Document Dv8zO1yQQRBEnZ0ggOzqm2z8n

....... \ a '3 IK i R ?. KLenke, J r. 4/8/53 - 3/15/54 s E. I. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY Serial No. Copy No. XH-54-S Y RETURN TO JACKSON LAECURATOR' NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report matsmv* g r een as. ~ mm irnmmm mm e,Ami. 1953 - MARCH 15, 1954 FILES DATE; 23342 5/W54 ... DUP050069696 Serial He, KM-SA-S Copy No. V Copy to; #1 - Numerical Pile 2 - Research File (223.42) 3 ~ Library File (22342) 4 " V. H. Ghalup3kij, Newport 5 - J N. Tully/A. Siegel, Newark 6 * W. F. Kayden/0J.C. Klein/#14 Bldg. File 7 - J# H# Cooper, Newark - Mo A. Perkins, Jackson lab., Orohea 9 -* W. J, Clem, Chambers Works, Orehem 10 ~ Eo Fo Klenke, Newport 11 ~ Extra 12 RETURN TO JACKSON LABORATORY! FILE ROOM NEWARK PLANT CHEMICAL DIVISION-COLORS Final Report TITLE? S}MGNASTRAL" GREEN GX - PLANT DEVELOPMENT STUD! PERIOD COVERED; APPJL 8, 1953 - MARCH 15, 1954 CHAR* A-I-C-13 J SUBMITTED BI: E. F. KLENKE, JR. APPROVED BT; J. H. COOPER DATE SUBMITTED: 4/8/54 DATE ISSUED; 5/L2/54 DUP050069697 ~1 - in KN-54-7 there is reported the laboratory and Semi-works development of a process# which eliminates the need for oil ling to produce a CPC Green of improved quality over the existing standards. This report covers only the prt study which resulted in the development of a standard process for Newport manu facture of this new product# now called "Mpnastral Green GX. sn During the period 4/8/53 to 3/15/54 the pigmentary green process, re ferred to hereafter as the nGX process59# vuiderwent several modifications and simplifications. The final process requires very little new capital investment (approximately 150,000) s and should ultimately reduce finished green costs by 10-15 cents per pound. The GX process also contributes to safer operating by eliminating acetone milling and the bastards associated therewith. The GX process produced material of improved quality over the solvent milled green. In general, the GX standards are more intense and yellower in tint, stronger and superior in texture and rate of strength development compared with their solvent milled counterparts. Plant development of the GX process started on 4/8/53, at which time chlorination charge Cl-227 was cade# using standard conditions, except that 268# of anhydrous aluminum chloride was used as the catalyst (i.e. a itl A1C1,* blue crude ratio). Ho difficulties were encountered in the autoclave; however, at the end of the standard rotary dryer cycle the material was still moist, and extra drying and an extended dmping cycle were required to discharge the dryer* This batch was shipped to Newark for u?iq in processing studies. A second GX type chlorination (Cl-359) was made on 5/12/53 to collect more operating data* Unlike Jl-227, tie charge behaved normally in the rotary dryer, except for the characteristic severe fuming of the discharged crude due to the presence of the large amount .of AlClj. Gy the end of April# a number of modifications of the original process had been developed in the laboratory (see appendix I)j therefore a cost study was made to determine which procesr; wca potentially the most desirable (Ssf* l). \ DUP050069698 During the psrlM 6/X--6/XL/53 the first plant trials of the GX process J j (charges G-l, 2 api ware^mds using the so called "granule88 process (B-3 process jj see appendix I);\0.65 parts of ODCB Cortho-dichlorbenssne) per 1.0 part of CPC, Jf added subsequent tbwater slurrjlhg the rotary dryer crude. Due to the sandy, I / pasty nature and rapid settling of the "granules" resulting from this process, I' considerable operating difficulties were encountered (Ref. 2). The "granules" it plugged the lines during pumping, and left sizeable heels agitator. | Charge 3 and combined charges 4 and 5 were processed in the plant during the period 6/L&-6/20/53 using the same process as above, but at different batch sizes. The large batch (4 & 5) was shipped to Newark as N-764, lot 1, which, by rubout versus GT-674-D (SD-121), was rated 105:100, yellow, s* intense. By ink mill test, lot 1 was equal to standard in grit, but markedly inferior in rate * of strength development. Ibis quality deficiency, in addition to the operating ,, difficulties (Ref. 3), made this process unattractive. /' %j >---v A slight modification of the above process, the formation and,iSfiat^tion 0^0.65^granules (0DCB;CPC), and subsequent addition of ODCB to reach ^'0.85 ODCBTCPC ratio before distillation, gave some quality improvement. Thfe laterial, produced on 6/29 as N-764, lot 2 (crude charges G-6 and (3-8 combined), was rated yellow, intense, 100:100 versus GT-674-D (SD-121) by rubout, and was superior to B-764* lot 1 by meet other tests At this time, it was decided to modify some of the existing CPC plant equipment to facilitate further Green CS plant development work; therefore, project PXK-38 ($18,000) was submitted and approved on 7/L/53, to provide these "interim" facilities. Subsequently, during the period 8/18-8/27/53* a 5*000 lb, plant cam paign (see Appendix XI) was made by the modified "25 process", to collect additional quality and operating data. A review of the August campaign data (Ref. 4) confirmed the results of f lot 2* The problem of damage to the rotary dryer by excessive bar movement, due to the formation of pasty lumps during the distillation of the sulfur chloride, was solved during this campaign. The solution involved the use of 3Q0 lbs , of , however,tfiis plugging tendency remained a potential source of trouble. Distillation of 0.85 "granules" ( 0.65 made up to ,0.85 parts ODCB:CPC in the still) posed no significant operating problems. One lot (N-764, lot 7), which was made using a high ODCB:CPC ratio (10 si) for expected texture improvement! required an excessively long distillation time. DUP050069699 ** 3 -- Equal portions of N-764, lots 3, 4# 5 and 6 (0.85 ^granules") were used in the Newark plant manufacture? BGT-751-D, lot 57765, which was quite dose in quality to Semi-works lot 3397 (which it was intended to match). The same deficien cies were noted in rates of strength development and of grit elimination as were observed in lot 3397. 