Document b5Dko7Mk4GJMvme36py865391
.NEWARK PLANT PIGMENT COLOR RESEARCH REPORTS
MARCH-1035
: f.
N36965
PIGMENT COLOR RESEARCH REPORTS
MARCH - 1935
I - PIGMENT GREEN B Pigment Green B GT-68-P (AAB) ..................................... * * (EJH) ...................................... " for Paper Coating & Dyeing (AS)
Page
1-2 3 4
II- RUBBER COLORS (AJS) ........................................................................ 5-8
III- PERMANENT RED SB (AAB, GWJ) ................................................... 9-10
IV - NEW ORGANIC PIGMENTS (a) Special Organic Lakes & Toners (AS) ............... (b) Ortho Chior Para Nitraniline (AAB. GWJ) ...
11-12 13-14
V - LITBOL REDS (a) Calcium Lithol by Azo Sulphate Process, CS7801 (AAB. SWR) 15-16 (b) RT-300-B (EJH) ......................................... ........................ 17-18 (c) Extended Lithols for Rubber CS-7664-65 (ADR) 19
(d) Barium Lithol RT-364-D (ADR) ................................ 20
VI - CHROME GREENS Light-Past Greens. Meadows Type G-389-D (JM.ADR) 21-23
VII- CHROME YELLOWS & ORANGES (a) Medium Yellow Y-359-D (PLP) .................................. (b) Primrose Yellow (PLP) ........................................... .. (cj Oil Retention of Pigments (SCH) ........................ (d) Improvements in Lightfastness of Light Chrome Yellows (SCH.HCM) (e) Excelsior Yellow (PLP) .............................................. (f) Preparation of Rust Inhibitive Pigments(SCH)
(g) YO-27-D (PLP) ...................................................................
24-25 26-27 28-29
30-32 33 34 35-36
VIII- WORKING PROPERTIES OP PIGMENTS Plow of Pigments - Use of Barium Hydroxide(RKH)
37
IX - PHOSPHOTUNGSTIC ACID PIGMENTS (a) Improvements in PTA Pigments (SCH, HCM) ... (b) PTA Yield Studies (EJH) ...........................................
38-40 41-42
X - MPG. STUDIES Grinding of Toner Pulps (JDM) .......................................
43
XI - MISC. ORGANIC PIGMENTS (a) RT-208-D Pire Toner (EJH) ............................. ........... (b) Meta Nitro Para Toluidine (SWR) ........................... (d) Maroon Toner RT-354-D (ADR) .................................... (d) Peacock Blue Lake BL-151-D (EJH) ........................
(e) Pigment Rubine Toner RT-359-D (ADR) ................. (f) Black Pigments (AAB & SWR) .......................................
(g) Color Lakes of Vat Dyes and Acid Dyes on
Wool Acids (AS) .....
(h) Sulfogene Brilliant Blue 5 GCP (AAB) ...............
44-45 46 47 48-49 50-51 52-53
54 55
DUP050315592
2.
XII - RAW MATERIAL TESTING (AECP) ................................................... XIII- SEMI-WORKS PRODUCTION (HA) .....................................................
Page 56 57-63
DUP05031 5593
PI&MBNT COLOR RESEARCH REPORT
SUBMITTED 3Y: APPROVED BY:
PIGMENT GREEN B - GT-68-p
233. 7/
FILES ESJK=?55rs
DATS:
Q35
INTRODUCTION
The work on this problem was concentrated on the paper testing of semi-works and plant batches of GT-68-P and on the study of the paper testing method.
Some little attention was given to the dry colors for rubber, and a few experiments were run to improve the strength and yellowness of tint of the green toner pulp for paper dyeing.
SUMMARY & CONCLUSIONS
Paper Testing Method
Although our results on plant samples of GT-68-P have been in
fair agreement with those of the Du Pont Paper Laboratory, some diffi culty has been encountered in duplicating oiir results. A study of the testing method and technique has revealed some of the causes for our troubles. Metal paddles have been substituted for wooden paddles, which probably absorbed color in varying amounts. It has been found necessary to agitate at 240 R.P.M. for a period of at least two hours in order to obtain maximum dyeing of the paper pulp. The technique of drying the papers has also been improved. In view of these im provements in the testing method, the tests on semi-works batches, which are available for mixing, will be repeated in order to determine their suitability for paper use.
Dry Color for Rubber
A few experiments were run in order to obtain better dispersion in rubber and cleaner tints, but these were unsuccessful. It lias been decided to abandon the problem of developing a dry color for rubber for the present.
Pulp Color for Rubber and Paper
A lead was uncovered in the laboratory whereby stronger, yellow er and cleaner products were obtained for both paper and rubber use. Substitution of caustic soda for the soda ash in the precipitation of the green toner was successful in making the tint yellower, and in addition gave improved strength. This new formula, 444-383, will be tried in the plant.
EXPERIMENTAL PET''-.115
N.B. No. 444
Series 444-34 tried to improve the texture and rubber dispersion of the dry co'lor"*from method 406-6SC (standard GT-SS-p) by treating with blanc fixe alone, and in combinations with diglycol stearate
and Duponol. 'None of the above treatments was beneficial in improving the
rubber dispersion of the dry color.
DU P05 0315594
2 7.'
Series 444-37 varied the diglycol stearate in the dry method 411-120 from"0.5 g. to 2.0 g. per 0.1 mol.
Increasing the DOS in 444-12C from 1.0 g. to 2.0 g. made the dispersion in rubber worse, and a decrease to 0.5 g. gave an improve ment. However, the best dry product was still weaker and dirtier in tint compared with Rubber Green D.
Series 444-55-56-40-4S-44 were paper dyeing tests on semi-works and plant batches of GT-68-P for purposes of classifying available material into groups satisfactory for rubber alone, for paper alone, and for both purposes. The testing method was also studied further.
Further study of the testing method revealed the causes of some of our difficulties. It was found that the wooden paddles were un satisfactory because they probably absorbed color and sizing solution. I'.etal agitators are being used at present. It was also found that rapid agitation (about 240 RPK). and a stirring period of about two hours was necessary for maximum dyeing. These changes will be em ployed in further tests on new material and on repeat tests on the available semi-works batches.
Series 444-58 studied the effect of increasing the caustic soda in the bisulfite ester of 406-66C (standard GT-68-P); also the effect of substituting caustic soda for soda ash in the precipitation.
Increasing the alkalinity of the ester tend.ed to give stronger and brighter colors both by rubber test and by paper dyeing tests. Substituting caustic soda for soda ash in the precipitation had the surprising effect of increasing the strength, yellowness and clean ness of the color both in rubber and in paper.
Series 444-41 checked the effect of substituting caustic soda for soda ash in "the precipitation of 40S-6SC; also varied the alkal inity of the ester.
In rubber and in paper, the caustic soda precipitated colors were yellower, cleaner and stronger than the corresponding soda ash finished colors. With increase in the alkalinity of the ester, the strength seemed to improve slightly.
Series 444-43 varied the alkalinity of the strike in the caustic soda method 444-38D.
All of the members of this series were practically alike in paper. In rubber, it seemed that increasing the alkalinity of strike tended to make the colors weaker.
DUP050315595
PIGHB2ST COLOR RESEARCH REPORT
J3Z. 7& 3
PIGMENT GREEN B GT-68-P
SUBMITTED BY: 61'^ APPROVED BY* ^
7/
FILE: M5trr-^0UB!IS
DATE: MARCH--1935
1 PRODUCT I OH
There were no strikes made in either the plant or semi-7,rorks on this color during the month. However, a considerable amount of time was spent in the Semi Yorks in adjusting the dry content of the most recent plant batch. 41873. to 27# preparatory to setting it up as a paper standard.
SUMMARY & CONCLUSIONS
Continuing the work of last month. Lot 41873 GT-68-P was finally adjusted to approximately 27#. A total of 769;# pulp at + 27# dry content was secured from this batch.
The total yield from this plant lot consists of the following: 6.1# dry (stump) + 45.2# dry (in mix with SY-6676) + 205# dry (in standardized material) = 256.3^ dry. This weight represents 67-1/2,# of estimate, and a loss of 58# dry due to processing. Most of this material was lost in the re-pressing necessary to secure a satisfac tory dry content. The many pulverizations necessary for mixing and adjusting were also responsible for a part of this loss.
One barrel of 350# pulp a 27-1/2# of Lot 41373 has been shipped to Philadelphia Dyestuffs Sales for test by the customer. Results are not available as yet. The other barrel of 41S73 will be set up as a paper standard on receipt of an OK from Philadelphia.
Lot 13926. shipped last month, has been set up as the rubber standard by the Rubber Laboratory, and lots 13915 and 13925 will be shipped as OK for rubber to partially fill a 1000 lb. order. Two 2 mol batches have been scheduled in the plant to complete this order
and to set up a stock on this color.
On completion of paper tests on recent Semi-works batches, mixes will be lined up to secure OK rubber and OK paper material from these lots. Results will be reported next month.
DUP050315596
mmusmi MP asjPtro
FIGMENT 8RSSK B FOR PAPER COATING AMS DYEING
3S--1/
i'
SUBMITTED BY* APPROVED BYi
AS3.7/
FILE* rasffy-TONBRSr DATE* MARCH 1935
INTRODUGTIQK
>
Orientation experiments, conducted in October 1934, on Pigment Groan B paste milled with dextrin and leucanol in a W A P mixer resulted Is a dry powder which dispersed completely in water* This powder when coated with
clay on paper was found to be touch superior to the corresponding paste in strength and brightness. This lead is now being followed In an investigation started this month, with the object of preparing a water dispersible dry Pigment Green B powder for paper coating and dyeing.
SUMMARY & COHCLUSIOKS
Pigment Green B paste mixed with dextrin and the dry mixture milled
in a & P mixer with additional dextrin* leucanol and a small quantity of water results in a dry powder which wets and disperses readily in water and which gives paper dyeings equal to those obtained with the corresponding untreated pigment paste. The pigment content has boon increased to 32$ with satisfactory results, and it is proposed to Increase th pigment content to 50$.
The dry powder when mixed with elay, starch size and water, and coated on wall paper results in approximately 100$ greater strength, yellower, cleaner and more brilliant shade than the corresponding untreated paste. How
ever, the addition of a mixture of dextrin and leucanol to the paste, without special mixing treatment, results in strength and brightness equal to the tT & P milled dry powder. This result is quite surprising sad further investi gation along this line is in progress. Aliho dextrin or leucanol aL one, when mixed with the pigment paste, results in alight improvements tincterially, neither products the great strea-rrfch obtained with a mixture of both.
Further investigations are in progress with the object of obtain ing a super strength paste and a dispersible dry powder for paper oeating and dyeing without involving W ft P milling.
BXFgRDiKKTAL DETAILS
Sxpts. 450-48 and 450-50 N.B. pp. ISO and 180 respectively.
