RH u tO *H<D 01 ^ a ca t ftto ja t -P ft ft w ftoo tt e c s p H OQ O O O O O tD Q O O O OOlOl *p>0 rtrltOH tO = O 8 e b ss OQ O O Soi8 H H H U) 3 Tl p s 'S to to ft ft fot tft ft to <rl <4-1 <2 Eh H TABLE X I I (2 ) See T able *? *? 9 *? *? 9 I Hit s* co to 01 o p 1 c- (jtjai? sPOH^ ol O CO CO t> CO 01 C- HO tO o| CO 01 01 H 01 Ol tO fc (OlO ol 111 til I II I I fwl fwlt(Cl fCrQi |wj Hto Eh EH Eift ^ POOP DUP050069212 J, 0*1 s s c e e Ct, s ft K Wes ao H Oft ft ft ft ft 03 'S ft 03 ft O-SP^.P^PiSP'S? rjr) W H rl W rl ft ft ft ft P^O^O,CO rlH H H o oo o o OOOO < o to kft pQ fc- ke OO e* k H r-t H rHi-4 otO ob- o ofc <k rlrlrlH lO MH B Sol-3t H 03 r4 03 r- r4 03 H 03 03 J3 fNrst < I C 6-t a: O IO CO H OO Q COft H QO to ^H OOOO too O to H to H 'S* H o. u(H-33 ss ^ !* CD sJ' CO sP 03 03 H 03 03 H 03 sH 5? CO 8 4cfBt Uo a <oH to rt CO n n A n ^ ^i i p^i r?i r i i i i(~'i) I ^i^i Wi Oi Qi Oi biOS O ffl fc 03 0> I CO 03 03 r4 03 03 03 (3 Einft3i ii4 at t i-i3 i Ei j S *?<?*? 9 *3*0 H EtoIviJH> Oin 1ioI0 &&*a OO O O DUP050069213 VAT 240^39C APPENDIX II 6 CODES U A f?rt A ...if3* K-l GOALS_______ ______SIZEl- BIAZO VAT: COUPLIPG VATl STRIKE VAT s. W/ TS /\ Approved By: EK: 5-24-50 -wru^w SAME: "MONASTRAL" GREEN , NInstructionsjuse Lbs} Codj Acot, Lbs --4*^i ft*JEtaaSSSSISS-- -6--_3i -S----t-a----r-t- ---c---i-r- *c-tWuWWlaW^tWiftoj n..... . vat S90''lLRiaBoF*saF an circulate vat 240 10 mins. or long iL>Jis&g&Ajg^^ agitation M. 65C *'>S9C ` adsjga-tligaiL 11'. Stir drum of prenared ertmlslon and vat.240 through chute,__viatch,,foam... lg.i|IiMn|Wj:^tJoITOWWWMW' 12. Stir at 190 -195 for 90 mins. v;jth40 GPM oAx*oxxXsvXony^^y?AtcH fosuft Kcox^oTj uxino stJ&i*** ____ `telgh and add in 4-6 mlnu 14. Continue circulation for fvV^esww TCTairvarm MMHa W jt9'rn,ud^gir 'aacryjssorgi ^7TiOTS1^52T 21. Press with agita^onT~^""^w'' --BTJ`IW--tfSwirra~yjPrJr.W*- ........... ttmimm nrii . k i jiu,, ~r DUP050069214 - 27 - ? AT-674-D Process* -Goal; 1 Ofinif , Date < t t a s-pd-an rftyTVG ARP a wnnrre t v *. s_q..*yv 'RfimarVs PRESSING AREA INSTRUCTIONS PRESSING AREA NOTES Vat MSB, JEiia. 240 Describe vour yield ;KvS(KB,* Recovery conditions ^alg&ssaJaL .toaaJiSLi *SAJ: '*r>aJaWW* -wE^fe*wX9 saamm. P^aafl-jaj-tbT ,n---------a?1 tatl on------_- Wash to DO NOT WASH Ohms Honrs washed MalceflrsEtesFafteF ftr s Ohms jjoah on & oars ^ ___ jfoyer carsaotuiur^Dy pulp containers SpeolLaT,l'YnstruoWonT NW^USFSfS'G .<>Ull Win IwWWMfCTgMiMWIWWPWWWPWBW^MIWW^MBM> Notes on soecOri ihstrnctlons 7HFmpr^MSp^W^ir^BFr"* ing washing in toafolcrexce s s Ive use orwash water Deliver to GRINDING AREA INSTRUCTIONS Scla&ssJ&u M 'S'fimhl'es' 1 2 GRINDING AREA NOTES Contaminated,with Remarks -Uis l . - -.-......-............ T....... - , . . . V1 . . .,.......... Deliver to Control tabdratory Sampled by Do not mix before sampling Date m3xed Packaging See IJhart 1 ?uaiity remarks ^aa5-^ldit,,jihaGk-___Z~________ _ DUP050069215 STANDARD PSHSMU!A NOTES Til (D) process replaces the previous (G) formula, and differs from it as follows* 1, Batch size has been increased from 4,'j O# to 1260#. 2. The material is processed thru the draft tut unit (Vat 390) rather than in the Abbe Lehart mixer. 3. Recirculation time has teen increased to 120 minutes (see special notes). 4. The quantity of N-666 (TEA-Cio ester) has teen increased from 1% to 2#. 6, To match standard GT-S74-D using current N-624 made from Orohem crude, 2# N-657 is added. The grinding and testing remain unchanged. Processing g t -674-d in the draft tube unit was justified upon a labor and testing savings resulting from the increased batch size possible in this unit. No quality advantages are claimed how ever, there are indications that some strength improvement is ac complished. CALCULATED COMPOSITION GOAL YIELD CPC Toner Blanc Pixe 1200 lbs. 95# 60 a 5 imrmximi SPECIAL NOTES 1260 lbs. was Is" 1260 lbs. anhydrous moisture - nil Refs See calculated composition The following items remain f or further study, 1. If the motor on Vat 240 is changed from the present 7-1/2 lbs. to a size capable of handling a full vat of color, the batch size can be increased to 1640 lbs. (3000 gal. final volume). 