Document JkOdOnnmeLVB5omEODjz1QJX

E. |. DU PONT DE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK. NEW JERSEY Serial He. KN-49-8 Copy No. 1 Numerical File NEWARK PLANT PIGMENT COLOR RESEARCH REPORT Final Report \ Titles RT-571-D, LABORATORY DEVELOPMENT 5-nitro-2-amino-anisole "Lithosol" Acid BON, Manganese Period Covered-. Charge: FEBRUARY 1946 to MARCH 1948 A-IIC-180 FILE: 222.2 DATE*. 11-14-49 14 N42192 mm **? #1 *Humerioel Pllo 2 - Research Offlo* S V. CT'ialtifUilpO : Millt * SD*. IB*. ` Serial Ho* EH-49-8 OW 80. / '" S' -:r ,, ? % - ' -;.i. . -S'- , - y. >, 4'-^ _ 4; i , - . v ;, 4 ' ' ' -4 ' # - , v. ymiaa<w GQitOB IU5RQR7 rlaftX Roporo *nti* % S-ni " <f LABORATORY BBVEiBPMEBf " " ` eolo * ttIAthoaoltt Aold BOH, Period Covered* mBBmm 1940 to MARCH 1948 Charge I A-JIG-18Q -S !v ';4' * ! "S 4 -t ' '.= : m vSJ: *% SUBMITTED m A* D. HILLS APPROVED STi 8B8 ims&t 1*27-49 BATE ISSTJEDl 11-14-49 sf DUP050067161 IVBBOlPOTIOVi A study was uadartakaa to rsduoa op lialatU tho roaotirlty la alkyd of ths outonotlira naroon RT*588*B (fl*V02~8VHf*anlsola * Vaphthanll* ASD) foraarly known as RT-Ml-D(A), Ths problam was approaehad froa too anglss. aaaalj (1) a warlabla study oa RTHJ88-D pap so sad (8) aa attsaat to slthar add soas agsat op ollalaato oa* tpaaooas materials which might affaot ths reactivity, ths major portion of tills work Is oovspsd la a popopt oa tbs Roaotirlty of M-6S1-D but tho labopatopy dsrslspnaat of aa additive (Rf6Tl*D) whlSh was affaotIt * la raduoing reactivity Is covered sapapataly herein* It la known that ahaa "Vaphthanlls" spa dissolved la oaustla soda at olevated teaperatures* saaa portion Is hydrolysed to Bata Qay Vaphtholo Aald* Basad oa this fast soas 6*nitro*2*anino*anisole BOV was ppapspad as tha fraa aald. aodlua. and aaaganasa salts* Vhaa thasa *ara addad to Bt*S88HD la lvjC aaouats tha raaotivlty was paduaad sad tha thixotropy ppaotlaally sllalnatsd. aoMiAinr a b b o o v o l p b io v s i "Llthosol* Aald BOV was substituted fop tha Haphthaall" ABB la Rt-588*D (K*3898) sad laked with aaaganasa eulfate* this produot, aodad RT-571-D* vhaa addad la 10 aaouats to BT-588-D pa* duoad tha paaotlrlty of tha lattar considerably* A variable study was aada aa Rt-571D with several impart* sat ravolts as follows* 1* Elimination of tha aodlua bloapbonata ad uss of aa all oaustle eoupliag gaps vary thlok alurrlas aad tha produota vara lafarlor la raduolag tha reactivity of K*8898* 8* Several othar aatala vara uaad for laklag with all products exhibiting aoaa effectiveness la raduolag reactivity aad several equal to RT*I51*D(D), Baaauaa of variations la aolap this Study vas not axtandad st this tiaa* 8* Ths pH of coupling should not bs lovar than gg o p a brownish typo plpaat will rasult* 4* Development la tha aost lapoptaat variable atudlad* A prolongad haatlag oyola will rasult la a conversion of tha plvsaat fpoa a dark* bins, vsak typa to a light* ysllov aad vary strong produot, tala so*oallsd "flopped* aatarlal la absolutely ineffective la raduolag tha reactivity of itMSBHD* 6, tha BOV aaaaot ba addad to tha XABD aad ee-eoupled la say way* All attaapts raaultad la iaaraaaad raaatlvlty* DUP050067162 mm m* M the course f the variable study on Bf-571* all the usual variations were tried and in most eases had no offoot on tended to ho detrimental ottn* BOB*W #F^F W WW-Sril WWilWnwf * W#i* jp laments