DUP050315597
PIGMBHT COLOR RESEARCH REPORT
SUBMITTED BY APPROVED BY:
RUBBER COLORS
/
FILE: -RUBBER COKCKT DATE: MARCH-1935
IHTRQDUCTIOF
The study of colors for use in rubber has been continued ac tively in the laboratory the past month. Considerable time has been given to orientation studies looking toward additional colors to round out our line. Also there has been some evaluation of special products and a rather large number of control tests . In a number of cases it is still necessary to select batches to obtain material for
shipment.
SUMMARY & CONCLUSIONS
The Green Lake to match Imperial's Green X-1292 has been set up as CS-7854 and is now ready for Semi-works development.
CS-7789 (GT-347-D shade for rubber) (Rubber Green EG) has been studied in an effort to reduce the crocking by treatment with Alumina Hydrate. The effect on the crocking was negligible but there was a noticeable decrease in the ease of dispersion. Hence the work has been abandoned and CS-7789 is considered ready for Semi-works devel
opment.
The 'companies color. Brilliant Green B- PTA based on GT-354D, has been given some study and found to respond to the same treatment as used on other PTA colors. Some variables have been run. and a procedure decided upon which will be used as the basis for a counter sample and semi-works development. This color is known to crock perceptibly but the results on CS-7789 cast doubt on the wisdom of
spending any time attempting to correct this defect.
As a further companion color on the yellow side, the PTA of Thioflavine TCU has been investigated in a preliminary fashion. It also responds to the special treatment used, and gives a greenish shade of yellow which should prove valuable in shading the above
Green PTA colors. It has also been considered as.a substitute for
Hansa Yellow and has the definite advantage of being non-migrating. However, it is much greener and dirtier and will require more careful evaluation before any final conclusions are drawn as to its use for such a purpose. It is also inferior in lightfastness according to our preliminary tests.
Some additional experimental work on the use of Quinoline Yel low P has given products of fair texture with a shade similar to that of Hansa Yellow but about one third the strength. It is non-migrating but much less resistant to exposure to light than Hansa Yellow. Our future course, in regard to it. is somewhat doubtful and will be de termined partly by the outcome of the evaluation of the Thioflavine
Qolor.
DUP050315598
2 !=>
A preliminary experiment on the Victoria Blue R in a PTA for
mula similar to CS-7759 gave strong colors of excellent dispersion in rubber. They were considerably redder than CS-7759 (even redder than Blue YD) and appeared to show less tendency to bleed into parch ment paper than did CS-7759. An additional sample of the dye hap been requested.
A trial of lithosol Brilliant Blue E- alone* in the CS-7854 method failed to give attractive products for use in rubber. It is apparent that a satisfactory Peacock Blue for rubber remains as one of our major problems. We still believe that BL-143-D can be manu factured so as to be satisfactory for use in rubber, but it would be highly desirable to have a stronger color and such is not available at present.
In the field of special products, we have tested CS-7807 and CS-7808, the special oranges developed at Jackson Laboratory. We find them both to show very poor dispersion in rubber. CS-7808 is poorer in lightfastness than Orange YOD while CS-7807 is somewhat better.
Some old samples of Lake Red D have been tested vs. Orarge YOD. While these samples are not especially attractive, they are sufficient ly close to the desired color range to justify a snail amount of orien tation work on the color.
Lead cyanamide (D-1950) was tested vs. Y-305-D. Although quite close in shade in raw stock, it proved to be quite reactive during the cure and gave a completely gray sheet after curing.
In testing control samples we have encountered considerable dif ficulty in. supplying Red SX (RT-300-D). The difficulty arises partly from a difference in standards, which we hope to correct as soon as possible. However, the plant has been unable to manufacture RT-300-D which is suitable for use in rubber, and RT-379-D has shown only oc casional batches which can be used. It is apparent that the difficul ty will be solved either by -
1) Development of a new and better calcium lithol or 2) Better control of the manufacture of RT-379-D so that more batches are suitable for rubber, and a new standard can be established.
Pour batches of &T-57-P were tested by latex dispersion. Three of them were passed as OK. but the fourth was much too blue and the recommendation was made that it should not be shipped until approved by the Rubber Laboratory.
In attempting to build up a stock on Y-366-D, a peculiar diffi culty has arisen for which the answer is not yet available. Out of some half dozen lots tested, all of fairly recent manufacture, every one has shown, to a greater or less degree, dark spots which are apparent only in the cured rubber slabs. The appearance of the spots together with the known effect of certain lead salts in the rubber cure 'have pointed to the conclusion that the spots are the result of contamina tion with more reactive colors. Experiments are under way which, it is hoped, will definitely confirm this conclusion and likewise indicate the point of contamination and thus the remedy.
DUP050315599
7
Three batches of the extended Barium Lithol (CS-7664) have been manufactured in the Semi-works and are all quite close to the CS, being very slightly on the yellow side.
Two batches of the extended: calcium lithol (CS-7665) have also been made, one of which is quite good but the other shows poor dis persion and is not suitable for use in rubber. It is planned that these batches will be used in further mixes to offer to B.F. Goodrich Company as substitutes for RL-400-D.
5XPBRXMBHTAL DETAILS
Control tests and special tests are recorded in notebook #405, pages 69-75.
Experimental work is in notebook #435, pages 174-199.
Series 435-78. Special treatment of GT-354-D for use in rubber. Series includes use of Gardinol, use of Blanc Flare extention and use Of diglycol stearate on both HC1 and HsSO* colors. The H2SO4 colors afe uniformly superior in rubber and the combination treatment as used in CS-7789 gives the best dispersion. 78H represents the opti mum in the series. Some crocking is apparent in these colors.
435-79. Addition of Alumina Hydrate to CS-7789 does not improve crocking and, when used in any considerable amounts, gives distinctly poorer dispersion.
435-80. The amount of extender in CS-7789 waB reduced by draw ing partial waters from the toner. These colors were tested and were also treated by replacing the extender with Alumina Hydrate. In no case was there any noticeable improvement in crocking and there was considerable evidence of poorer dispersion. It is, therefore, decided to proceed with semi-works development of CS-7789.
435-81. CS on Green Lake like Imperial's Green X-1292 (C-37280), This was set up as CS-7854 and rated as OK; ws blue & s.clean against CS-7854. It is ready for semi-works development.
435-82. Further experiments on Quinoline Yellow lake. A is a barium salt of the dye on 30/15 alumina hydrate. B, C, 3> represent various uses of aluminum salts in striking the dyestuff with BaCls on 30/15 alumina hydrate. The products are all fairly soft and indicate the problem is workable. A was tested vs. Hansa Yellow and found to be about l/3 as strong, but quite close in shade. It is non-migrating but much poorer in lightfastness than Hansa Yellow.
435-83. Victoria Blue R in CS-7736 formula with use of Gardinol and special treatment for use in rubber. Very excellent products were obtained which are redder than Blue YD and much stronger than CS-7759. They also showed less evidence of parchment bleed,and an additional sample of the dye has been requested for further study.
435-84. A study of the effect of varying the amount of Gardinol in 435-78H method points to an optimum as regards strength at a lower amount than that used in 78H.
DUP050315600
4,
455-85. peacock Blue Lakes on CS-7854 formula showed poor dispersion in rubber. The products were 10-40^ stronger than BL143-D but dirty and unattractive.
435-86. A further study of the use of Gardinol in 78H. The' lower amounts of Gardinol give an apparent strength which is, however, accompanied by an undesirable dirtiness and some evi dence of instability. The amount as used in 78H gives a slightly weaker product, but it appears to be more stable and is much cleaner and more attractive. 435-87. Thiflavine TCN PTA for use in rubber. The series A, B, C* 3) represents increasing amounts of dye and shows some increase in strength and cleanliness. The special treat ment with Blanc Fixe and Diglyeol Stearate shows the usual improve ment in dispersion to give products which are close to Hansa Yellow (Yellow HKD) in strength. They are non-migrating but are much greener and dirtier and somewhat poorer in lightfastness.
/V-V.
DUP050315601
PIGMENT COLOR RESEARCH REPORT
Sd~' 73
?
LITHOSOL RED 2B
SUBMITTED BY APPROVED BY:
IHTRODUCTIOH
<yv-S
S. 3?
PILE: 'MiaO^TOl^S-
DATEs.MARCH-1935-
The problem of developing a barium toner of Lithosol Red 2B was begun this month.
Lakes of the calcium salt, employing various extenders, were also prepared and will be evaluated in printing ink in our General Laboratory and in rubber at the du Pont Rubber Laboratory.
SUMMARY & COHCLUSIOHS
Barium. CS-7745 (calcium toner) was used as a base formula for the beginning of the barium toner problem. The studies included pH of strike, temperature of development, temperature of strike, variation
in para soap, reverse strike, volume of strike and amount of barium chloride.
A neutral strike was found to give the best results with respect to strength and lightfastness. An acid strike was weaker and decided ly inferior in lightfastness. An alkaline strike gave a duller masstone and lower tinctorial power.
Development of the barium toner tended to give lighter masstones, with bluer tints.
Variation in the temperature of strike from 20C to 100C was accompanied by an increase in depth of masstone from 20C to 60C, beyond which the masstone became lighter and duller.
Para soap tended to brighten the masstone, increase the strength and yellowness of tint. Increase in para soap from 1 g. to 4 g. per 0.05 mol strike caused the pigment to become weaker in tinctorial power.
Reverse strike apparently offered no advantages over direct strike
Volumes of strike between 1000 cc and 2000 cc per 0.05 mol strike showed practically no differences.
Increasing the excess of barium chloride tended to give lighter masstones with lower strength.
As a result of the above variable studies, 447-16C was developed
and has been selected as the temporary laboratory standard. Compared with RT-313-D (barium Red for Lake C). 447-16C is slightly darker and browner, slightly weaker and bluer and decidedly better in light fast ness. The 447-16C formula also seems to be quite stable.
Calcium - Samples of 45# lakes on alumina hydrate, gloss white and blanc fixe bases were prepared from a semi-works batch of calcium toner. These samples will be evaluated both in printing ink and in rubber for the purpose of determining the advantages, if any, of an extended color over a toner.
DUP050315602
z
Our own ru'ober tests have shown that the extended colcr s possess better dispersion than the toner, but showed no improvements in crock ing. These samples* together with a sample of the toner pulp, were submitted to the du Pont Rubber Laboratory for their evaluations and decision as to whether we shall standardize on/dry extended color or a dry toner for rubber purposes.
BXPKRIMENTAL D3TAILS
N.B. 447
Barium 447-11 was a study on the pH of strike. It was found that a PH of 7 (neutral) gave a lighter, yellower toner, having more brilliance, greater strength and lightfastness than either an acid or alkaline strike. The acid strike gave better texture, but was weaker and decidedly inferior in lightfastness; an alkaline strike gave a dirty masstone and less strength.
447-12 was a heat development study of the toner, starting at 40 and ending with a 30 minute boil.
The heat treatment increased the blueness of tone, but decreased
the strength. Differences were more pronounced between masstones than strength.
447-13, 19 were studies on types and amounts of dispersing agents.