2. If the batch size is increased to 1640 lbs., the recirculation time can remain the same (120 min.). 3. There is evidence to indicate the 120 minute recirculation time is longer than necessary. It is quite likely that for the 1260 lb. batch size a 60 minute recirculation cycle would be adequate, pro vided the pumping rate does not drop below 40 GPM. DUP050069216 - 29 - 4. High temperature drying (200P) has been found by Chemical Div ision end Quality Control tests to cause no color degradation* This higher temperature drying reduces the drying cycle by 50$. EFKsoc Signed E. F, KLENRE - 5/24/50 H. ARHOTJL - 5/24/50 DUP050069217 29--A -- (A) GT-710-D FORMULA NOTES This process was developed primarily to produce a "Monastral" green toner with better dispersibility in vinyl plastics than GT-674-D (D). Material produced by this process is unsuited for ink or paint use (see GT-674-D (B) notes), being weaker and duller than GT-674-D standard. Essentially the process is identical to the BT-284-D (0) formula, being a 10$ 0C14 treatment of a 10$ pignut slurry In the plant draft tube unit. The treated slurry is pan dried and high speed pulverized. SPECIAL NOTES The following items remain for further study - 1. The batch size may possibly be Increased to 2400 lbs. (2900 gal* final vol. at 10$ slurry concentration). 2. If batch size increases are made, the following recirculation time to batch size ratios should be maintained until sufficient quality data have been accumulated to indicate a change. 1200 lbs. - 1500 gal* - 90 minutes reciro. at 40 GPM minimum. 1600 lbs. - 2000 gal. -110 n o i 2400 lbs. - 2900 gal. -160 0 " "" a CALCULATED COMPOSITION CPC Toner-1200 lbs, 100$ GOAL YIELD 1200 lbs, "as is" 1200 lbs. anhydrous Moi sture 2 nil Reference: See calc. comp. EFKsCC Signed E, P. Klenke - 6/9/SO Approved g, Arnoul - 6/12/50 DUP050069218 DUP050069219 - 31 - BT-284-P CP.) .1260# 4 V HAs 5-17-50 mv ii"' JES: 5-25-50 fai '240 '' 'rjee^WSSJ* -* >.>, ! -->>! ?| J** f :| X* > : i ' 1 b: fulfil* ! Ii^,> h-SC. &/ rrf-s.? %, , . _______ : .............i j .: "t < ' -. jv^s s ^.:tt...PPfl H t. -_ V - . =^.. .... '* Ag5i; ni ;n " ] . ................................................... Of 1 . & j; ' W . HfS- . ;! ! j.rjib On 15 pars- see other side, i , : JilJi io;n3.,M0M-BLEE01IC5. , , `l Must, not.contaminate with iron jj ' '...... ........... P...... ' 'blue. '" <- -V. .. > t... . . . .7 iv 1 ".. .., b'v/Vr V P-Ma^r 0-v; .bp'"-' ill "&`:r*. ;. v 24 ' 220 i<}$ tUicnim X,J ^i i* .. 16 ' . 220 ,:.T.,7b 7 7b . 1 -.slU '*wo .css M&: . : H*.!Bf I20TI3 > si tii * ... ! ' . \*n>p ' See' Chart. '`'f 111 .... ......................................... Must not contaminate with ..iron ..bliiei7 ., Sprap.e pans.,,,,. jfc.. e:i3 ' "f :ggg)''; <^3., S|'.. ti ' fib* . .!**<** V"'.** >1 ......... ...~" (k -i___ Giiamg jjri listRtiiitcss4 <lr',,nd.f;7 L,S.P. . i mk mm >*1tm - OS - U s't - iVitts - CotJ!SJj**i*ti. *1U ,,J I..' Must/contarninate '-with'iron blue. V ('npt'*r.b.b zrbbTM.i. b',,ir, ~v Crt -11 ** ' ' ' ' 'I'" i* ______ 1 jr/ .-------'----- - To Control Laboratory. jl : .-->-... ................ Cb' Ho? 'IKx'l^TbriT BiiipF::nj - --.s 4^*." .a*..... a. ... *. ''.** -- Jis '.Ht* By -I-' *. .-..See Chart* DUP050069220 32 1. Agitate vat 240 for 3 minutes just prior to pen loading. 2. Stop agitator. 3. Immediately pan load to an even depth of 3/4", thru 1/8 screen. 