Document oXdO9n1XXOa6g702omeayMw8

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Serial No. KN-48-6 Copy No. 1 NEWARK PLANT PIGMENT COLOR RESEARCH REPORT RT-455-D Period Covered: SEMI-WORKS DEVELOPMENT AND PLANT DEVELOPMENT AND STANDARDIZATION OF THE DIRECT LAKtfC PROCESS FOR ROSINATED RED 2 B TONER* November 1944 - March 1947* NJSA7B .. FILE: DATE: 5/20/48 N42155 .. .. Serial So. KN-48-6 Copy No. i Copy to* 11 * Nuasorieal Filo 2 - Research Offlee (222*24) 3 - Lihrary Filo (222.24) 4 - #10 Building file J*T Chalupeki, Float files 6 - Inperial Chemical Industrie** Ltd. 1m e Q,, * * * 9 W. F. Speagesan, Newark 10 - Extra HEVISE PLANT FIGMENT COLOR RESEARCH REPORT Final Report Title* 4 RT-455-D Sead-Works Development and Plant Development and Standard!cation of the Direct Laking froeeso for Resiaated Red 2B Toner* Period Covered* November 1944 * Sards 1947. Charge* 1100-12-33 (A-IC-33) SUBiOTlSD BY* S. J, Hee DATE SUBHIT12D* 5/6/48 APPROVED BY s C.lfforriooa >/#/ DATE ISSUED* 5/20/48 DUP050066936 -1 INTRODDCTIOH th# Seal-fork* development study on tit* direct taking economy formula for 87-455* was started in. November, 1944* Laboratory vork on tbit rosimted "Watchting" rod ton*r bad shown that a fairly eatiafaetory match to tba "isolated dye1* standard could bo obtained at a saving of upproxiaately twenty sent* * pound (so# KH-44-74). 7b* original laboratory formula, K-2052, required number of shaagos, nscossltatlng more laboratory work, boforo tbo plant atudy was started. "N*.' Semi-Works manufacture on tbo laboratory formula, K-2052, ni eonsiderably dark and dull la mass*on* and blue la tint versus both th* K-2052 laboratory standard saspl* and tbs *lsolat*dN dy* type RT-455- standard* lot 31554* As tbo quality of tbo K-2052 sampls (graded a dark - OK - a blu* versus lot 31554) rsprooeated ib* maximum desirable donation from tho "isolated dys* standard known variables wars applied In an attempt to obtain tbo doslrod quality but without sueosss. It was finally decided to use another formulat 940-55Ba as a basis for tbs study. This entailed a east penalty of about five esnta a pound resulting principally from th# us* of oaustio soda and calcium ohloride as the source f' of alkali and tbo precipitating seta! instead of hydrated line* A Semi-Works batch made usingth# 94055Ba formula ground out light and blue versus K-2052 and tbs RT-455* standard* Subsequent manufacture made using variables designed to give a darker, yellower product (lowered coupling tempera ture and elimination of tho lump baking step wore the principal variables tried) averaged dark in mansions and strong and intense In tint versus tbo laboratory standard. Meanwhile, the first plant trial batch of tbo direst taking foraula was scheduled for April, 1945, A procedure similar to 94Q-55Bg except for a cut in coupling temperature (55*f instead of 86*F,) mao used as tbo basis for tbs plant study. In tbs early work, th* eight hour taking at l30*f# (after drying at 140*F) was eliminated in order td supply dark, yellow shading material to consume existing light, blu# substandard ("isolated dye* formula production), and it was msesasary to include this step in the standardisation work. f. s - > The considerable masstone j>th increase .resulting from the use of 180F, taking mads it necessary tot use a combination of a number of light maestoso fSSPfk1! SMffi x\m<' , ,, >"i ' . >- ,.ti 's'*. 'V\ ,, 0 V*c h& tom. tM)b 4. direct 'lakinK.fOPmulaifoit Uiti^pwofeSia8twtiitaE'ftotata*iimo Poyem^er, IMJkend designated K-2236. K-2236 was based upon the procedure then in use in the plant and differed from the laboratory direct taking process, Kv2QSta aasfoumm* ws* ot^stia. mm~ m - 1* The use of lime was eliminated? caustic soda is used as the source of i.... DUP050066937 -2- alkali and oaloium chloride as ths source of oaloium. 2* Hapbthenic aoid las boos eliminated from the process. 3. Tbs rosin amount bus boon increased 25$ (replacing the naphthenic sold) wad K Wood rosin las boon substituted for M. Gum rosin. 4* Tho use of both sodium acetate and ammonium chloride as buffers has boon introduced. 5* Tbs diato solution volume and ths BOH solution volume bsfors coupling bars boon approximately doublod. 