Para soap gave a brighter masstone, increased strength, but also more bronziness. By increasing the Para soap from 1 g. per 0.05 mol charge to 4 g, the pigment was made brighter, but weaker.
By substituting diglycibl stearate and Duponol for Para soap, weight by weight, the pigment is made bluer, weaker and possibly less lightfast.
447-14, 15 were studies on the temperature of strike from 20
to 100. Increased depth was produced by striking below 60 - above 60;
the pigment became lighter and duller in masstone.
447-16, 19 were studies on the volume of strike.
Decrease in the volume from 3 liters to 1 liter gave practically no differences in properties. A single strike in#L9, cutting the vol ume from 3 liters to 1-1/2 liters gave results contrary to previous work. Therefore it was decided to repeat the volume run in #19 at
some future date.
447-15. 16, were studies on reverse strikes. It was found that the effects of reverse striking were practically nil.
447-18 were studies on barium chloride excess in the strike.
Increase in barium chloride excess tended to give lighter masstones and less strength.
DUP050315603
PIGMBBT COLOR RESEARCH REPORT
* /!
SUBMITTED BY* APPROVED BY:
SPECIAL ORG-ARIC LAKES
2.ZC
nia* tss&T^roS^s DATE: MARCH-1935
IKTRODUCTIOK
Investigations on azo color lakes were confined this month t orientation studies of new intermediates for the preparation of dyes and color lakes therefrom.
SUMMARY & COHQLP3IOHS
2* 4* dlnltro 4 amino diphenylamine
This intermediate diazotized and coupled with beta naphthol, R Salt and aceto-acet-anilide yields dyes and pigments varying from very deep claret to light yellowish rede. The calcium and barium toners and alumina hydrate lakes are deep clarets, non-bleeding in
oil and possessing only moderate lightfastness. These eolor lakes are of no interest#
The beta-naphthol pigment dye is a deep brown of poor general properties and possesses no merit*
The aoeto-acetanilide pigment dye is a light yellowi*. red, non-bleeding in linseed ell and possessing good light stability. This pigment is lighter, duller and appreciably yellower than Para Red Y RT-22-B, and possesses no appreciable merit.
1 naphthol 3:6 diaulphonic acid
This isomer of R Salt, coupled with diazotized anthranllic acid and prepared into lakes by the RL-211-B procedure results in a deep brownish red of yellow and dull shade, and therefore is not of interest*
It5 disulnho 8 aanhthvlareiwe
The barium-alumina hydrate lake of the dye, diazotized It5 disulpho 2 naphthylamine --^ R Salt, is a deep bright red of yellowish shade, non-bleeding in linseed oil and good in lightfastness. Altho the dye contains four sulphonie acid groups , it precipitates complete ly with barium chloride. The barium lake possesses some merit but does not appear to possess sufficient promise as to warrant further investigation at the present time.
3*amlno 4>methoxy ortho benzoyl benzoic acid 3 *4^ nitre amine ortho benzoyl benzoic acid' and S'V amino 4* asthoxy ortho benzyl benzoic acid.
The above intermediates coupled with R Salt yield brilliant
dyes ranging in shade from yellowish red to deep bluish red. These dyes possess no merit for the preparation of color lakes owing to their extrema solubility. These dyes either do not form metallic salts or their metallic salts, Ga, Ba, Sr, Sg and Fb, are very sol uble*
DUP050315604
f-u2#
3jhe above intersiediatea ooupled with beta naph.th.ol and laked with barium and calcium yield red lakes ranging in shade from light yellowish red to deep bluish red* All the lakes bleed in linseed oil and possess no appreciable merit tinetori&ily.
BXPBRIMSSTAL MAXIS
2* 4* dinitro 4 atsino dinheuvlamlns -4 B.S1 (Ba lakes & toners
R SaltjCa "
"
A *A A
Escpt* 450-37 H*B. 450* page 184
1 na-phthol 3>6 dlaulphonic acid
anthranilic acid - Ca & Ba lakes.
Expt * 450-3$ 5.B. 450, page 132
It5 disulnho 8 nanhthylaralne H Salt - Ba lakes
*......... "llxplu 450-43 B.B. 450 , page 146
xt amino 4* mathoxv ortho benzoyl benzole add
DUP050315605
PIGMENT COLOR RESEARCH REPORT
SUBMITTED BYi APPROVED BY:
ORTHO CHLOR PARA NITRANILINE
/ait ^
PILE: !3SU-e3lS DATE: MARCH-1935
INTRODUCTION
Shipments of lots 1 and S of ortho-chlor-para-nitraniline were received from the du Pont Dyeworks and were tested in the RT-208-D formula.
A brief study of the coupling formula was also carried out.
SUMMARY & CONCLUSIONS
Lot 1 of ortho-chlor-para-nitraniline was received as a paste
(RMD 123) and in dry form (RMD 119) . Lot 2 (RMD 184) was received as
a paste. Lot 1, both wet and dry, was quite lumpy and contained con siderable quantity of very hard material which was difficult to screen and which did not diazotise. Lot 2 was better in this respect. Tinctorially and in yield of coupled product, there was no substantial difference between the wet and dry forms of lot 1 and lot 2. The
average yield obtained was 300 grams per mol. The formula card yddld of`-RfwgQSwBflis 310; theoretical yield is 328. The shipments were prac tical checks to the original material (Jackson Lab. No. 190; our D# 1887) tested by Mr. Siegel. Compared with RT-396-D, the products were very close in mass-tone, slightly blue and slightly weak; vera&a RT208-D, they were light and bright in masstone, slightly weak and blue. The new intermediate gives products which bleed distinctly less in turpentine and/Werstriping with white paint than RT-208-D and RT-396D.
The brief study of the formula included reduction in urea, reduction in sodium nitrite and the addition of Duponol in the diazo.
Reduction in urea from 7.5 g. to 3.0 g. per 0.1 mol OCPNA gave a brighter masstone with slightly increased strength.
Reduction in nitrite from 8.4 g to 7.2 g. per 0.1 mol OCPNA gave slightly lighter masstones. The use of 7.2 g. sodium nitrite
(5% excess), however, was accompanied by a decrease in yield.
Duponol gave increased strength and yellow tint but the masstones were duller.
The formula 219-48C, used in the above work, was found to be fairly consistent with respect to masstone, but variations in strength and in tint were obtained for some unknown reason. No further work on this problem is contemplated for the laboratory at the present time.
EXPERIMENTAL DETAILS
219-46. 50 included tests on samples of ortho-chlor-para-nitro
aniline. Lot #1 paste (RMD 123) and dry (RMD 119) r#1945, and Lot #2
(HMD 184) returned practically identical results, indicating uniformity of intermediates, whether in paste or dry form. The pigments prepared
DUP050315606
2.
were very close to RT-396-D in masstone, but slightly lighter and brighter than RT-208-D. In strength, the pigments were bluer and weaker than RT-396-D and RT-208-D.
219-48 was a study on the effects of urea in the process.
A reduction in urea from 7*5 grams to 3 grams per 0.05 mol
charge gave a lighter brighter masstone and slightly greater strength.
Absence
urea resulted in a very dirty brown pigment.
219-49 was a study on variable nitrite excess.
Decreased nitrite, varying from 8.2 grams to 7.2 grams per 0.1 mol charge, gave a lighter, yellower masstone and slightly increased strength. This change, however, was paralleled by a corresponding loss in yield.
219-48, 49 was a study on the effects of Buponol.
Duponol gave increased strength and yellowness, but it also gave brownness and dullness to the masstone.
219-47 was a study on the effects of screening the ortho-chlorpara-nitro aniline.
There were no appreciable differences between the pigments pre pared from screened and unscreened intermediates. The unscreened material gave a slightly higher yield, probahly due to less manipulation
losses in the process.
DUP05031 5607
PIGME33T COLOR RESEARCH REPORT
SUBMITTED BYi APPROVED BYj s
CALCIUM LITHOL BY A30 SULPHATE PROCESS CS-7801
e? 'S'/
PILE i TsZTimr-fmJS DATE: JABa-1936
if t r o d u c t io m
further study of the CS-7801 process for preparing calcium lithol red was carried out with the possibility in mind of obtain ing a suitable pigment for use in rubber.
SUMMARY & COHCLUSIOHS
It was explained in last month's report that a considerable amount of calcium chloride was required in the laking of CS-7801 in order to obtain maximum strength by rubout, but that this same color was rather poor in rubber dispersion. It was also discovered that a sample which was struck with a lower amount of calcium chloride and which was weaker by rubout than CS-7801, was quite satisfactory in rubber, in fact, was slightly better than C3-7665. an extended cal cium lithol prepared by the orthodox RT-379-D formula.
In accordance with the above suggested idea that lower calcium chloride in the strike of CS-7801 would result in better dispersion in rubber, an experiment was run in which the calcium chloride was varied. The results confirmed the previous findings. A product was obtained which, as a toner, was distinctly better than RT-379-D stan dard in rubber dispersion and which was about equal in strength, slightly bluer and cleaner than C3-7665. Extending this pigment with blanc fixe, and treating with diglycol stearate gave no added improve
ments .
Reducing the amount of ammonium chloride in the strike of 446-23C (low calcium chloride strike) gave an improvement, by rubout, in masstone, strength and cleanness of tint. In rubber, however, the whole series was poor in dispersion, including the control to 44S-23C. This point will be re checked.
It is hoped that- the azo-sulphate process for preparing calcium lithols will help us out of the troublesome situation which confronts us in the matter of standardizing shipments of calcium lithol toner
for Rubber SX.
EXPERIMENTAL DETAILS
".3. #446
Series 446-42 tried lower amounts of calcium chloride in CS-7801
in order to try to obtain a soft texture and rood dispersion in rub
ber. Lowering the calcium chloride 50L in CS-7801 gave a fairly soft
texture and also good dispersion in rubber, equal to C3-7665. In creasing amounts gave harder texture and poorer rubber tests. There fore it appeared that the lower calcium chloride was necessary f or soft texture. On the other hand, the rubouts showed a decrease in
depth, strength and brightness.
Series 446-43 extended the low and high calcium chloride toners
DUP050315608
/(>
2 with 30-^ blanc fixe similar to C3-7665 and tried the effects of di glycol stearate.
The extended low calcium toner was no better than the toner itself, while the high calcium toner gave poor results. Diglycol stearate had no advantageous properties.
Series 446-44 varied the ammonium chloride in the low calcium toner (446-2 3"c)".
The results were weak in rubber. Decreasing the ammonium chloride gave dark, strong, and bright results- versus 446-23C by rubout.
DUP050315609
PIGMENT COLOR RESEARCH REPORT
/2
RT-300-D
SUBMITTED BY: ' APPROVED BY:
#J23.//
PILE: LSTSfeEB
DATE: 'MARSH-1935
I3JTRGDUCTIOH
'S'ork was started in the Semi Works during the month in an ef fort to prepare light, bright material for shading and to set up a formula that will give light, bright material in the plant.
SUMMARY & COUCLUSIOKS
The first batch, checking the standard RT-300-D formula, C3-7038 gave dark. s.brown, blue, s.strong material. Lithosol acid TOB Lot 132 was used in this batch.