aaWW gr W*qjS#HWr#Of CV WOO 00.4010' aa other methods of preparation of S-iiltyo-a-ttialno-onlBolo * BOB did not affoot the reactivity* Shea the effectiveness of tho HT*5?1D additlve was first discovered an attempt to oo*oouple tho NASD and BOB vae nado with no beneficial results* from tint to tint various modifications of tho oo-ooupllng technique von# tried hot to no avail# The sodium bicarbonate vaa oliminatad and several variables ran on tho all caustic type coupling hat tho slurries vara quits heavy and tho offoot of too produots on tho reactivity of B7*688*D (K*2292) vaa not oqual to RT*371*D Following a "flopped" batch in tho plant, the problem vaa returned to the laboratory for a complete development study* Title light type material Is a function of both time and temperature of development# It can be obtained at 100c in 15*30 minutes# at 900 in 9 hours end at 70C in over 24 hours* However, if the slurry is seeded with lOg of the "flopped" material the change la greatly accelerated, producing the lip* material in 5 minutes at 100*0*# SO minutes at 90*0 and 5 hours at 70*0# Zt is believed that developing at 70*0 is a safe temperature for plant manufacture* Zt is undesirable from m operating standpoint to finish tho slurry off undeveloped as the pressing cycle (already long) is increased tremendously* Various other metals vare substituted for the manganese with several resulting in effective producta but aomovhat different in color# At the time no further work vaa done. The RT*871*D in preascake form may be added to the BT*S88*D finished slurry with satisfactory results but is more costly from an operating standpoint * DUP050067163 4* vmm 8 n 8 8 8 8 1243 8 n ti 8 n 8 8 8 8 8 8 8 8 8 8 8 8 9 Preparation of 8H< 4 Eval* of #3 * la * BOH* Na,Ma,H+ to R2-5SX-DU) Bval* of #3 :1m 1Q amounts mo: different lot RM2&*B 13 Go-coupling of USD oad 10nB 13 Preparation of large aampls of 17 Ival* of 1197*13 & 18 iAn %"rn `blende* of $-Aa e BOH* Mo by various proctdurea. Seal* of eeml-woifcs preparation 33 Attempt at co-coupling bo m and 34 Preparation of RT-S71-D on .011 eamotio formula* J 1 Variation in p8 of coupling on all caustic formula* 4 Repeat of 1845*1* increased amounts of manganese sulfat and caustic eoda* 14 Variation in BOB excess* id Variation in amount of manganese sulfate* 19 Variation in sodium bicarbonate. 30 Variation in sodium hydroxide 81 Variations in volume and use of Variations in development time* Study effeot am quenching Repetition of 1848-22* Study rate of deusSopmsut* Consistency series* Study temperature of development* -30 Variations in amount of oanstie soda for 31 Repeat of 1246-30 with another atop. 38 Further variations in pH of ooupling* 33 increasing oauatio soda in BOH solution*. Variation' in development time on 1846-33B* 39 Repeat of 1245-38 with quenching* 41 pH of coupling study* 48 Co-coupling Of HASH with 10$$ BOB. 48 Repeat 1845-42 for confirmation. 31 uee of othor metals for precipe 38 Of 1843*42(5 Si* G' a' ................ . of other metal salts (Ba,Sr, Addition of Rf-STl-B pressoake Comparison of adjusted ooupling with 8 Caustie eoda vsrisblo is ooupling* 13 Variation in eauetie soda In adjusting* 17 Bee of erudo 8B0g-8BH2*A*iisole : *49*6 * Reactivity of R7-861-B, KB-49-9-10- plant .end Sami-works BSH-49-10 & 11 - riant .and Semi-Works Of Bf*571-D* ` of R3?-S71*B* DUP050067164