2- ZSsmJ&JSmsML. By the end of September, the laboratory and Semi-works development of the *70" process (Cr3 process, see Appendix I) reached the point Where a plant trial was required. Therefore, on 9/30/53, chlorinations G-22 and 0-23 were finished in the plant as N-764, lot 8, using the "70** process. , Since the "70" process did not involve the granulation" step, the pump- ff ing difficulties associated with the "25" process were automatically eliminated. || The only operating problem of ary significance encountered during the processing f of lot 8 was the excessive distillation cycle, attributable to severe foaming during 1 the steam distillation of 0DCB. By rubout versus the Semi-works reference materiai (Lot 3457-1), lot 8 was rated ws weak, s dull and vs yellow, with a light masstone, iy ink mill evaluation, lot 8 was at least equal to S.W. 3457-1 and GT-674-D (Lot 121) in separation, rate of grit elimination, and rate of strength developmentj at one, three, and five tight passes it was superior to 3457-1 and GT-674-P in strength Mid yellowness. The foaming problem was solved in the Semi-works by utilising a water spray nozzle in the still and installing a demisting screen in the still vapor line to control foaming and entrainment, and using tricrasyl phosphate as an anti foam agent. The success of these measures was proved during the plant processing of G-26 and G-27 as N-764, lot 9 (11/15/53) * The packed lot material was a very smooth free-flowing slurry that did not' exhibit hard settling in the drums (a marked improvement over material made by the "25" process), and the quality was completely satisfactory (see Appendix XI). In December, 1953, a 10,000 lb* plant campaign was made to provide material for standardization and sales promotion, and to collect operating and/or design data to enable preparation of a project for permanent facilities for plant manufacture of Green GK by the improved "70" process. J Considering the fact that the entire campaign was made in ^inteiim?' make shift equipment, no significant operating problems were encountered, and the quality of the finished material was uniformly satisfactory (see Appendix II) versus the temporary Semi-works reference (S.fef* 3457-1). However, the over-all yield (blue to green on a 100$ pigment basis) of 78$, was disturbingly lower than the plant 12 month average of 93 5$ for solvent milled green. Furthermore, laboratory ami Seadworks yields for the Green GX process were consistently comparable to those realized In the standard solvent milling process. It was, therefore, suspected that serious (but elusive) mechanical losses bad been encountered in the plant campaign* DUP050069700 4 In March, 1954, the plant "interim" facilities for CEX manufacture were modified to insure against color losses, and a 10,000 lb. campaign was conducted to check yield and collect cost and capacity data. An over-all yield of 93*8# was achieved. The quality of the finished material was again uniformly aatisfacto From the data collected during these two relatively extensive plant campaigns (Ref. 5 and 6) it was estimated that savings (versus solvent milled green) of roughly 15 cents par pound should be realized, once the permanent plant facilities were installed and additional operating experience gained. Consequently, on 4/12/54 the "Green 70" process (Appendix III) was sxfaaitted (Ref* 7) to the Operating Division for acceptance. EXPERIMENTAL DETAILS The details of the plant development study are covered in the summaries issued at the conclusion of each campaign (References 2, 3, A, 5 and 6), and in the laboratory monthly summaries for the period April, 1953, to %rch, 1954* REFERENCES 1. "Green 25" Process Order of Magnitude Cost Data E. F. Kienke to J H. Cooper, 5A/53 2. "Green 25" -- Summary No. 1 C. K. Cooper to C* Higgins, 6/15/53 3. Summary of Batches G~2B, G-4 and G~5 A, D, Volk to C. J. Higgins, 6/23/53 4* "Green GX" - August Campaign E. F. Klenks to J. H. Cooper, 9/17/53 5. "Green GX" - December Plant Campaign E. F* Kienke to J. H* Cooper, 1/13/54 6. "Green GX" - March Plant Campaign E. F, Kienke.to J. H. Cooper, 3/29/54 7. Letter: "Green C - *70 Process*" S. F. Kienke to V. H. Chalupski, 4/14/54 DUP050069701 s jl $!l* C31* fn u >$ $llfe SlS 9 !!tB ^mSS oi fc$' * t* S >J '^C SlW Vt S'S [f< s> lls- S K -*> <Sn w iSl*vl> <14Lu. s a i 4lu ** jfS i9t iiiL $* k Ii in ^Iv l< I** ti- ti K j[l L* 4 tt ,f 1**% & sc ** _* & K VKJ5 |*'l N Jliig 4 ?s <{*' % i* wC * S.!l* .1*3 H. m *& JSl f "** It ^ >. 1M tit $5 **+ ^ & iti 3! % |S 4> <a X&A <1L >%t 85v Ct ^5N* Jj a tir ijiv s9 H *"* lift 4,,^ SfK $*$ C?MJ ,0rt _ K un-UK tg I $1 It ? *#*8 * i^ 9 v<! * f ***[* tj '%. a s*5 t 1- 1^ t% I*W |* . * r 1 ** V*s 4H :<! o\-%-i$ *5**5 <||&. h ill 1H *^Sf~3St ^ l*S * ir$ M *81? s$5 X *9 >1 X* * DUP050069702 om m um DUP050069703 Average PL 3 ,;V^ 7>" DUP050069704