Checking the above batch except using a more recent shipment of T03, Lot 141, also gave dark and brown masstone material.
The next batch was made checking an old semi-works formula, S"'-5238, which previously had given bright material. Lump results on this hatch were also unsatisfactory, being dark, weak and blue versus the standard RT-300-D.
A modified RT-379-D formula was finally set upon as the most likely to give bright results and a batch was made which gave fairly satisfactory results, it being v.s. light, bright, vvs str.. yellow and clean versus the RT-300-D standard.
In an effort to secure light material a batch was made checking this last batch with the exception of adding .4# sodium phosphate {2 per mol) to the 3eta Uaphthol solution before coupling. This re sulted in a batch s.light and bright versus the standard, but a still
further increase in lightness is desired.
In an effort to secure this lightness a batch was made using the modified RT-379-D formulation, but developing at a boil instead, of 190 C'P. This batch was dark, blue and weak versus the standard.
Prom these results it appears that the variable most likely to give lighter material would be a large amount of sodium phosphate in the coupling. This variable will be checked and reported next month.
ki.
DUP050315610
EXPERIMENTAL DETAILS
N.B. 441, pages bO-88
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DUP050315611
PIGMENT COLOR RESEARCH REPORT
SUBMITTED BY: APPROVED BY*
EXTENDED LITHOLS FOR RUBBER CS-7664-65
33. //
J? IJjiQt # *VEV!tw3ft` DATES ^gj|ajfci.g25
INTRODUCTION
Additional material of the type made in October 1934 -was made
in the Semi-works this month to check the procedure and to obtain a stock of RL-400-D, the rubber color in which these lithols are used. Three batches of RL-7664-D and two of R1-7665-D were made.
SUMMARY & CONCLUSIONS
The extended barium lithols were fairly close to the CS-7664 standard by rubber test, being slightly yellow and clean, but prob ably readily shadable.
One batch of calcium lithol was weak on rubber test but a second batch coupled at a lower alkalinity was equal to standard.
The effect of this variation on rubber dispersion of this color appears to be very definite.
Mixes will be made to match the RL-400-D standard.
SXB3RIMENTAL DETAILS
N.B. 353, p.96
SW Variation
Rubber test
6858 CS-7664. 2x SW-6454 (Oct. 1934)
vs CS-7664 - s.yellow & clean
6867 Check SW-6858 but reduce alkalin
ity after coupling by addition of acetic acid
* - vs wk, s.yel & cl.
6884 Check SST-6858 but dry in steam dryer instead of electric dryer
" - s.yellow and clean
6873 2X SW-6455
vs CS-7665 - weak
6879 Check SW-6873 but reduce caustic soda for Beta naphthol from 15.6 to 14.4#
* - v.v.s. yellow
jKf
DUP050315612
PIGMENT COLOR RESEARCH REPORT BARIUM LITHOL RT-364-D
SUBMITTED BY: (y . *) . APPROVED BY: ^
'
PILE: -IfSTHOBS DATE: MARCH-1935
INTRODUCTIOH
Two batches of RT-364-D were made in the plant on the alkaline coupling formula CS-7514 to obtain material suitable for RT-344-D by rubber test.
SUMMARY & COHCLUSIOHS
Both batches were made on the modification of CS-7514 found to be beneficial in the Semi-works, i.e. lower alkalinity of coupling and
lower amount of barium chloride.
Ho mixes have been made as yet but one batch which is darker and bluer than RT-364-D appears to be suitable for the purpose far which it is intended. This type was obtained by use of an increased amount of para soap.
EXPERIMENTAL DETAILS
N.B. 385, p. 82
Lot 42666. Check 40652 (Hov. 1934) vs RT-364-D - s.dark; v.s.yellow? OK? v.s. yellow
Lot 42715. Check 42666 except increase Para soap from 8 to 24# vs RT-3$4-D - dark, s.brown? blue? v.s.strong; blue, v.s.dirty
DUP050315613
PIGMENT COLOR RESEARCH REPORT
LIGHT-FAST GREENS MEADOWS THE G-38SD
Jr~r u
SUBMITTED BY APPROTRSD BY:
INTRODUCTION
eewoid CX o^1
T FILS DATE MARCH 1935
About twenty batches of this color were struck during the month
in the semi-works; but as grind results are available for only four of these, the majority of the results will be reported next month. A comprehensive study of the process variables has been carried on, and the most favorable of these have been incorporated in plant proce dure .
In the plant, production of all shades of the G-389-D was car ried on with special emphasis placed on obtaining more brightness of masstone, particularly in the lighter shades. Four batches of G-389-D,
. two of G-390-D and one each of G-391-D and G-392-D were made.
SUMMARY & CONCLUSIONS
Semi-Works The use of tin crystals alone in the treatment of the yellow after washing gave a product that was slightly blue in masstone and yellow in undertone and tint. The lightfastness on vat control was very slightly superior to standard, but on grind results was worse;,
showing the color to be unstable. The addition of copper hydroxide to the above procedure evidently made the color a little more stable, the lightfastness being a little better although still inferior to
standard. Strength is also decreased by this procedure.
One batch struck at 130F instead of 110F was decidedly olive and dirty, showing the same instability mentioned in the previozs para graph.
The use of soda ash and tin crystals as treating agents after washing resulted in a dull product, yellow in drawdown and tint.
Although, grind results are not yet available, there is every reason to believe that the omission of soda ash in the treatment of the yellow gives a product that is bright and slightly blue in masstone and clean in undertone.
Plant The low bichromate formula for G-389-D tried last month did not give satisfactory results on a check run and was not abandoned. Use of a double amount of tin crystals, found to be beneficial in the Semi-works was not helpful in the plant on either G-389-D or G-390-D.
Very promising results have been obtained by omitting the soda ash on both shades from the after-treatment of the yellow on an other wise standard formula. The product is bright in masstone and clean in tint with slightly superior lightfastness. It was also possible to
omit the cupric hydroxide on this formula using only alum and tin crys'
tals in the treatment of the yellow.
DUP050315614
2
A 4600# mix of G-389-D was made up to fill existing orders but turned out too olive. This can be shaded with bright material ob tained by the above variation.
More material of G-390-D depth is needed before a mix can b e made.
One batch each of G-- 391-D and G-392-D, made on standard for mula, became slightly dirty in masstone during processing and may require the same change as was made for &-389-D.
SXPBRIMBHTAL DETAILS
sw m
Variation
Semi-Works JT.B. 436, p.168 Standard mass. Und
Light Str. Tint Stabi-
lity
6841 Check SW-6761 but omit
G -389-D
alum and soda ash after
Lot
washing
13794
blue
s.yel. OK yel. e.worse cl.
6847 Check SW-6761 but add only soda ash and tin crystals after washing
Cl
s.blue s.dull yel. OK #el. worse chalky
6849 Check SW-6761 but add only tin crystals after wash ing
n
s .blue s.Jrl w.fli yel r worse chalky etr&hgr Btr Ibw
6852 Check SW-6761 but strike at 130F instead of 110F
1C
olive
yel, OK dirty
yel. worse dirty
DUP050315615
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DUP050315616
PIGMBHT COLOR RESEARCH REPORT
MEDIUM YELLOW Y-359-P
r , rt
SUBMITTED BY: fn.
APPROVED BY:
x/y-/
PILE: gBROMB YELLOWS
DATS: 3$jjj^Ptfkfe>-
INTRQDUCTIOB
A study of this process was continued in the factory. Diffi culty in obtaining satisfactory tinctorial properties made it necess ary to run variables in an attempt to improve the color. Production continued to run satisfactory in lithographic resistance.
Most of the production during the month was made with lead ni trate liquor purified with feathered lead.
SUMMARY & CONCLUSIONS
Seven batches made previous to this month's production were somewhat superior to standard in masstone and lightfastness, and were OK in lithographic resistance. The lead nitrate liquor used in these batches was made from pig lead, and was satisfactory without purifica
tion.
During this month, seven batches were made using lead nitrate liquor made from lead sludge; these liquors were purified with feather ed lead. Six of these batches were-very slightly green and dirty in masstone, and showed a slight increase in strength. They were only equal to standard in lightfastness. Lithographic resistance was good
in all cases.
Differences were so slight that it is impossible to conclude
definitely whether any of the variables used had a desirable effect. Sodium chloride in the strike, and higher strike temperature were tried. Several of the lead nitrate liquors showed a trace of copper impurity.
KXEBRIMENTAL DETAILS
Notebook 448. p.70-71
5**
DUP050315617
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DUP050315618
PIGMENT COLOR RESEARCH REPORT PRIMROSE YELLOW
SUBMITTED APPROVED BY*
INTRODUCTION
UN
Jl /A/ PILE: 9EROMB'-Y33LLOW3 DATE: MARCH-1935
Semi-work batches of the new primrose yellow were made to study variables on a modified formula.
SUMMARY & CONCLUSIONS
Studies were made as 0,125 mol batches based on a revised for mula which differs from the original in omitting the sodium sulfate after the second water, and an increase in the amount of alum. This formula is represented by SW-6831.
The following variables were studied*
1) Increasing soda ash added after strike; this resulted in redder material of worse lightfastness.
2) Doubling the amount of sodium chloride resulted in a v.slight increase in cleanliness and very slight improvement in light stability. This was a press cake result and may be due to better drying conditions.
3) Reducing sodium bichromate with a proportional increase in sodium sulfate resulted in red. dark material of slightly better light fastness. Lowering the pH from 5.0 to 4.7 by cutting the amount of
soda ash resulted in greener, dark dirty material of very slightly worse lightfastness. ThiB batch was repeated with lead nitrate liquor. The product was much redder. One batch made as SW-6831 except using lead nitrate liquor resulted in material of slightly redder masstone and v.s. worse lfightfastness.
EXPERIMENTAL DETAILS
Notebook 448, pages 152-153.
DUP050315619
>
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DUP050315620
PIGTBNT COLOR RESEARCH REPORT OIL RETENTION OP PIGMENTS
3S'- ?3
SUBMITTED 3Y; J.C< Jhn** f
Alu-GOVED BY:
INTRODUCTION
PILL: 01-3Re3~gtta^rrJ DATE: 1Mm*SK.-1935
The problem cf oil retention and lithographic breakdown has received some attention during the past month. The theoretical aspects of the problem are discussed in several notes by the writer.
51HL1ARY & CONCLUSION
The experimental r,ork to date has re stilted in no new informa tion. Drying in the presence cf sodium chromate or sodium, resinate seems to give better oil retention than wren sodium sulphate is used.
Several experiments on drying in tha presence of water soluble oils gave irregular results.
BXPURINSNTh DETAILS
".3. 431
421-23. To prepare a pigment of higher oil retention by coat ing a chrome orange with an organic compound.
A sample of Y0-27-D (lot 42370} was filtered, washed and differ ent parts were treated as follows:
A Dry control
3 treat with acetamide
C " tri-amy phenol '
D " diphenyiamine (D-520)
" glycerine
11 glycol bori borate
G " tri e thanelair.ine
1? ix
n xylidine
I " hydroxy diphenyl methane
Results: No decided alteration in oil retention
observed.
