Document npK7Y0eQGp4E44Gewvxx43EK6

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Copy No. 1 Numerical File V / * Period Covered: NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report DIRECT LAKINQ PROCEDURE FOR RE-85-P (SCARLET 2R LAKE) APRIL, 1946 through JULY, 1946 FILE: DATE, 222=42 ^8/21/46 N39972 Serial Ho. KN-46-58 Copy Ho* i Copy Sot #1 - Sumerleal File 2 - Research Office (222.42) 3 - Library File (222.42) 4 - #10 Building File j-# 6 " 6 - Imperial Chemical Industilea, Ltd. 7 . if n it 8 _ H II 9 - W. F. Spengeman, Newark 10 - Extra NEWARK PLANS PIGMENT COLOR RESEARCH REPORT Final Report DIRECT LAKING PROCEDURE FOR RE-85-D (SCARLET 2R LAKE) APRILf 1946 through JULY) 1946. SUBMITTED BYt APPROVED BYi F. K. SLchnee F.K-, A. D. Reidinger 0^76^ * DATE SUBMITTED t 8/2/46 DATE ISSUED* 8/21/46 N39972.01 DUP050150177 i - imQiromit For many years RE-85-D (the hydrated lake of the barium pigment of Scarlet 2R) has been sold to the F&F Dept, at Newburgh as a pigment to be used In coloring various fabrikoids. The appearance on the market of two competitive productst Imperial's Soarlet Lake B-9072 and Calco's Scarlet Lake C-48875 aroused some concern as they were quoted at 35# a pound, the price of RE-85-D, but were two and one-half times stronger than RE-85-D. The one drawback of these products was their alcohol bleed which indicated that they would exhibit ,,cracklng,, in fabrikoids. At any rate, the appearance of these lakes on the market brought up controversy over the RB-85-D pigment. Either the strength of RE-85-D would have to be brought up without an increase in cost or the cost of RE-85-D (strength remaining constant) would have to be reduced to keep it as an attractive product. The only thing that seemed plausible at the moment was the preparation of Scarlet 2R dye at Newark instead of the purchase of it from Calco. ii - smsmisasL* RL-IO-D (an obsolete process for the preparation of the hydrated lake of Scarlet 2R) was used es a basis for experimentation because it was slightly stronger than the competive samples. A Scarlet 2R dye was prepared in the laboratory and laked according to the L-10-D procedure. A product approximately equal to the competitors' samples was prepared) the ingredients cost of which was 27# a pound. This attack on the problem was dropped as there seemed to be an immediate usefulness for the dye - direct laking of RE-85-D. The tinctorial properties of the direct-laked RE-85-D were so close to the original that the possibility of preparing a cheap pigment was immediately detected. After the completion of very little work on RE-S5-D, a plant formula was set up for costing. Since RE-85-D is such a weak lake, the charge of the dye would have to be very small for a regular 1000 pound batch of pigment. In fact no plant vats were small enough to accommodate such a charge, so it was increased five times or to a one mole coupling. This called for an unavailable 20t000 gallon vat for laking so it was decided that the dye be split and laked in two 10,000 gallon vats. The increase in batch size meant a greater reduction in cost. The original process which called for a 20,000 gallon vat was coded K-2332. Due to vet tie-up on K-2332, it was decided to Increase batch size of HE-85-D five times (coded K-2348) and compare cost to K-2332. The following is a tabulation of costs* DUP050150178 - 2- EsEfflBla K-9940 Goal Yield 1001 Cost Yield 1001 laSk 13.32 S*t 19*20 25.54 iaxiasa - (Std. formula using purchased dye) K-2348 5015 4940 13.25 (5 X Std. formula using purchased dye) 17*43 22.68 2.86 K-2332 5280 5217 10*21 13.36 17.11 8.43 (Direct-laking formula based on original lab* yield) K-2332 5280 4940 10.78 14.11 18.34 7.20 (Direct-laking formula costed on same yield as K-2348) From the above costs It Is evident that the direct laking formula K-2332 is more eoonomioal resulting in savings of $7*20 $8.43/100 lbs* over standard RE-85-D compared to $2*86/100 lbs* for K-2348. Two semi-works batches and four plant batches have been made to date. The plant batches had to be split for laking, thus, resulting in eight lots of finished products* Since the first plant batch was lighter in masstone than RE-85-D, varied amounts of Azo Bordeaux were added during preparation of the other batches. Two of the lots turned out to be O.K* straight while three were too light in masstone and three too dark* Mixes were made