4. Place each ear in dryer; sirat steam and fan within 1 hour after the oar has been filled. 5. Wash down vat sides using a one inch hose nozzle for maximum of 2 minutes (approx. 12 gals. ), 6. Collect washings in SO gallon drum provided for Ahh Lenart or Vat 240 codes. 7. Nofity making supervisor as soon as mixer is emptied. 8. Pan load washings from SO gallon drum using dipper. Note? If the same code is to he made again immediately fol lowing this hatch, omit steps 5, 3, and 7 and 8. Check with making area Croup Supervisor during step DUP050069221 - &3 - BT-284-P (C) STANDARD FORMULA NOTES The (c) process replaces the previous (B) formula, Tii (0) formula is written for the draft tub process and differs from the (B) formula as followss 1, Tb batob size has been increased from 400# to 1260#{see special notes}* 2, The material is processed thru the draft tube {Vat 390) rattier than in the Abb Lenart mixer. 3, To compensate for the increase in strength over the Abb! product 5$ Blanc Fix is added to the toner during the recirculation cycle, 4., Prying times have been r educed 50$ by increasing the temperature of drying from 140F to 2S0F. 5, There is no change in the number of dryer cars required per pound of color. Grinding and testing remain the same. Processing BT-284-D in the draft tube unit rather than in the Abbe Lenart mixer was justified in the basis of the 5$ increase in strength inherent in the draft tube process, and on the basis of the increased batch size possible in the unit, which affords considerable savings, SPECIAL NOTES The following items remain for further study - 1, If the Vat 240 motor is replaced with a larger one, the batch size may be increased to 2436# (2900 gal, final vol. at 10$ slurry con centration). 2, Jf the batch size is increased the following recirculation time to batch size ratios should be maintained until sufficient quality data has been accumulated to indicate a changes 1260 lbs, - 1500 gal, - 60 min. recire. at 40 GPM minimum 1680 lbs. - 2000 gal. - 90 * n n it n 2436 lbs. - 2900 gal, -120 * * * * n 3. it Is quite possible that the slurry concentration can be increased somewhat without causing serious quality degradationj however, the effect on agitator load mus t be watched carefully. 4. It is also possible that the amount of treating agent (CC14) can be reduced to5$ without causing loss of texture or adversely af fecting ink mill behavior. Ho experimental data are available at this time to confirm this. CALCULATED COMPOSITION CPC Toner 1200# Blanc Fixe 60 95$ 6_ GOAL YIELD 1260# "as is* 1260# anhydrous Moisturei nil Reference* See Calc, comp* EFKsCC Signed Approved DUP050069222 - 34 APPENDIX Vf Opst Group JUvts-L'jt'-M ALT. BL-288-I) .. -<K (1) Bl&ZQ GC9PL(S3- ..._________________ ..I" """`"'I,,, 10: 6-7-50 ts 6-7-50 IS 6-9-50 / ,AftS M EtK'fc X ,. I (3182) Std, Hours__ __. j o K-BIOTIKGa rs!tnf imt a m 390-240 2 1,1*JEM^ ,2Q0,0 . B-*1 .M^ mesi _AccisiLjiLs^ .^jlBEPy. .iCTtlJLp.Xfciujk&CL,HroJ?j s l 45. bglpw., the_] ...top .of, tto..tofcJnfltft>j s M. 4^tl^4ymJ^.2.3 ,&_j ^a^allflaJlsBe!Lfii. W-623 and N-567 Have teen added. ___....... _,... .^___ 75 Wash ITdrms wltlTwatpr.' '. i 8. Start vat 240 agitator. ~~T' f 9. Stir and circulate vat 240 10 minutes or longer r *' thru draft tube' maintaining'vat "'s"`"-*` from iilsc. TIP. Weigh and hoId""at "vat 390-240 sift into vat 390 in Www.i)'i'if > jLi^ sl^QP JQ 'r?r.----.-- >!-< _, 25-35 minutes H-19 -- ' ^*.***--* *+* ' ' 'MW--Ifr .rL...._ _. ...* ...._ . Kim-tt, u mi.. }i i "ir ***1 .-.s-w-- tr if tafcvNKt M'^'reW!i5riren^rwergET6^ water into 50 gallon drum. fij."Weigh and pour in M 115 r Heat to 128-i32F ` |l6rWeigh and_BouxCin_I___ 'JJZ,^,.,Stlr.^5-miftutLaa-J:Q .jaolriU^m x~ .-GY--, m.us.t-J?,e..