421-24. Continuation of 421-23. A YO-27-D (lot 42370} control
B & C treat with tri acetin P treat with later
Results: Latex gave a heavv ini:, ho improvement in oil retention in Bor C.
421-25. A sarnie of Y-359-D let 42624 was filter different parts were treated as follows:
A Control B treated with late::
, washed and
ing
C
D E P G E
O.lw
r* H acetir.
" '* glycerine n " xylidine slurry heated tc 150rP treated with sodium rerinate treated with sodium reninats-
sodium chromate.
but
washed
-ith
isr ccntain-
I treated with a very very small amount of sodium resinate
TM .. --
DU P050315621
.All of these samples r.-ere dried for 18 hours e:.rcept 2 4G which was dried for only seven hours.
Results - Apparently sodium chromate and sodium resinate im prove the oil retention slightly.
r ' >;
&
r
S'.
DUP050315622
PIGLET COLOR II3.UCH RL?0.:T IKPROViJlCSI^rS 1ST LIGKTPA3 3S Off LIGHT c h r o :
YH.1LO iiQ
SUB KITTED BY ALT:-:(Tr:3D BY:
*?// / PIIE DATA IWitfH- frP'35
I?TT.-:ODUCTIOK
The study of the new excelsior and light medium yellow process ha'- been continued from the past month. A further improvement in strength, appearance and lightfastness has been obtained.
A slight improvement in the new Y-202-D process has been ob tained thru the use of zirconium salts.
A study of the effect of zirconium oxy chloride and zirconium sulfate in chrome yellow formulations has been initiated.
s u it 'Pi y & c o in c l u s io k
The study of the excelsior and light medium yellow process men tioned in last month's report was continued during the past month. It was found that heating the pigment at the end of the strike caused a decided improvement in lightfastness. Keating generally improves the 1ightfastness but gives a changeable product. In this case nrobablj* because of the lead excess the product is not changeable. The strength is also apparently increased, it was also found that the use of addi tional quantities of alum improved both the appearance end lightfast ness.
A rather intensive study has been made of the use of zirconium salts in chrome yellows. Zirconium oxy chloride apparently is infer ior to stannous chloride as a restraining agent in greening yellows. Zirconium sulfate in place of alum in Y-202-D yields an inferior pro duct. It is also inferior to sodium sulfate in a chrome yellow strike. '"here alum is added after a strike and. precipitated in the form of hydrate, zirconium sulfate has in all cases been found equal or super ior to hydrate. It has been tried a number of times in the new labor atory -orimrose. excelsior, and Y-202-D type processes. Zirconium oxy chloride when added to the lead nitrate solution before the strike causes the precipitate to be lighter in shade and probably smaller in particle size. In the case of the new laboratory Y-292-D process the result is a slightly better finish and transparency, but in the case of the primrose the results is a greener dirtier mass tone. Where it is desirable to obtain a small particle size in the initial lead chro mate precipitate the use of zirconium oxy chloride may be very helpful. A number of other miscellaneous strikes using zirconium salts gave negative results.
glLRBRIiaiTTAL BBTV;IL? Notebook 453-452
452-16. Study the effect of zirconium oxychloride fied 415-50A procedure, also in Y-299-D.
Zirconium oxychloride in the lead nitrate resulted dirty pigment worse in lightfastness than the control.
in the modi ir. a green
452-18. Study effect of zirconium oxy chloride on the Y-359-Ii procedure.
MS;.
DUP050315623
3/
2
In this experiment it appears that the use of zirconium oxy chloride has a tendency to produce e very slightly cleaner product; it does not appear to aid in improving the lightfastness,
452-19. Try using zirconium sulfate for sodium sulfate in the 45-'~15A-l excelsior procedure.
It appears that zirconium sulfate when substituted for sodium sulfate gives a redder product,
452-20. Study the use of zirconium hydrate in 453-35B. ihfe improved Y-202-D procedure; also study the use of a large amount of sodium chloride in the 452-4A ;'a procedure used in the improvement study of Y-190-D. using only chromate liquor and lead nitrate.
In this experiment zirconium hydrate gave an excellent improve ment in lightfastness. The use of salt gave an improvement in light fastness, and it v/as also noted that the mounts of~this product did not darken upon drying.
452-22. Study 20A and 2OD (453-353 type), but finishing v,'ith a pH of '5.6 "instead of 4.7.
-In this experiment zirconium oxy chloride gave a dirty product poor in lightfastness. C made with the same amount of ziroo nium hy drate as 20D gave check results in lightfastness, while 3 made with l/2 the quantity of zirconium hydrate was very slightly worse in lightfastness, but much better in lightfastness than the control using alum. The final pH had no marked effect on the products obtained.
452-24, To study zirconium sulphate precipitated as hydrate, in the 45'3-i2C and 452-4A procedures.
In this experiment the substitution of zirconium hydrate fbr the usual alum-soda ash treatment resulted in a cleaner pigment accompanied by an improvement in lightfastness.
452- 25. Study the effect of titanium oxy sulfate on the 452-20A procedureT
Titanium oxy sulfate precipitated as hydrate gave results simi lar to precipitated zirconium hydrate.
453- 35. Study the use of zirconium salts in an improved Y-202D f orraula`^4 53 - 4A).
It appears that zirconium oxy-chloride in C gave a very promis ing clean light mass tone on modified Y-202-H with improved lightfastness.
453-39. Study use of zirconium sulf-te in standard Y-202-D for alum.
In this experiment, zirconium sulfate substituted for alum in the strike gave a very dirty brown product, with no improvement in lightfastness.
453-40. Study the effect of zirconium, hydrate on the 213- pro cedure
Zirconium sulfate when precipitated as a hydrate as in the alum-soda ash treatment gave a product very close to 213, with a very slight improvement in lightfastness.
.tjg;'
DUP050315624
3 452-21. Study on Y-299-D formula and Y-359-D procedure the effect of slowly heating to 180 ]p. Heating to ISO0? in 5 minutes or in two hour^had practically the same effect on products of these two procedures. 452-83. Study heating treatment on semi-works hatch of y--309--D . Heating the slurry of semi-worts hatch of Y-309-D (sample taken after the final t reatment). to 180F gave an improvement in lightfastness but the product obtained was somewhat dirty. 452-26. Study the effect of heating to 180']? in 10 and 45 min utes before flooding pigments made using the 452-22B procedure. Slow and rapid heating had no appreciable effect tinctorially, but slow heating seemed to produce a more flocculent slurry which did not settle very well. On plant scale this would probably result ir. a flop. 453-41. Preparation of 1 lb. samples of chrome yellow contain ing altax; made by dry mix.
DUP050315625
PIGMENT COLOR RESEARCH REPORT EXCELSIOR YELLOW
SUBMITTED BY: APPROVED BY:
'
PILE: eiBtatffi-3SH=eW DATE: MARCH-1935
INTRODUCTION
A semi-works batch was made to develop an excelsior yellow of special properties (high oil absorption and high finish), based on a laboratory formula.
SUMMARY & CONCLUSIONS
The laboratory experiment 452-15A, which resulted in material of the desired properties, was tried out in the semi-works. This formula differs from Y-309-D formula in omitting the basic lead car bonate, replacing sodium bichromate by sodium chromate, and an increase in alum. The material resulted was slightly green, v.s.dirty; vs green; of about equal strength; v.s.green, s.better in lightfastness and showed equal high finish compared with lab. 452-15A. These readies are from a press cake sample. A study fr ink properties will be made
on the ground material.
EXPERIMENTAL DETAILS
Notebook 448, page 26.
/ DUP050315626
3S-
PIG3SET COLOR RESEARCH RErCRj
SUBMITTED BY: APPROVED BYJ
INTRODUCTION
PREPARATION ON RUST INHIBITIVE PIQRENT
FILE; BATS:
l?3'~
OKilEtriU
ifss'
The work on rust inhibitive pigments was continued during the past month. As the results of the work at the Experimental Station become available the work at Neivark will be continued.
SUMMARY & CONCLUS TOY
3evero,l samples vere prepared for the Experimental Station dur ing the past month and seme experimental work was done on increasing the water impermeability of talc. The v/ork to date is reviewed in the letter of Dr. Horning to Dr. Patterson of March 6. 1?35.
EXPERIMENTAL PITAILS
Notebook 421
421-20. . Study the oossibility of improving the lithographic breakdown by tre- ating t-a---l-c-- with various agents.
A talc treated with sodium oleate
3 II
" resinate
Cn
lead nitrate
B ii Eu F ! G tf
tt soda ash and all tv lead liquor nitrocellulose tt latex emulsions
H I
China clay heated to red heat
Talc
II
ir
Results. F. G- E. and I showed increased water resistance on the board lithographic breakdown test.
DUP050315627
PIGMENT COLOR RESEARCH REPOST Y0-27-D
*r
SUBMITTED BY: fh
APPROVED BY: ^
PILE: -CHROMB-tmANaE DATE: MARCH-1935
INTRODUCTION
Plant study was continued on this color, following the work of the last month, which showed slight improvement.
SUMMARY & CONCLUSIONS
Pour batches were made during this month based on a formula
with a total amount of .61 mols chromate per mol lead. Three batches were made as direct strikes (chromate into lead). The effect of changes in acidity were studied. Direct strike compared with a previous ly made batch with reversed strike (both with 1.164 mols acid) re sulted in lighter, yellower 3hade and slight increase in strength. The second batch, with a decreasd in acidity, resulted in redder, stronger material. The third batch with an increase in acidity to
1.133 mols gave material fairly close in masstone to Y0-27-D, but of high strength. The fourth batch made by reversed strike with high acidity resulted in material practically equal in strength to standard Y0-27-D and fairly close in shade. This batch was left with a lead excess and heated to a boil. Then more bichromate was added to obtain a very slight excess of chromate; the last amount was added as sodium chromate to raise the pH to 7.3
Tabulation of batches follows: (Next page).
EXPERIMENTAL DETAILS
Notebook 448, pages 152-3
ft-
DUP050315628
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DUP050315629
PIGMENT COLOR RESEARCH REPORT
33--rf 37
FLOW OF PIGMENTS USE OF BARIUM HYDROXIDE
SUBMITTED BY; (/P/t
APPROVED BY
/f-^A
FILE;
TREATING AGENTS DATE; MARCH-1935
INTRODUCTION
The study was begun of the pigment properties of colors to which nave been added compounds inducing flow to the ink. The work to date ha6 been con fined to RT-283-D and RT-313-D, studying tne effect of Barium hydrate and other inorganic bases on the flow of the ink.
SUMMARY & CONCLUSIONS
The addition of Barium Hydrate (3-5%) to Duol Red RT-283-D made tne ink nave considerably better flow than the untreated control. Barium Hydrate was more powerful in this respect than any other base tried up to the present time. Soda ash was next, having about two-thirds as much effect as an equal amount of Barium hydrate. Sodium Resinate, Magnesium Oxide, and Borax had small but negligible effect. Barium Carbonate, Kadox, Magnesia, and Hydrated Lime had no noticeable effect.