of various lots of the plant material and two, Mix 6 and Mix 11, were deemed sufficiently desirable to have evaluated by Sales Service and one chosen as a possible standard replacement for RE-85-D. Mix 6, a combination of equal parts of sevSn lota of plant material, was considered the best and has been submitted to Hamburgh for approval* K-2332 has been superseded by K-2375 which differs from the original in two respects* (1) addition of Azo Bordeaux, an average of the amount used in the seven batches comprising Mix 6; (2) the use of two 10,000 gallon vats. K-2348 ustog purchased dye has been superseded by K-238O which differs from the original in batch size, being one-half the former. K-2375 and X-238O have been submitted for costing* DUP050150179 -3- III - DISCUSSIOH OF BgggMSl ' Very few variables were run on the direct-laklng procedure* Results on those tried are as follows! 1. Increasing the .concentration for dissolving the dye is undesirable because the resulting product is weak. This may be due to incomplete solution of the dye* 2. Increasing the volume of coupling Increases the bluensss mors than is desirable* 3* The slight Increase in strength obtained from the use of meta xylidlne over mixed xylldine does not compensate for the increase in cost. 4. The trial runs on lots of R-Salt and mixed xylldine from the semi-works and plant showed they were O.K* substitutes for materials used in the laboratory. However, this does not necessarily hold for lots purchased in the future. 5. In finishing off plant slurries it was found that the final washing and the addition of dry barium chloride could be omitted without harm to the tinctorial properties and without an Increase in alcohol bleed. The following data on the plant batches is of interests LafcJL M.T. Str. Tint Yield 33904 33905 33978 33979 34036 34037 34038 34039 It., brt. It., brt* O.K. 2% wk. vs It., vs brt* 4# str. dk., s.brt. 5# str. dk. 3# str. dk. ws str. It., brt. 6% wk. ws dk. OK clean vs worse 2522 clean, OK (s.yel) 2465 vs blue clean,s.blue vs worse(yel)l324 blue vs worse 2538 blue vs worse 2594 blue,clean ws worse 2382 blue OK (yelm) 2612 e.blue ws worse(yel) 2696 The average yield on the plant lots la 4908 lbs. However, the yield on lot 33978 is abnormally low and cannot be accounted for* Lot 34039 and lot 33978 are O.K* Straight. Mix 6 (possible standard replacement for RE-85-D) consists of equal mixes of seven lots, lot 33979 having been omitted. Mix 6 Is very slightly light in masstone, very slightly blue in tint, and about 2-1/2# strong versus RE-85-D. When strength Is adjusted tints appear almost equal. In alcohol bleed Mix 6 is no worse than RE-85-Dj it is merely more yellow. The laboratory goal yield was 5229 lbs. "as is" and 5020 lbs. anhydrous. DUP050150180 - 4- iv. Experiments recorded in Notebook 1202. Expt. II - Orientation 13 - Variation of concentration for dissolving dye* 16 - Use of raeta xylidine. 17 - Data on G#, RE-8 ?-D, experimental . 1$ - Variation of volume for coupling* 19 - R-Salt & xylidine from semi-works 20 - R-Salt & xylidine from plant* 21 - Methods of finishing off plant slurry* 22 - Data on plant batches. 24 - Goal yield on K-237J. v. Notebook 1202. Letter of J.B*Callaway to Messrs. Dawson and Siegel, 4/16/46 - Calco ScarletLake C-48875 Letter of A.AeBrlezolara to Mr. Siegel on 7/22/4$ - Scarlet LakeBE-35^n DUP050150181 COLOR CODEBate 7/23/46 -Scarlet Lake5-3375 , . ,, OBJECT* Dlract-laked RS-35-P tyoe i?.iga.eBt.>---------------------------------------------------------- BASED om Plant trialBQfK-2332. toH SIZE MOLS.: IlIO-------------------------------------------------------------------------------------------------- Lbs*or Wt. Oas. MaterialIQSl_______________ MU------------------ ftaAPtt,lfl.USB--------------------- Wl mm 1350 lee 109 Muriatic Acid (+31.5J8 HC1 sol'n) 121 Mixed Xylldines 75 Sodium nitrite (99.7# NaH02) Dump into Vat 301 and make to 57 5* with water. Add 109 Stir 2-6 minutes. 