6. Slight increases in tbs solution teaperaturee of tho intermediates baud Yimrnm mmAm* K-2236 showed a saving in total cost of approximately twenty cents per pound compared with the"isolated dye" formula, K-1422. A good part of tbs saving is a result of tho increased batch else mad# possible by us* of the direct laking formula <550# for K-2236 as cenpured with 307# for K-1422 in a 10,000 gallon vat). A portion of a batch (lot 27698) mode on a slight modification of tho K-2236 formula was baked at 1@0*F. in the Bead-Works as lot 8609 (tbs maid portion of the batch was not baked), mixed with 10$ Blase fixe, and sot itp, in April 1946, as tbs plant standard for direct laking RT*#55"D, lot 0643, A rubeut comparison Of lot 8643 versus the"isolated dye" formula standard, lot 31554 follows* Lot 8643 vs Lot 31554* s dark, intense - vs blue, higher bron*o - OK - s blue Light fastness* equal A dirset laking RT-455-D standard formula, K-2313* bassd on lot 8643, wast set up to replace the "isolated dye" procedure, K-1422. K-2313 differed from tho direct laking "costing" formula, K-2236, as follows* *1. Tbs BOH solution volume before coupling has bson out about 15$. This is equivalent to an approximate 20$ increass in the BOH volume used for the laboratory K-2052 procedure. 2. Approximately 10$ Blase fixe is added to ths BON solution before coupling to adjust to standard strength. 3. Eight hour baking at l8oF, subsequent to drying at 140"F has been incorporated in the formula. 4. Fins grinding to give satisfactory material for rubber is formulated although lot 8643 was not fine ground. tfeaaqiile, there had boon no plant manufacture on tho direct Inking procedure from December, 1945, to April, 1946. Production mao thin resumed on the basis of K-2313* nineteen batches wore mads during ths period April, 1946 Harsh, 1947 The majority of those batches mere dark and yellow (twelve of nineteen batches) probably a result of variation in raw material quality. Most of those batches ware shipped without shading because of tho heavy demand for DUP050066938 organic pigments and the short supply of intermediates during thie period* Attempts to obtain lighter masstene by lnereaoing the BON solution volume by 1C$ acre unsuccessful. Subsequently it ass found possible to obtain light shading notorial by ineroaaing ths coupling toaporature to 80-85*F. Caro mist be exercised in using this variable because of tho possibility of obtaining weak usd dull material* Tbo use of Ootanol as sn anti-foaming agent apparently gives a aery slight increase in bluinses of tint* A slight decrease in foaming resulted but ss there aas no *wasb out* difficulty aith RT-455-D as aas experienced aith RT-428-D (see KH-47-21) tho uso of Ootanol was not introduced into tint otandard RT-455-0 formula* As in the ease of ths other Bed 2S colors tho erroneous suppliers analyses of the Red 28 acid aas corrected by analysingtho sodium salt solution ef ths intermediate in the vat before diacotisation and adjusting as required# A new standard formula, K-2444, was aritta which differed from ths previous formula* 8*2313, ral? in tho introduction of tho Red 2B acid analysis step* Ths usage of tho intermediate per batch was increased by 55 which represented the average difference between the suppliers analysis and ths corrected figure* Meanwhile, attssfts ware nsde to set up a mere representative plant standard by blending a number of batches* The first ef these, let 49275, a blend of five batches, was submitted as a proposed standard in Oeteber, 1948* Although color properties ware satisfactory (slightly darker and yellower than let 8643) the let was rejected because of an undesirable lacqusr overstripe bleed which was probably due to contamination* A second proposed standard, lot 80468, submitted for evaluation in April, 1947, ae also rejected for tho earns reason. Because of those contamination difficulties the Production Division agreed to accept supervision of manufacture of RT-455-D without reotandardisation and thie was done in March, 1947* Production was finally successful is sotting up a satisfactory replacement standard for BT*455*D, lot 82960, in December, 1947* There is no patent restriction is the manufacture of Red # 603009* It is not believed that thie study has resulted in any patentable The roainated calcium salt ef the coupling of Red 2B acid diaio and Beta hydroxy naphthoic acid* Aboit l6j of Calcium roainate and 9*# of Blano fine are present In tho finiehed toner* DUP050066939 RT-428D The calciua-streatiua salt of tho coupling of Rod SB aoid dia*o and 80ta hydroxy naphthoic acid. Red 2B Aoid Ortho oblo? acta toiuidine para sulfonic aoid* . hydroxy naphthoic aoid* of tho Rad SI dyestuff. Preparation of tho finished pig&ent from the fcaeio intermediates without isolation^or removal of the mother-liquor free the dyestuff. RT-455-8 Seasi-^orke D8N*48-3 Part I RT-455-D Plant DSS-48-3 part n .v.-w.* DUP050066940