^^If- 119 Weigh and pour in 120, Stir B-lO^minute s 121. Repeat s ................. "`.w.mi * ' Ion drum _ to smooth Coated oa DUP050069223 m * DUP050069224 - 36 - it, .21 ji j.ft& BL-288-P ALT 3179# (1) * HAS 6-7-50 T ftft} -; f ift fty JRG 6-20-J ' fcftftTC Kftsy 240 sort; ft i.y To,.;- ` ft:" Tftft. lftft : sr- fto-ft;ft 1?' *$'*? %y.J: >'..r ''ftjft: 91 140 .r. ..>-:ft. ;. *.v':< ft:?-1 ''"'K \ - ft T''"IX) NOT WASH .;; , i! / fmd &" loi : ft:? 4 oars ft S :; ' ft;yft> , :* ft : _i; A ^ _ ftk :: f#;x:; ;4v yft fttft, NON-BLEEDIHG '1 > _ 'ftftys -ft ftftft. f/t;. f,t * t T bBi :,o ...ft.... ft.|; -ft' f ft. .... ... ': ftft-Cift. " ft'.'. \ .'ft ft',.!; "ft ft" ft'...ftftYft" fftr-wr !r\.v. ?,, .h ,ft, ift: s;t*..24 _ '.'`eKjft iso.. ; fty'-ft.*''' 24 ' 180 ... !) i ft>;<:,, fjotiss ; t, -sp ft\ _ _ #\'i, * v'4 *v .........S....c...r..a...p....e.....p....a...n...s...... . .. . .. H>- , % ;*vpp ft}n*u?.-:r s q Chart. 'J' T-ftft, -ft . ;........ . .. ............. yft.-ft yr `ft,,......... ....................... cuii*o a k a :j x '; ... ft >ift "ft ^ Oy-, i .ft ;'* it r ft.ftft-ft -V I* 7;' ' 'aft :: ? .tcnc . rea mms ?ft2 envelopes . +.?ft.> f-t:f;'t:-';t?r.X ft ft i:er'....... - ft ---- ); ......'Tr ' To Control Laboratory *' r`h.'-Wtax r. te.i-s.-i.f.g.-<;!..JAfWrt.g.... . '. .V See Chart. F i. i wxisd . .................... ..... ............ ........... . Rafts . . . . .......... . w,ww-*-------- ----- -- . ^ DUP050069225 - 37 gdgggBLJUU. STANDARD FORMULA MOTES The "IR process does not replace any previous standard for mula* It Has beer established as an alternate formula for manufacture in vats 240 and 390 when the #2 Abbe Lenart is not available. This process requires filtration of the slurry in order to avoid the use of a large number of dryer cars which would reduce the Dry Room capacity. After more experience has been gained, it is planned to study the effect on strength of pan loading versus pressing. An advantage of this process is that the CPC is all passed thru a 60 mesh screen. This should eliminate or reduce streaking in pale shades of linoleum. All material ratios are based on the "H" process; the weights have been doubled. The resinous oil Is also emulsified in the same manner as in this process. The following calculation composition is copied from the BL-288-D (H) formula and applies. The goal yield has been doubled on the basis of batch size. CALCULATED COMPOSITION Lbs. CPC LB M -"ror- Treating Agent* 134 Whiting** 2196 $ W 4.23 69.27 lOCMScpf GOAL YIELD 3170# "as is* 3170# anhydrous Moistures Nil References 1313-37 and BL-288-D (Q) ^Assume 85$ retention of treating agent, **Assume 0,15$ moisture in whiting. Additional information and variables can be obtained byreferring to the BL-S88-D (E) formula notes. LG S CO Signed. Approved LL E. ARKODL - 6/7/50 j, H. POPPER - 6/9/50 DUP050069226 - ss - W.o$KS D&z^r Tur Un i?- /AX./S* DUP050069227 DUP050069228 (Ref. 1) - 40 GGi E. P. Klenke A. A. Brlszolara NEWARK, HEW JERSET DECEMBER 8, 1960 DR. J, H. COOPER GT-674-D QUALITY I -understand that the quality of CPC green from Newport (N-624) has been poor lately, and that variables have been employed in the GT-674-D prosesa here at Newark in an attempt to improve the material, in that connection, X would like to make a suggestion based upon some recollections of my past work on GT-674-D. At that time I noticed that when the N-624 was sub-standard (weak and/or dull), the GT-674-D made from it would sometimes show a tinctorial improvement. This occurred primarily in those oases where the pH of the normally alkaline Newport pulp (pH 8-10) had been adjusted in the vat with hydrochloric acid to the range 6-6, prior to the heating and ester-emulsion addition steps. The pH adjustment step was written into the original GT-674-D formulas (B and