Document 9Jj1eLzGgB6G59aV68jk04mqL

/ E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOl STREET NEWARK. NEW JERSEY Copy No. -1 Numerical Fila STM ' NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report CALCIUM LIXKOL RED LAKE FOR RUBBER, RL-408-D DEVELOPMENT AND STANDARDIZATION OF ECONOMY PROCESS * Poriod Covorod: MARCH 1946 - AUGUST 194? FILE. DATE: 222all 1/6/49 N42184 ^, \ // Copy to* #1 * Numerical File 2 * Research Office (222.11) 3 - Library File (222.11) 4 * #10 Building File 5 V. Chalupski, Plant Files 6 - 9* F. Spengeraan, Newark 7 - Extra, Serial So. KN-48.38 Copy So. 1 NEWARK PLANS PIGMENT COLOR RESEARCH REPORT Final Report CALCIUM LITHOL RED LAKE FOR RUBBER, RL-408-D DEVELOPMENT AND STANDARDIZATION OF ECONOMY PROCESS. MARCH 1946 - AUGUST 1947 SUBMITTED Mi E* I, Hess APPROVED Bit J. 0, Morr (yml4K DATE SUBMITTED* 12/23/48 DATE ISSUED* 1/6/49 DUP050067115 mami3ss Development work on standardization of an economy dry mix process for the calcium lithol red lake for rubber, RL-408-D, eras started in March, 1946. Failure to obtain a satisfactory product made it necessary to devise another means of obtaining the desired saving* dales finally authorized standardization at a lower strength (decreased toner) level to solve this problem* Preliminary investigation in the laboratory indicated that the following blend would give a satisfactory match to the RL-408-D standard, lot 4505, at a saving of about two cents per pounds RT-425-D (K-2058 type) RT-364-D (K-2057 type) RT-432-D Blanc Fixe 52*75# 21.00# 4.25# 22*00# Before laboratory work was complete, RT-364-D was eliminated from the blend because of the possible patent Infringement complica tions resulting from the use of this naphthenatsd toner in mixes with rosinated products* Attempts to set up a dry mix RL-408-D from RT-425-D, RT-432-D and blanc fixe on a plant seals were unsuccessful* The following blends were made and rejected for the reasons Indicated1 isi RabkaK-iaal.-15Q5 48428 49089 6# str. * ws bl* OK - yellow too strong Lot 49089 based on 48428 therefor probably nonuniform* Subsequently, on the basis of the Sales* decision to lower the toner content of RL-4O8-D to give a product 10# weaker than lot 4505, lot 49089 was reduced with blanc fixe to the desired strength. However, before teste were made on this material (designated lot 49628), it was decided that much of the previous difficulty withthe dry mix process was due to the unsatisfactory resistance of the com ponents to tide rubber curing process* Work on the dry mix procedure was abandoned, therefore, and restandardization in the plant of the normal K-1611 type process at a lower strength level was started. Standardization of a modified K-1611 product at the desired strength level was accomplished by increasing the blanc fixe extender by about 56#. A new RL-408-D standard,' let 81660, replacing lot 4505, was set up and a new RL-408-D standard formula, K-2509, replacing K-1611,* was issued in August, 1957* The Production Division assumed supervision of manufacture of RL-408-D in August, 1947* DUP050067116 m<sasiiflEt Preliminary work In the laboratory during late 1944 Indicated that a satisfactory match to the RL-408-D standard, lot 4505, could be obtained with the following blend of economy lithols add "Duols"* RT-425-D (K-2058 type) 52.75% RT-364-D (K-2057 type) 21.00% RT-432-D 4.25% Blanc Fixe 22.00% A saving of approximately two cents per pound in mill cost would result from the use of this process. Before large scale work was^started It was decided that a possible patent Infringement WsmnihrtKliedln mixing of pigments con taining naphthenic acid (RT-364-D) and rosin (RT-425-D and RT-432-D). This problem was Inactive In the Research Laboratory during 1945 although a satisfactory product using RT-425-D and RT-432-D and eliminating RT-364-D from the mix was developed in the meanwhile by Sales Service. An apparently;7 satisfactory blend consisting of 76.6% RT-425-D. 1.45 RT-432-D and 22,0$ Blanc Fixe was issued as K-2388 in August, 1940. Meanwhile, a proposed RL-408-D standard, lot 40428, based on this formula, was submitted for evaluation. Lot 48428 was apparently a satisfactory match to lot 4505 <6% str.