Document JQJGoDNv9JLjqXr75RdNMYGv

E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Copy No. 1 ^ \ V, ' nf'V- \ * 2. o2Y t NEWARK PLANT PIGMENT COLOR RESEARCH REPORT DIRECT LAKING FORMULA FOR RT-525-D, K-2302 (Mb toner of Lithoeol Red 2B) Period Covered: January 9 * 1946 to June 12 9 1946 s. NJ027B FILE: ^^ DATE: 9/3/46 N39971 /fv /- Serial Ha. KJM6*59 CojV No. 1 Copy tat #1 * Humerioal rile 2 Research Qffioe (222*24) 3 - A. Siegel/Library File (222.24) 4 - #10 Building File 5 - #6 6 Imperial OheariLoal Xaduetrlea, Ltd. ,, w a w* 9 - W* F* Bpengemaa, Beaark KtEBTARg f|4Ff PiafflElif COLOR RESEARCH REPORT Fragraaa Report Title! DIRECT UIHd FORMULA FOR Rf-52JM> * K-2302 (Ha toaer of Lithoael Rad 2B) Period Covered! January 9 1946 ta June li 1946 SURMimi) BYI appr oved by DATS SOBHZTESDi Ally 29, 1946 DAYS ISSUES*. 9/3/46 N39971.01 DUP050150172 A direct laking formula for the manganese tenor of Lithosol Bod 2B dye. RT-525-D Bad been developed ao reported la KK-45-45. However* this product, K-2178* wee somewhat darker and duller than was desirable aad was aloe very week in tinting strength. Zn Tie* of the expected inereaee in demand for HT-525-D it uee decided to renew the attempt to derelop a hettir natch for the preeent etaadard with the lew cost which le peeeihle using the direct laking procedure. mMLmjmmm A new formula* K-2302, wee developed which differed froa K-21?8 in the following rospeet* 1. The coupled code oalt wae run into manganese sulphate held at a toil instead of the latter being added to the BOJJ eolation before coupling. This change reeulted in greater intensity of meetone enanel end in increased blueness ef tint. 2. Use of para seep in the coupling wae necessary for depth of assetone and blueness of tint. 3. An increase in batch site was made to utilise ooppoidyioffthe additional strike vat required in K-2302. The product obtained on this formula was net as dark or as strong as RT*525** and after this was confirmed by a Send-workc trial, further nodifloat!on was node. It was found that depth and strength could bo Increased by use of accessory first components, preferably by replacing 1.3^ of the Idthocel Red 2B aeid with ortho-toluidine-meta-BUlphonic acid. The product obtained was slightly Mrs intense than RT-525- in ttasstone enamel and only a trass weak and blue in tint. This formula was also triad in the' Bead-works and gars a produst darker than standard. Strength ean be further increased by reduoing the amount of disedium phosphate in the coupling, ^fcis however has the added effeet ef reduoing intensity to some extent. Cists calculated for the K-2302 formula indicate a possible savings ef $36.10 per 100 lbs. compared ta RI-525- mads from Lithoeol Bad 2B dys. It is not planned to write a new formula for the modification ef K-2302 employing the accessory intermediate until plant trials haws been mads. All modifications ef the original K-21?0 which employed a direct method of strike - manganese sulphate added te the BOB solution or to the coupled soda salt-failed te give the deisred depth, strength and blueness. Slight improvements on K-2178 were ashiovod by use of para soap in the ocupling and by control ef tbs alkalinity ef dsrelepmont obtained by adjustment ef pH after the addition ef linSOe from 8.5 te 7*1 - T.* allowing the pH to fall DUP050150173 below 7*0 during the development rooulto la exceptionally wook produotf of Salts present la the slurry* Dilution of the slurry at this poiat to as audit as four times the original voluao was practically ineffective* The poooiblo offset of the salts woe avoided by reversing the order of trike and running the eoupled soda salt Is the manganese sulphate which was hold ot s boil* this resulted 1s as increase is the intensity of full shade enamel and the blueness of tint* Is combination with the use of accessory first components the reverse strike aloe appears to bo essential for maximum depth, strength and blueness* A number of intermediates were tested for their aooeoeery effect when substituted la small amounts, for Lithoool Red 29 add* Of those ortho-toiuidinemeta-sulphoaie acid , used la amount equal to 1*3$ of the bed 2B sold, gave the boot tinctorial aateh for RT-525-D* Otlfer properties such as opacity and baking resistance were only very slightly inferior* Hbtrtwasfcer bleed mao increased but wao only slightly poorer than RX-525-0 The decreasing order tfl effectiveness * 0T1SA, PTOSA and FTUSA is of interest in connection with peosible causes of the accessory action* Of those intermediates there appears to bo some correlation involving cheadcal structure, for example the relative positions of the amine and aulphonio acid groups oeiqpared to Rod 2B add* It is also poeoible that the offset Is duo to the greater solubility of the 0XB8A - BOH salt* The QTM8A used in the laboratory experlisente (D-4795) was purified sodium salt having a nitrite value of 73*8$, equivalent to 66.0$ as free acid* This material contains about 25$ moisture or water of orystallisation* A more recent sample of Ha Salt, D-6275, gave Idential results and a sample of QTMSA crude, analysing 95*7$ as free acid was equally satisfactory* wmmjiiL 1147331 32 33 34 35 36 37 -38 39 40 -41 42 -43 -44 -45, -46 04? Modifications of K-2178. OmiBBion of disodlua phosphate* Lower pH of coupling* Para Soap usd ether agents in coupling* Reduce alkalinity ef coupling* Reduce amount of ungaasso sulphate* Ditto Boat development of Ha salt befors strike* Adjustment of pH of Hasalt before boating* Toner fro* isolated fere eenpsred to direst lake product* Modifications of K-21?8 using RT-4284) direct process* Time and tesgeraturo of development* Longer development tine* Reverse order of strike Ha salt into HnBO* K-2302. Roehook Bxp. 43. Reduce amount of manganese sulphate in #43 formula* Znereaoe volume of development. HnSO* into Ha salt* Reveres strike, oadt phosphate* Reduce alkalinity* DUP050150174 *3* U47-48 Reeheek 114T-46 #49 Jtoid tfs ow^U)Ut 50 Omit phoephat. Xneroaoe alkalinity tf itrlki. -52. Doe of other buffor* ia coupling* 52 Similar to Sap* 4f -53 Rcroroo strike* Reduction la amount of phosphate* *|4 Doe of accessory first eoag>oaento* -|5 Vary amount at OTRBA and P6AM8&* 56 Vary amount of P08A* 57 Vary amount of Lake Red 0 Base* 56 Vary amount of FTHSA. 55 . Caspars direct and reverse strike using OTMSA aa aeeeseory first 90^0tt4Al -to Addition of sodium rosinato to K-2302, -61 Casparloon vmh erode and purified* 62 Coaparleon omi trade and piodfled* t DUP050150175