C) in order to facilitate pressing. Al kaline CPC pastes are very thixotropic and consequently resist pressing and yield thin, soupy presscakes, An acidic slurry, how ever, will press without difficulty. When the (D) formula for the draft tub unit was written, the acidification step was believed unnecessary and omitted, I suggest that trials in the plant draft tube unit be made, to determine whether quality improvements can be realized With sub-standard N-624 when the soft powder treatment is carried out on an acidic slurry. The effect can be determined by rubouts of the finished GT-S74-D lump versus a sample of the untreated N-624. Because GT-674-D at present is reported to be erratic in pressing behavior, batches made on the revised process should be followed through the pressing stage, if the expected improve ment in pressing behavior Is realized, it may be possible to use fewer frames and decrease pressing time. MBVjCC M, B. VER NOOY CHEMICAL DIVISION DUP050069229 (Ref* 2) - 41 CC Messrs* R* A, Kaiser, Wilm, J. E. Booge, M J. 1. Bailey, Nwk. V* Chalupski, B C. D, Atkinson," H. Amoul, " C. W, Oskins, Nwk. J. deL. Moomaw, * A. J. Hughes, " D, B, Killian, " A. Siegel, n L. B. Magruder, " Newark, New Jersey May 10, 1950 DR. J, H, COOPER, NEWARK "MOMASTRAD" BLOE AND OREM DRAFT TUBE STtJDY This letter is intended to review the original objectives of the draft tube study and to summarize the results to date of the plant development program. Such a summary Is desirable, since the plant program was conducted at a rapid pace more consistent with production than development requirements. As a result, some Con fusion may have arisen and some incorrect conclusions possibly drawn. ORIGIN; Installation of the plant draft tube unit was originally justified on the basis of the following; 1, BT-284-D Semi-works data predicted a 5% Increase In strength and greater intensity over standard Abbe Lenart processed material. No Improvement in texture was claimed or predicted. Savings were predicted on the basis of dilution with blanc fixe to compensate for the increased strength* An increase in batch size from 400 lbs. (Abbe batch size) to 1200 lbs, was forecast, the size being dictated by capacity of the dryers and not by that of the draft tube unit per ee* 2. GT-674-D An increase in batch size from 4 ;0 lbs* to 1200 lbs. was forecast for the plant unit, thereby affording labor, processing, testing, etc. savings, calculated at $7.26/100 lbs. No quality improvements were claimed. Here too the 1200 lbs. batch size was selseted largely because of limited dryer and press capacity. 3. BL-288-D This code was included in the project for further develop ment work since a few mis on a semi-works scale indicated better DUP050069230 42 dry lump uniformity than by standard Abb& Lenarb production, thereby reducing re-mix and testing costs. In addition, there was some indication that greater strength might be obtained. No definite claims were made for this code, since development data were limited, RESULTS: Development work started In the plant draft tube unit as soon as it was available (April 4, 1950). The results of the 16 CPC development batches made to date indicate that the performance of the unit has actually exceeded expectation. Furthermore, the ex perience to date indicates that, with some additional modifications, appreciably larger batches can be processed thru the unit with possible attending economic advantages. The following is a summary of plant experience to date* ) 1, BT-284-P The first draft tube batch was Intense in -tint and 6# stronger than a control batch made in the Abb& Lenart mixer (using identical raw materials). The batch also was 1200 lbs., as compared with the standard 400 lbs, in the Abbl. Subsequently, 8 successive batches were made in the D.T. unit with Z% blans fixe added before panning out. The resulting products were in variably equal to or slightly stronger than standard, and all were on the intense side in tint*. 