- ws blue in rubber) except for a slight strength advantage* Because of the extra strength It was decided to dilute lot 48428 with about 4$ Blanc Fixe to obtain a product closer to lot 4505* This blend, lot 49089, was made and a process based on the new blend was issued in October, 1946* The process, K-2397* had the following composition* RT-425-B (K-2058 type) 73.60% RT-432-D 1,35% Blanc Fixe 25.05% Lot 49089, by rubout test, was equal in strength but yellow in tint versus the standard, lot 4505* At the time it was thought that this change from the vys blue tint result obtained with the original material, lot 48420, compared with the yellow tint of lot 49089 was due to some non-uniformity of the blend. Meanwhile. Sales had decided to lower the tinting strength of RL-408-D by 10% in order to effect a further aavlng of about three cents per pound in mill cost. Accordingly, let 49o89| was reduced further with blanc fixe to obtain the desired strength. This blend, lot 49628, was never evaluated as a proposed standard* however, as further study by the Sales Service laboratory indicated that the tint change pre viously noted was due to inferior resistance of thedry mix product to the rubber curing process rather than to non-uniformityl there DUP050067117 ~3 was some question at the time as to whether the use of a new electric curing press rather than the regular steam press was responsible for the difficulty but it was finally decided to rsstamdardlss on the basis of a K-l6ll type product at a lower strength level. Accordingly, in Hay, 194?, plant manufacture was started using a modified K-1611 procedure. The principal change was an increase in the blanc fixe extender amount from 28* to 33*. a series of sight hatches mads on this formula averaged about 8% strong and slightly blue In tint by rubber test versus an adjusted standard Clot 4505 adjusted downward 10% in strength). Five of these bitches plus sufficient blanc fixe to give the desired strength in rubber were blended to give the proposed standard, lot 8166O, which was submitted for evaluation in June. 1947. A com parison of lot 8166O versus the RL-408-D standard, lot 4505, follows* Lot 81660 vs lot 4505* light, yellow - weak (115100)~ vs yellow. Light Stability1 MT:equal Tint* va superior. flttfejfefiOfiaM.. Lot 81660 vs lot 4505* weak (110*100) - vs blue. Migrations 0,X. Lot 81660. was accepted by the Sales Division as the H1-408-D standard in August, 1947, and a new standard formula, K-2509, (now designated RL-408~D(A)3, was issued, K-2509 differs from the pre vious standard, K-1611, as follows* 1. The caustic soda, sodium nitrite and. hydrochloric acid weights were adjusted to conform with other lithol red toner economy processes, 2, The extender amount was increased approximately 56* to give a strength decrease of 10%. The blanc fixe content of the color was thereby increased from 28$ to 37*. The Production Division accepted supervision of RL-408-D manufacture in August, 194?. zmmjmmm* There is no patent restriction in the manufacture of RL-408-D. It is not believed that this study has resulted in any patentable development. / DUP050067118 GLOSSARY RL-408-Ds An extension of a calcium lithol toner (Tobias Acid Seta Naphthol) containing 37# blanc fixe* A bar inn lithol toner (Tobias Acid - ol) containing about 8# barium naphthenate, 5# barium rosinata and 5# blanc fixe. RT-425-D (K-2058 type) i A calcium lithol toner (Tobias Acid Beta Naphthol) containing about 16# of calcium roainate BT-4^2-D: A calcium *Duol" toner (Tobias Acid Beta Naphthol) containing about 37# of calcium roiinate. Tobias Acldt Beta naphthylamine-1-sulfonic acid. M^^mXSLMXU d petroleum by product - acid number 225* unsaponiflable matter - 10#. EtWgniBWM. DETAILS! DSI-4S-37. DUP050067119