28 Add 121 Stir 4-6 minutes* Temperature 530 should be 22-24op. (xs of Ice) Add In 9-11 min. maintaining temperature at 22-24F. dissolved in 5 60 cold water in a drum. Stir 14-16 min. Test must be +CR, +KI. Record KI 1 CR 248 Final volume 12" in Vat 301. - - - S.ouple_at once. b -s a l t s o l u t io n 91 Caustic Soda (+50^ NaOH soln) 366 R-Salt, 100$* (50# R-Salt paste) +450 Ice 366 720 Run 15 inches water into Vat 300. Add with agitation* Then Add 7 Stir to solution in 25-35 minutes. Make volume to 20 inches in Vat 300 at 60-62F. using 125 57 Couple diazo into the R-Salt solution (H-12$) under surface thru a distributor in 45-60 min* Maintain temp. In coupling vat at 60-65F. Stir 30 min. (Tests* must be -diazo and -t-R-Salt! pH should be 10*5-11.0 . R-Salt PH .. - 8 Azo Bordeaux 750 Sodium Sulfate 3060 4080 Run contents of Vat 300 into Vat 200. Dilute to 45 inches in Vat 200. Heat to 17&-l82F. Add dry to dye solution and 47 Stir 10-15 min. to dissolve , 108 the contents, of Vat 200 to is* aDOve dye soln. into the following previously prepared base rapidly as possible (25-35 minutes) DUP050150182 2 Lias* or 100$ Qms.Material_________Ms. Sai*MMLtoB3#&taa-----;---------- EJL 1125 Alvua, +107$ 513 Soda Ash, "as is" 2250 Barium chloride, "as is" 250 Barium Chloride "As Is" 1125 450 2688 513 432 6432 2250 1491 9216 Dissolve and adjust to 25" in Vat 321 at 178-182F 15 Run to strike Vat 105 end make to 28 inches* Add in 19-21 minutes dissolved and adjusted to 3 24 inches in Vat 321 at 178-18207. Stir base 55-85 minutes. Stop agitator until base is needed. Record (Normal pH 5*8-6.4) Adjust the dye-base to 6?" in Vat 105 at 124 - 126F. Strike in 9-11 minutes with dissolved and adjust to 16 21" in Vat 206 at 124-126F. Stir struck slurry 10 min. Record pH (Normal8 3*8-4.4) Test bleed# Record _____ (must be negative). Flood to 96" in Vat 105. Draw 2 waters down to 48" Vat 105 or lower (estimated time)# 5 hrs. and 12 hrs. respectively). Flood to 96". Add dry 16 Stir 10 min* Press, dry and grind as specified in the processing data sheet. 1125 513 2250 250 Alum, +10758 Soda Ash, "as is" Barium Chloride,"as is" Barium Chloride,"as is" Repeat as above with second half of dye using strike Vat 106 and consuming ' 15 3 16 16 Barium salt of Scarlet 2R 11.1$ Alumina hydrate 14.7$ BaS04 from alum 46.0$ BaS04 from Na2&04 24.0$ Moisture 4.0$ Azo Bordeaux ibilol Package 250# per "I" Bftl. Cost Group 57 Signature# F.K.Schnee Goal Yield 5229#, "as is" and 5020# anhydrous. <4jC moisture) S.B. 1202-24 Use 4940# for cost purposes. DUP050150183 mssLM.feazs i. umm. K-2375 supersedes K-2332 being based on plant modifications of the original process. In recent plant runs it was necessary to split one mole couplings for laking because the volumes for striking and flooding a one mole batch are greater than the capacity of any plant vat. The first plant run was made according to the K-2332 process but since the resulting product was too light in masstone for RB-85-D replacement) various amounts of Azo Bordeaux were added to the other plant batches. Eight pounds of Azo Bordeaux per mole batch appeared to give the most satisfactory results* K-2375 is based on the above findings. Mixes were made of the eight plant lots of the lake in an attempt to set up a standard but to date the final standardization has not been approved. II. YIELD The over-all average yield of eight plant lots of material was 4,908 lbs. which is low but oan be accounted for by one abnormally low yield. The goal yield of 5,229 lbs. "as is" and 5,020 lbs. anhydrous is based on two laboratory couplings and 4 lakings (comparable to plant procedure). Befer to notebook 1202, experiment 24. III. EFFECT OF VARIABLES Ho variables were run on K-2375 but the few made on the K-2332 process can readily be transferred to the new formula. A. Increasing the concentration of the dye solution before the strike resulted in a decrease in strength of the pigment. This may be due to incomplete solution of the dye at the reduced volumes. B. Increasing the volume for coupling seemed to increase the blueness of the pigment. C. Meta xylidine substituted for mixed xylidine does not warrant its use as the resulting product is slightly light in masstone and blue and slightly strong in undertone and tint versus the control. D. Several shipments of xylidine and B-Salt for semi-works and plant use were tested in the laboratory and seemed to be OK. Substi tutes for materials used in the laboratory. E. Addition of 8 lbs. Azo Bordeaux per mole batch of pigment seems to result in a pigment with a masstone about equal to the masstone of RE-85-D. In using more than 8 lbs. Azo Bordeaux, the masstone becomes darker than is desirable. iv. HMSffi* Notebook 1202 -- Experiments 11, 13, 16, 18, 19, 20, 21, 22, 24. FEBj CC F. K. SCENES RESEARCH DEPARTMENT DUP050150184