The effect of Barium Hydrate on Red Lake C RT-313-D was greater than on RT-263-D or RT-332-D. As little as 0.5% Barium hydrate caused a noticeaole flow in RT-313-D ink and 1% caused considerable flow. The effect on RT-331-D was not as great for an equal weight as with RT-313-D.
Further work is planned to investigate the stability of Barium hydrate, its effect in the presence of driers and on other properties than flow, and also to try several other basic materials not examined to date, such as Di and TrxSodiura Phosphate.
EXPERIMENTAL DETAILS
See N.B. 458, Exp. 4
RT-2B3-D
* * " " "
H "
"
"
RT-313-D
* "
HT-331-D
Flow of control
0
0 0 0 0 0
3 3
3
3
3
0
0 0 0
7
Flow of treated Pigment
47. Barium hydrate 21-33
3% "
30
5% *
39
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10
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4
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0
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5
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46
4% Barium Hydrate 26
,.5^ .
DUP050315630
PIGMSKT COLOR RESEARCH REPORT XMPROVEHSKT 3 IH FTA PIG131TTS
INTRODUCTION
PILE: P PATE: MARCH-1935
A study of the Byev/orks Halopont colors from the standpoint of toner formulations was made during the past month. Although these products have merit, it was decided to discontinue work because of the low strength of the products having good lightfastness.
A new process has been developed which gives products superior in strength and lightfastness to BT-125-D but somewhat dirty in undertone.
An intensive studj$of sodium orthovanadate resulted in no new information. It was not found possible to prepare improved products through' the use of hydrate.
SUMMARY & CONCLUSION
A new process for the preparation of a molybdate toner of Vic toria Pure Blue BO- containing a small proportion of vanadate as in CS-7287. has been developed during the past month. The pigment is considerably stronger and better in lightfastnesslthan 31-125-3. it is dirty and strong in undertone and slightly green and equally clean in tint versus BT-125-B. It is ore pared by a reverse strike which gives a cleaner more lightfast product. It is necessary in addition to avoid a large precipitant excess and particularly a large acid excess.
'./here the cleanliness of undertone is important, a new Victoria Pure Blue 30 toner developed during the past month may be of inter est. It is very clean in undertone versus all Victoria lure Blue 3G toners heretofor prepared. It may be prepared equal in lightfastnness to C3-7736 and slightly weak. or close in strength and worse in lightfastness. It is prepared by the use of formic acidas in the toner formulas of the Haloponts- in place of sulphuric acid, formic acid gives a clean undertone and tint but for a given strength the lightfastnesn has always been somewhat worse than that obtained with sulfuric acid. The other essential features are a long boiling per iod and probably also a reverse strike. A mixture of 251 formic acid and 75% sulfuric acid appears just as good as 100b formic acid. It is possible that the valuable'feature is not specifically the formic acid but the more desirable pH conditions resulting from its use. Several strikes were made using this process with the dyes Icronol 31ue A3 and Lithosol East Blue SC-. Inferior product-: were obtained in both cases. Considerable experimental work was involved in the development of the lure Blue 3C toner and it is probably that similar efforts would be required with Acronol Blue AS and Lithosol fast Blue 6G.
Experiments with sodium ortho vanadate and zirconium tannate gave no new leads.
M'.:'
DUP050315631
2
A study of the effect of hydrate on PTA pigments gave no addi tional information. Hydrate dry maxed with the toner alters the bronze but does not give a cleaner or more pleasing appearance. Hy drate struck in or slurry mixed improved the finish and appearance but reduced the strength more than it increased the yield.
EkPGEIHENTAL DETAILS
Notebook 426
Vanadate Study 426-38. Study the use of vanadate in a molybdate toner, with out reducing the amount of molybdate. In this experiment the products obtained using vanadate were greatly inferior to the control.
426-37 Study the effect of volume of PTA solution, also study the effect of adding Sodium ortho vanadate after boil in.: the already precipitated dye 5 minutes.
In this series, it appears that the volume had no marked in fluence. The use of vanadate after the pigment was developing re sulted in a slightly dirty and weal: rroduct.
425-39. Study the effect of sodium ortho vanadate on BT-3S9D
an1. GT-3G7-D. It appears that the use of vanadate in the abcve-mentioned
orccedure? favors a slightly dirty product
426-41 Check several members cf rhe 3;
ro.es a J
;ud\ use
of zirconium tannate. In this series a dlecrease in dye resulted
a decrease in strength - ithout affecting the liig.hhtt stability
Zirconium tannate used in the h~thyl violet toner gave reo.
product, slightly weak and v.v.i worse in lightfastnesn.
426-42. Preparation of PTA toners using formic acid instead of sulfuric.
Jormic acid tends to produce strong toners, poor in 2igktfastness .
426-43. Study use of formic acid in a molybdate tener of Vic toria Pure Blue BO.
Pormic acid used in the Victoria Pure Blue BO formula resulted in strength and poor llghtfactneoe.
426-44. Study the use c-f vanadate cn the kho? a .in~ C GDI" and Victoria Green dyes; usin'- 41b as she basic proce Pure.
In studying the u p e of Vanadate on tire 4IB type procedure using Brhod amine 5 C-D1T and Victoria Green dyes, it was observed that the products obtained were somewhat dirty. Vo marked improvement in lightfastness or strength was observer.
426-45. Study variation of acid, and dye in a molybdate tenor using formic acid; also study a longer beiling period and use cf Gardinol.
Decreasing the dye and increar. ing the acid appears tc decrease the strength. The extended neriod of boiling tended tc produce a weaker pigment. The use of Gardinol in this experiment resulted in a somewhat weaker pigment.
V isah." Hm .
DUP050315632
3
426-46. Continu.aticn of the study of molybdate toners, using 43A as the b3,sic procedure.
B. made with a slight decrease in dye gave the best lightfastness of the series.
D- made using a cut in acid seemed to be somewhat stronger than A- the control,
C. made with a slight increase in dye gave a slight increa.se in strength.
426-47. Continued from 426-44C: study the use of vanadate when used in a Victoria Green d.ye procedure.
The use of vanadate in C gave a dirty weal: product with no marked effect on lightfastness.
Reducing the dye resulted in a decrease in strength, but no improvement in lightfastness was observed.
426-48. Continuation of 426-43 and 46; study use of formic acid and three hour boiling period.
jj'ormic acid gave a product weaker and worse in lightfastness than the control using sulfuric. Developing for 3 hours gave a slight improvement in lightfastness, accompanied by a slight decrease in strength.
426-49. Study the three hour PTA development of the Dyeworks. Three hour development period gave a marked improvement in lightfastness but also produced somewhat weaker pigments. However, these products were made using formic acid, and thereby the series as a whole was considerably worse in lightfastness than those made with sulfuric acid.
426-51. Study variables that seem to influence the cleanness of pigment, using 426-49C as the basic procedure.
Increase in volume from about 1500 cc. to 3500 cc gave a clean er and stronger product. Increase in dye gave a slightly stronger product, accompanied by a slight decrease in lightfastness, slight cut in acid did net seen to have any narked effect on the pig ment obtained .
426-52. Study the effect of sodium orthc vanadate when Victoria Pure Blue BO dye is used.
In this experiment, the use of sodium ortho vanadate gave a clean strong oroduct which v,ras better in light fart ness than DT-125-D.
DUP050315633
PIG-MSNT COLOR RESEARCH REPORT
3* --?*
PTA YIELD STUDIES
SURIvIITTSD BY: APPROVED BY: ^
%/
PILE: PTA"~C&L9R3 DATS: MARCH 1935
INTRODUCTION
PTA toner production still remains high with yields on the v/hole being only fair. Two batches from February are included in this r eport.
SUMMARY Sc COM PLUS I OHS
Average yields on the three 3T-100-B batches reported were good, being 99# of estimate. However, of these three batches, the first, held over from February, gave a yield of 106# of estimate and the last a low yield of 88# of estimate. This abnormal differ ence in yield on identically prepared batches can only be explained by pressing or drying losses especially since quality results are satisfactory in all cases.
A batch of 3T-122-D held over from February gave satisfactory ru'oont results and a yield of 106# of estimate.
Three batches of BT-92-D made during the month were satisfac tory tinctorially and gave a yield averaging 106',' of estimate. This is an improvement of 8', over a previous batch.
The yield on a batch of GT-354-D made during the month was very low being only 77# of estimate. Laboratory stripes on this color with no special attention being paid to yields shot- an average yield of 100-i/2# of estimate. This color was satisfactory tinctorially.
Average yields on two batches of GT-347-D were fair being 98-1/2# of estimate, a" decrease of 1-1/2# compared to previous batches. Satis factory tinctorial properties were secured.
The batch of 3T-95-D made checked a semi-works formulation (SW-6460) in which Duponol is used to replace Para Soap n the PTA solution. The yield on this batch was low being 91 d of estiiate or 6# under the yield of the previous batch made on this formula. The color was satisfactory tinctorially.
A batch of BT-125-D for 3T-150-D gave a low yield of 88-1/2# of estimate. This is a decrease of 5-1/2# under tne average yield of the two batches reported last month. Tinctorial properties still continued satisfactory.
Average yield on t^o batches of RT-392-R were low as compared
with last month, being only 96# of estimate,_a drop of 9, under last
month's production. Rubout results were satisfactory.
PTA toners still in process will be reported next month.
DUP05031 5634
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DUP050315635
PIGMENT COLOR RESEARCH REPORT GRINDIm OP TONER PULPS
SUBMITTED BY! M. dsl.W0u3 APPROVED BY*
PILE! &FGV"STUDTBS PATE: MARCH-1935
INTRODUCTION
One Batch of RT-7848-P (pulp of RT-359-D) was passed through the 12" Mikropulverizer to get rid of lumpiness in the pulp.
One hatch of BT-65-P (pulp of BT-125-D) was ground in the same pulverizer.
A portion of a plant lot of GT-67-P (pulp of G-354-D) was treated in the same manner.
SUMMARY & CONCLUSIONS
The action in the ease of each color ground was similar; namely that difficulty was experienced both in getting the pulps into the Mikropulverizer and in removing them from it. Especially in the matter of the feed the pulverizer is not as adaptable to the grinding of pulps as to dry colors. A decidedly smoother, more homogeneous pulp is, however, obtained.
Set up of Mill
100$ wt 100$ wt $
Speed
SW Number Color
in
out Yield Screen RPM Hammers
6869 6894
BT-65-P 10# RT-7848-P 11#
3# 30$ 5/8* 3300 Multiple
9# 81.8$ n
It
Lot 42378
GT-67-P
9-1/2# +80$
0
DUP050315636
PIGMENT COLOR RESBARCH REPORT RT-208-D 3?IRS T013SR
SUBMITTED BY APPROVED BY:
INTRODUCTION Pour plant Batches of RT-208-D were made during the month,
using ortho-chlor-para nitraniline from the Dye Dorks instead of freshly prepared material as made on the plant. A modification of the regular RT-208-D formula was used in making these Batches. A product Blue in tint was desired for use as a shading materia,!. SUMARY & 'CONCLUSIONS
The ortho chlor paranitraniline used was in Both dry and pulp (about 10%, dry content) form. On slurrying and screening.both the wet and dry form showed a large amount of pebble like material which would not break down ontihe screen, and which when dumped into the vat was undiazotizable. Both of the lots received (Lots 1 and 2) showed these undesirable hard particles, But lot 2 was somewhat Better in this respect.