5 No operating difficulties were encountered and the number of dryer oars required per pound of color was actually somewhat lower than for standard Abbe processed material,. 2. QT-674-P*BM This code was actually the first batch to be processed in the plant draft tube unit, a decision dictated by the need for improved material to fill an open order from Hasland. The process differs from the conventional GT-674-P in that only the CCl* treat ment is used and ths product is high speed pulverized. Prior draft tube development work was restricted tome semi-works run. Where it was established that the material produced was superior to standard GT-674-P for vinyl dispersion. Despite the lack of com plete operating data, the plant batch was fully equal in all proper ties to the semi-works standard. 3. GT-674-P To date 4 draft tube batches have been made (1200 lbs, each) with no operating difficulties encountered. Evaluation of the first batch indicated it to ho 5% strong versus standard (lot 451) and *0ne 1650 lb, batch was made (4 x Ab'o& size batch) with no deter ioration of quality. All draft tube hatches ware equal to standard in ink mill behavior and texture. DUP050069231 - 43 - possibly Si trace better in printing ink properties. Subsequent batches were made with 5# extender added. However, ink mill tests indicated a 2-5# strength advantage still remained, with the same slight superiority in ink mill properties. This quality improvement exceeds expectations. Since this code has always been pressed, there was no change in the dryer capacity per unit of color, 4. BL-288-P To date only two batches have been made in the plant draft tube unit. One 1585 lbs, (equal to an Abbe batch) and one 3100 lbs. Although complete evaluations are not available as yet, those that are can beieported as follows. The first batch was 8-10# stronger than standard by Armstrong rubout test, and 20# stronger by Sloan-Blabon test. In dry appearance the draft tube product was completely uniform and required no remixing (remixing is required on most Abb! batches). Despite considerable difficulty in pumping and screening (60 mesh) the heavy slurry (+25# solids), the large 3100 lbs, batch was scheduled to provide operating and quality data. The latter are not yet available. However, in view of the serious pumping problem, it was recommended that further production of BL-288-D in the draft tube unit be delayed until more suitable pumping and screening facilities can be provided. The two draft tube batches used precisely the number of dryer cars predicted from the limited semi-works study? i,e, a significant increase on a unit color weight basis compared with a standard Abb! batch. This was expected, since one of the features of the draft tube process, by which the improvement in dry uniformity and ultimate strength are obtained, is to use heat development which causes an Increase in volume and wfluffiness". In an effort to re duce the demand on dryer car facilities, a portion of the 3100 lbs, batch was pressed before drying. By the Armstrong rubout test the pressed material was fully equal to standard BL-288-D in strength, but weaker than the Counterpart which had been pan dried without pressing. In sumaary, it can be said that sufficient evidence has been accumulated from production of BT-284-D, GT-674~D and GT-674-D*HM in the plant draft tube unit to demonstrate that this unit has at least fulfilled expectations, and is completely satisfactory for use in the regular production of these codes. EPKsRMK E. F. KLEHKE, CHEMICAL DIVISION DUP050069232