The four plant batches gave substantially the same rubout re sult Being dark, weak and Blue versus the RT-208-D standard.
Yields were only fair, averaging 91% of estimate. This low yield is no doubt caused By the large amount of undiazotized material in the ortho-chlor paranitraniline which is used on an "as is" Basis.
4
DUP050315637
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DUP050315638
PIGMENT COLOR RESEARCH REPORT MBTA NITRO PARA TOLUIDIHE
SUBMITTEB b y * .APPROVED BY:
PILE: TSHttBiHrTXSffiR DATE: MARCH-1935
INTRODUCTION
A sample of meta-nitro-para-toluidine from Sherwin Willians was tested and compared with Du Pont material.
SUMMARY & CONCLUSIONS
The Sherwin Williams JSNPT wetted more easily and screened more readily than du Pont material. It also diazotised more rapidly and apparently more completely, giving a residue of about 0.5^ compared
with 1.0^ of residue from the du Pont MNPT. In the latter case,
the residue appeared to be mostly undiazotised intermediate.
Tested on the RT-386-D formula, the Sherwin Williams MtJPT was a substantial match for du Pont MNPT. The yields were equal.
EXPERIMENTAL DETAILS
Notebook No. 407, p. 88
DUP050315639
PIGMENT COLOR RESEARCH REPORT
n
MAROON TOKBR RT-354-P
SUBMITTED BY: CAPPROVER BY: ^
'i
5 a)- 9-
PILE* Miac. 'TOMBra DATE: MARCH-1935
INTRODUCTION
Two `batch.ea of CS-7685 were made in the Semi Works in a fur ther attempt to obtain material of standard depth and brightness on this formula.
SUMMARY & CONCLUSIONS
An increase in amount of Pigment Green B used to three times standard amoflnt resulted in a very dark hut brown product in lacquer. A mix of this and previous batches was equal in depth to RT-354-D but brown.
A reduction in alkalinity of coupling showed no increase in depth.
Fineness was satisfactory on both batches.
No further work on this problem is planned for the Semi-works, but the use of Pigment Green B for shading will be tried in the factory on RT-354-B.
EXPERIMENTAL DETAILS
N.B. #351, p.46
SW-6848. Check SW-6577 except increase Pigment Green B from 2.07 to 6.21#.
Lacquer Test - v.dark, brown Fineness - 99.0$ thru 80 mesh screen
SW-6854 - Check SW-6577 except reduce caustic soda in coupling from 39.33 to 37# and increase caustic soda in development by same amount.
Lacquer Test - s.light & brown
Fineness - 97.5$ thru 80 mesh screen
DUP050315640
PIGMENT COLOR RESEARCH REPORT
SUBMITTED .BY: APPROVED BYs
i:rrROBucTiQK
PEACOCK BLUE LAICS 3L-151-D
3./3* p il e : aasev-hasag DAYS: MARCH 1935
Semi-works production on this color has been resumed in an effort to secure green and clean shading material to mix off red and dirty substandard.
SULEIARY & CONCLUSIONS
The first batch was made on the standard formulation using Lithosol 3rilliant Blue E from the plant to check recent plant batches. The resultabt color was red and dirty with a heavy ink, checking the plant results.
The next batch was made using the same dye but cutting the soda ash in the base 10# to secure a lower consistency ink. This material was also red and dirty versus standard BL-151-D but gave a satisfac tory ink.
Using this modified base, a batch was made replacing the Lithosol Brilliant Blue E with a new shipment of Alphazurine special (RLE) 222}, An immediate improvement in the results were noted, the color being v.s. red versus the standard but other-wise satisfactory.
Checking the use of Xruponol in the dye solution, which gave green results in the laboratory, a batch was made in the Semi-worlcs using thisv ariable. Ko improvement was shown over the previcu s batch made without Duponol but as these are only press-cake results
they cannot be considered as final because of possible variations in drying.
DUP050315641
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DUP050315642
p is mo it c o l o r r e s e a r c h r e p o r t
P1GMEET RUBIAB TOHER RT-359-
SUBMITTED BY* APPROVED BYs & C&gJU/,
7
1PTRQDUCTIOH
PILE: aSSO-i--TCfHSRS DATE: MARCH-1935
Eour 'batches of RT-359-D were made in the Semi-works in a trial
of several variations which might be expected to give the yellowness of tint lacking in recent production of this color. It is suspected that the quality of the p-chloraniline m-sulphonic acid is the cause of trouble. Raw material tests show a slightly greater blueness of tint compared to standard material.
SUMMARY & CONCLUSIONS
All material made was dark and blue and although probably shadable is not suitable for present requirements.
A formula supplied by Jackson Laboratory, in which the dye is
developed and struck at 140 ^IP at the coupling volume, gave no promise of improvement.
Use of strontium chloride instead of nitrate gave a muddy bronzy product.
A check run on standard formula was dark and blue on control test. The toner was extended for use in RE-6857-D.
Part of a shipment of P.C.A.M.S.A. was purified by solution in alkali and re-precipitation. A toner made from this material showed
no improvement in shade. Separation of the dye after coupling and redissolving did not appear to be helpful.
A study of materials and of the process is being planned in the Research Laboratory.
DUP050315643
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DUP050315644
PIGMENT COLOR R3SB ARCH R3P0RT
3<T'?7
BLACK PIGMENTS
SUBMITTED BY: APPROVED BY:
INTRODUCTION
<3 FILS: MIgO. T0ISR3 DAT3: MARCH 1935
Du Pont Parlin found that the barium toner of Nigroaine vVSB showed promise as a black toning pigment for lacquer from the stand point of color, but that it was very hard in texture. Accordingly, work was started in the laboratory to prepare a barium toner of Nigrosine WS3 with satisfactory texture.
SUMMARY & CONCLUSIONS
During the preparation of a sample of the barium toner of ITigrosine Y/SB for further tests at Parlin. it was found that the preci pitation with barium chloride was incomplete and that the filtration was very slow.
Attempts to obtain complete precipitation of the dye with bar ium chloride under various conditions, such as acid strike, alkaline strike, boiling development, were unsuccessful. The addition of 25% alumina hydrate or of 25% carbon black did not improve the precipi tation. Treatments with turkey red oil and naphthenic acid*were'
practically without effect upon the precipitation or the texture of the pigment.
While searching for other metallic salts, it was found that basic lead acetate (lead liquor) gave complete precipitation. Nor mal lead acetate and lead nitrate did not precipitate the dye com pletely. By our own lacquer tests, the lead toner was slightly pur plish compared with the barium toner. The lead toner was also very hard in texture.
Samples of barium toner (^59-2A). lead nitrate toner (459-53) and lead acetate toner (459-5A) were submitted to Parlin for evalua tions from the viewpoint of color. Parlin reported that the lead toners gave similar results to the barium toner. It was Parlin's belief that we should continue our work to obtain soft texture on the basis of the lead toner.
A sample of (459-4) co-precipitated barium nigrosi ne and barium naphthenate on carbon black was also prepared. Parlin has reported that the latter sample (459-4) was unsatisfactory because of color.
BXPJBRIMSMTAL D3TAIL5
N.3. 459, pp. 6-23
Series 459-1 rc 6 tried the effect of turkey red oil, naphthenic acid- 25'S aluminum hydrate and 25-> gas carbon '"'-2ni in the precipi tation of the barium toner of Nigrosine "S3. None had any benefi cial effect on the hard texture, deep bleed, and difficult filtra
tion.
Series 459-2 & 5 prepared a sample of the barium toner of Nigrosine USB for Parlin.
5; DUP050315645
. 5^
2
Series 459-4 prepared a sample of Kigrosine 77SB precipitated on gas carbon W-201 containing barium naphthenate following 267-52B for Pariin. The result by lacquer grind was black, less red than 459-2. It tested OK in grit but was less black than C3-6519 by Parlin laboratory tests.
Series 459-5 prepared the lead toner of ITigrosine USB by sub stituting lead liquor and lead nitrate for barium chloride. The lead liquor (basic lead acetate} precipitated the dye completely and filtered rapidly while the lead nitrate did not precipitate the dye completely and filtered slowly. They were purplish versus 459-2A.
Series 459-7 studied the lead liquor precipitation of ITigrosine WSB. Lead nitrate, normal lead acetate, and acetic acid neu tralized lead liquor did not precipitate the dye completely. Small amounts of lead liquor added to these samples brought out complete precipitation. Therefore it appears evident that basic lead acetate is necessary for complete precipitation.
,VT '-j*'
DUP050315646
PIGMBST COLOR RESEARCH REPORT COLOR LAKES OP VAT DTgSS ABB ACE) DYES OH WOOL ACIDS
SUBMITTED BYl APPROVED BY:
PILE* ms&r-ht&gsDATE: MARCH 1935
IHTROBUCTIOK
lairatigatIons were continued on the preparation of lakes from vat dyes, and lakes from wool dyes ana wool acids. .The re
sults of studies on this problem, which was mentioned in the Febru ary report, have been more one ouraging this month, and altho no definite conclusion can be drawn at this time as to the workability of this problem, the results obtained warrant continuation of these investigations.
s u mma r y & c o s o x s s io h s
The present methods employed for the preparation of lakes from vat dyes involve the mixing of the vat dye paste -flth a wetted sub stratum, The dyeing of cloth with vat dyes is accomplished by vatting the dye, e.g, obtaining the dye in a soluble or highly disper sible form prior to the addition of the cloth or fibrous material to
the dye bath and then subsequently precipitating or coagulating the dye by oxldatiop or other means, on the fibre*
The preparation of alumina hydrate lakes from vatted and dry
dispersible Pensol Blue GD and Jade Green Supra dyes has resulted, in several cases, in odor lakes superior to those prepared by ordinary mixing of the dye paste with the substratum. The improved
products are stronger, cleaner and more brilliant in shade and tint than the lakes prepared by ordinary mixing.
The use of wool acids (dissolved wool) in the preparation of lakes from acid, anthraqulnone, and chroaable dyes did not at first appear very promising. However, further orientation experiments have resulted in products possessing some merit and recent results
are sufficiently encouraging to warrant further investigation.
EXPERIMENTAL DETAILS
Vat d.ve Lakes
Indianthrene Blue 2g h s l Alumina Hydrate Lake
Expt. 450-40 H.B. 450, page 13d
Ponsol Blue GD) on blanc fixe and alumina hydrate.
Jade drees
)
Expt, 450-41 & 49 H.B. 450, pages 138 & 176.
Wool Acid Lakes
AnthraqtAione Blue A3
on blanc fixe and wool
pontaehrome Azure Blue B acids
Expt, 450-35, 36, 38 & 42 H.B. 450, pages 116,
120, 130 & 142.
DUP050315647
PIGMEBT COLOR RESEARCH REPORT
SULFOGSHS BRILLIAST BLUE 5 GCF
SUBMITTED BY* APPROVED BTs
INTRODUCTION
*23
PILE* JKSCv-LAKEB DATE: MARCH-1935
A sample of Sulfogene Brilliant Blue 5 GCF (B#1928) was evalua ted as a possible substitute for Indanthrene Blue 2 GSNL in BL-86-D. Consideration was also given to the dye for possible use as a DryDispersible Color or as pulp color for paper coating.
SUMMARY & CONCLUSIONS
Lakes were prepared from Sulfogene Brilliant Blue 5 GCF by pre cipitating the dye solution with barium chloride on various bases which included all alumina hydrate, mixtures of alumina hydrate and blanc fixe and all blane fixe (freshly precipitated). It was found that the texture of the lake became harder, the strength was decreased slightly, and the lightfastness was improved as the amount of alumina 6 hydrate in the base was decreased.
The above lakes were tented by lithographic varnish rubouts, by Duluac and Duco grinds and were compared with BL-86-D. The lakes
from Sulfogene Brilliant Blue were all redder and dirtier in tint, and distinctly worse in lightfastness than BL-86-D.
When prepared as a dry dispersible color on a barytes-alumina hydrate base, the pigment was very hard in texture and possessed very low tinctorial power. It was found that the use of freshly precipi
tated barium sulphate gave a decided improvement in texture over reslurried barytes or blanc fixe,
Brushouts in casein vehicle showed the barium toner pulp of Sulfogene Brilliant Blue to be inferior in lightfaatness to B2-134-D and Ultramarine Blue.
BXPBRIMEIgTAT, WSTATTS
Notebook Ho, 307
Series 307-46 was the preparation of a 13,5^ lake of Sulfqgene
Brilliant Blue 5 GCF on blanc fixe and a barium toner. The toner and the lake were both very hard in texture. The lake
was considerably harder in texture and weaker than B#1878, a lake prepared at Jackson Laboratories.
Series 307-47 were preparations of 13.55& lakes on various types of bases ranging from all hydrate to all blanc fixe.
Soft textures were obtained in this series. Lightfastness was improved as the amount of hydrate in the bases was decreased. Texture
became harder as the hydrate was decreased. Compared with BL-86-D, the lakes of this series were redder and dirtier in tint and inferior in lightfaeineea,
Series 307-48 was a barium toner pulp from Sulfogene Brilliant
Blue 5 GCF. Brushouts showed this color to be Inferior in lightfastness
to Ultramarine Blue and B1-134-D.
DUP050315648
PIGMSRT COLOR RESBARCH REPORT RAW MATERIAL TESTING
3$-'foa
5%
'
SUBMITTED BY: APPROVED BY:
PILE! AW-MATSRBtES DATE: MARCH-1935
The four samples not finally reported at the time the last report was written have since been satisfactorily tested.
This month 106 shipments of raw materials were received and
sampled, and have the following status: 58 tested in the laboratory and found to he acceptable; 4 satisfactory when previously tested; 8 OK In the plant; 1 handled by the Research department; 1 for Semiworks consumption; 1 awaiting completion of analysis and 32 reported
without test.
A shipment of Anthranilic Acid from du Pont when tested an the RL-211-D procedure resulted in a muddy masstone. Various methods were employed in the laboratory in attempts to clarify the product, the most satisfactory, comparatively, being a salted out dye made
without any special treatment in its formulation. The muddiness was
to some extent decreased but the masstone remained flat. The ship ment was rejected.
RAW MATERIAL ^SAMPLES
There are no samples outstanding from previous reports.
Eleven samples were received this month:
RMS 1388 Lake Red CR Pulp from Sherwin-Williams. Unsatisfactory too bronze in undertone.
RMS 1389 Trisulphoil Soap from Scholler Bros. - Satisfactory. RMS 1390 Alphazurine 3?.G. Cone. Special from Rational Aniline - Sat
isfactory.
RMS 1391 Lake Red CR Pulp)
1392 * * ) from Sherwin-Williams. Unsatisfactory,
too bronze in undertone.
RMS 1393 Azo Bordeaux from General Dyestuffs - Unsatisfactory too blue in tint.
RMS 1394 Azo Bordeaux from Rational Aniline - Satisfactory RMS 1395 Lithosol Scarlet Bade M from du Pont - Satisfactory RMS 1396 R Salt P.E. Paste from Rational Aniline - Unsatisfactory-
too dark RMS 1397 Azo Bordeaux from Rational Aniline - Unsatisfactory - al
cohol bleed too strong. RMS 1398 Methyl Violet R for Lakes from du Pont - unsatisfactory com
pared with Standard Methyl Violet Paste - not same type.
DUP050315649
FIGMENT COLOR RESEARCH REPORT
SEMI-WORKS PRODUCTION
ityl,SUBMITTED BY:
.
APPROVED BY;
,
-fif PILE; sUE=aeDATE: MARCH-1935
INTRODUCTION
75 Batches of 19 different colors were made. These included 20 hatches of lightfast green G-389-D, 12 hatches of Y-315-D, 7 hatches of RT-300-B, and 6 hatches of RT-7745-D.
SUMMARY
RT-265-D, Calcium Duol - Three hatches were made for production of yellow tint shading material.
RT-300-D Calcium Lithol - Seven hatches were made for the pur pose of improving the formula for this product.
RT-359-D, Pigment Rubine - Pive hatches were made using varia tions tending to give yellower material.
RT-7745-D- Permanent Red 2B - Six hatches were made completing, for the present, work on this new color.
RT-354-D, CS-7685, Maroon Toner - One additional batch of this improved grinding product was made.
RT-7848-P. pulp form of RT-359-D - An 8# sample of RT-359-D press cake was micro-pulverized.
RL-7836-D, Lake Red C Toner for Rubber - One hatch was made in a trial of the formula for this new product.
RP-7664-D, Barium Lithol for Rubber - Three batches were made to obtain additional material and to check the consistency of the process.
RP-7665-D, Calcium Lithol for Rubber - Two batches of this shade were made for the same purpose.
RE-6857-D, Ext. Pigment Rubine - Two batches were made for pro duction.
RE-381-D, Scarlet Lake for Dry Dispersion - One batch was made to fill an order.
Y-309-D, Med. Yellow - One batch was made in trial of an im proved formula.
Y-315-D, Primrose Yellow - Thirteen batches were made in dev elopment of an improved product.
BT-65-P, BT-125-D in pulp form. A small batch of this color was micropulverized.
BL-151-D, Peacock Blue - Pour batches were made to obtain super ior material.
BkL-6619-D, Treated Black - One batch was made for Parlin. BT-150-D, PTA Toner - One batch was made in a yield study. G-389-D, IdJjht Past Green - Twenty batches were made in continua tion of the process study being made. GE-388-D, Ext, PTA - One batch was made to fill an order.
23 mixes were made in the Research semi-works for the planifc during March, 1935.
DUP050315650
2
Mixing
PTA Toners Blue Lake Red Toners Yellow Bulk Lake CP Yellow CP Orange CP Green
Charge
751-s
It
n
758-s 753-s 754-s 755-s
*
Batches
4 2 1 1 3 2 10
2*
lbs
703 417 259 895 1000 1037 5523
*83*
DUP050315651
!flO b u i l d i n g PRODUCTION REPORT FOR MARCH 1935
o 35
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0%
ro o X o 0 7 o --1 H
in S. o n o ?o x X
i
CM
n T> CM n CM :o co ro ro m t
CM
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n
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DUP050315652
I
SUMMARY .Off #10 B1DG. PRODUCTION REPORT POR MARCH - 1935
Mo. Batches
Code
3 RT-265-B 7 RT-300-D
4 RT-359-2) 6 RT-7745-D 1 RT-354-3? 1 RT-7848-D
1 RL-7836-D 3 RL-7664-D
2 R1-7655-B 2 KB-6857-B
1 RE-381-D 1 Y-309-D 12 Y-315-3? 1 BT-65-P 4 BL-151-D
1 BkL-6619-D 1 BT-150-B 20 Gr-389-B 1 GE-388-3)
lbs. Struck
708 574 120 136 140
-
62 414 236 1479 318
39 468
10 204
13 32 676 252
5851
lbs. Packed
723 566 113 137 140
9 61 403 230 1432 328 34 430
3 213
13 30 642 249
5756
% Yield
102.1 98.5 94.1
100.6 100.0
98.3 97.3 97.5 96.2 103.1 87.1 91.9
-
104.4 100.0
93.8 95.0 98.8
97.5
DUP050315653
MATERIAL TRANSFERRED DURING- MARCH 1935 EROM RESEARCH SEMI -WORKS
Lot 3999
4000 4020
4024
CR-200
6
6 6 6
Color Gode SB -36*3-D
RE-6857-D RE-6857-D
4002 4003
4004 4005 3718
10 YR-324-D 10 n 10 10
10 RX-7516-D
4021 4015
11 RE-381-D 11 BMf-6619-3)
4014
12 RT-219-D
4039
25 RT-329-D
4011
132 G-7764-D
4030 4031 4035 4032 4033
4034 4036
4037
4040
1 1
RT-26 5-D
1
1 RT-354-D
1n
1W
1 RT-300-D
1 It
1 RT-354-D
4026
4027 4028
2 GX-7826-D 2 SX-7828-D 2 GX-7827-D
4017 4023
3 Y-305-D 3W
4022 4038
4 G-389-D 4 G-317-B
4025
5 B-160-B
lbs.
271 356
475 957
Groub 2 2
2 2
Cost Unit 9.94
11.28
123 2 133.56
122 2
124 2
124 2
58 2
32.00
330 1 13 1
16.03 60.72
27 1 803.95
41 2 312.18
1191
11.99
236 2
236 2
236 2
140 2 114.49
144 2
142 2
82 2
69.48
83 2
426 2 114.49
70 1 159 1 150 1
7.58 9.02 9.10
267 2 259 2
7.89
187 2 169 2
12.09 11.31
350 1
30.03
Total Cost
DUP050315654
/ 26
RBCAPITULATIOK
Colors transferred from Semi-Works to Plant during March, 1935.
Toners Ext. Colors Yellows
Greens Blues
"BE** Lakes "RP1* Lakes
"EL** ** "RM** ** Maroon Tonerg PTA Toners
1725# 379 526
1547
350 2389
493
58 13 27 . 41
Total 7548#
In addition to the above please credit Semi-works with 7# GT-68-P at $65.04 per 100#, as same was used In toners (dry),
which I will debit to Croup #1 in my monthly report.
DUP050315655
J#ATj2HxAL"iN PROCESS" AS OF APRIL I ,
19S5 - RESEARCH SEMI-WORKS ft 10 RLDG
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CO
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DUP050315656