Document b5owvKZ1VNBL6VLpLKwXLNoNo
fl) r*
E. L DU PONT DE NEMOURS & COMPANY
256 VANDERPOOL STREET NEWARK, NEW JERSEY
Serial No. Copy No.
Ot-Sfcrtt
/
NEWARK PLANT PIGMENT COLOR RESEARCH REPORT u
Pinal Report
'Tv *1
(A)sr-3764> (moxAziNE mat t r )i saa-WM3 MunpicnsB
Period Covered *, 1953 to OCXOCBR, 1953
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DP cL '
NJ 44*7
FILE: DATE:
2&8
9/7/54
)
Copy to*
41 Kuaariool Filo 8 * Beeeeroh Fll# (223.8) 3 * Library File (229*8) 4 * J* Tully/A. Siegel, Beuerk 5 - 8* S* Strove. Wilmington o |l4 Bld* File, Neweric 7 J* H* Cooper, SeMark 8 - Extra 9 Sfe&na
3rlftX So* 0NM7
Copy Bo .
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BBKABK FZ4BT OHiUTGAL DIVISICB-COLORS
Final Report
TITLE* (A)BT*376D (DICSAZXBE VIOLET FH)i SEUX-WORKS HASUFACTDHE H3RICD COVERED* MARCH, 1953 to OCTCfflEB, 1953 CHARGE* JW-C-52
DATS SDBMmED* ADSOST 13, 1954 DATS ISSUED* September 7, 19.54
DUP050069946
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1 floooulatlaa rwlittnt font of NDlca9uiiw Wwiatn w boon ndi
In tho laboratory W pi^ipitollnf, itt the presence of "Dicocatine Violet*,
thft *\*md**mm mH a # a ml
RMavitlllft V|M||yiA ft liftfl (KttttldiMd
JpflN(pHJW(^ -jfc *^Jfc3PJp (MBS(jp3L^J <SJA' j^MNN&^W9)^tQIK IbO^ii 'fe^lj .
tho ohl*
fcoition *wii iWw nronoiliimo and to owvldt materiel lor tntitiir p* aimri!^p ^^^p^^^p^p^*^p*^^p
b p p ^p
j ^p ^p -^p * p
^^^p |p ^p ^p ^p pppp^^p b p *bpbp ^p^ppp ^pppesj^^p mOPPOP b^j o IPWBBPP
X ft**! ifjiHi't^ mere stmoeesfolly serried out in tho
2* tho
,, to tho laboratory preparation nod ill mlottivni to fltwoMl it! .
3* lTenlatnnnn to tho
Tirifl Kith tho system in
5. the tho noiti 1*0 tho 00 follaMSI
coded mWfr*
aBtli* lAtMMW*JS|OWJL*Vjll' IV*"!U' 43JmOMXtmO (ipATVprUI i<HUIUHOmDii
flolOt* erode* .f n portion of 'tho ItMwwriw Violet".
DUP050069947
2-
Sulfonation me carried out according to Rart A of the process
(a)8T-376*8, given in S&driMt HI, in two Sesd-works ea^rlaants, lots 3355
and 3357* The first was discarded because of contamination during process-
tog* The sulfonation and subsequent drowning proceeded without any procees
difficulties, except for alow filtration* The paate waa snalyaed V *
Kjeldahl nitrogen detenrfjaXtion, and the results expressed an the aooo-eodiua
agli of "Blax&zine 71oietn* Hw yields fna both batches. aoHuad aa
"Dloxaaina Violst# were* lot 3355* 554*} lot 3357# 52.7556, baaad on lot
302 aa a reference standard* taken at 100*. the extent of making with
HagSCh aolntion specified hr tho laboratory process earns excessive, and oan
probably ba reduced, in view of tha further washing given to the laka after
the precipitation of tha
salt*
Tha process ms carried out on tha fliunl antint products
firat on a laboratory soala, in Ssnt-wwka lot 3435* the quality* as shown in Exhibits I and XI# waa eonsidsred acceptable both bar robout and by floccu lation test* During the proooss obtained by addition of BaOB aolwtion# waa neeeaaary to dissolve the sodium salt of the sulfonate. Held was awry slightly in exoeas of theory*
The large-scale leking was osrried out without difficulty In a tile lined vat# according to the presets in Exhibit 111# fart 8* 8o
difficulties were encountered, bub the pressing and washing tinea ware long* Hold waa approximately theoretical*
Quality of all aanplea me tested by rUbout, and of tbo Silas
by floeadLation teats in aUyd aa wall* In general, tha llias ware"found to ba quite similar* though jwlloaar than the original KS-5lG-b ample by rtdipfc* and eqpal to or better than K8"520-b or 88*279-8 standard in 4HMm lation in allod* Reboot results are tabulated in Exhibit 1 and flowulstion teats in Exhibit II* It nsy be noted that In eonforalty with the expected oenavxor# tn laboratory prepares xiooewis&too reiu*ua im mu better in
GB-2527 than in CE-2454 allyd* Tbo Sawi-worka scale lake was not the equal of the laboratory preparation from tha sane nor Materials, in rssistaaes to flocculation, but ms ws batter than tha original KS-520-b sample* Flooculation test results ware not oomplstely consistent, aa ealdameed by tha feet that K8-520h flooded in one teat (A# Exhibit H) and floaodatad in another (8* Exhibit XX).
X* Dulfcnation of BicsaMdwa Violeti H.B. 1398-132* 2* KS-520-b, preparation of original saaplat 8*8* 1325-170-8
3* 3.W* lota 3274# 3344# 3345, 3355, 3357, 3346# 3367# 3391* 3435* 3463* 4* Valuation laboratory Job umbers 53-414* 53-445* 53-503* 5* of aulfonated KS-71* 1465-36*
DUP050069948
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DUP050069950
f o r mu l a mmr
COLOR COOK (a JBT376-Iat s /23/54 . MAMsDiosaain Violet lake
*6-
.,,. gJ^ct&lAt&on rosigtafe.lgflcg^Z,,._____ _-.-____________ ....-..r^n^:..... --.
bas s o on....... ,,... ,..S'sL ..Xptf0...335yiu .,34.^3a------ .--...,, --,---.--__--
........
bat c h smwiota.-- j bat c h h o . or "if* aumn--_--_--,------------ .,----- ------------ ---
......
"fclr
fmVIVaOiaTtViaflNLI
NsfSwr. ' eM.
c. c.
awinwtenaN
. pas t a.
......
, ..
Premise a ouantity ttf SftlferiWited
Dloxaaine Violet as follows!
Set up a 10 gallon stainless steel drum in a deep nan. Equip drum .with ,
nX.ihtninn agitator. ice and /water*
Fill nan with
Sulfuric Acid 98^5 `
-1 12.! i- Crude for BT-309-P
* 1 ..
Set qp q pump, to penjove vaster fnqjsy;
melted.Ice. '
...................................
!.
Add to drum ... ^
. . . . . . . . . . . . ,._. .. -
Keen drum covered to avoid water
absorption. 1
Agitate acid, and cool to SO*?? or. . . . . . . . . .
lower.. . . . . . . . . . . . . . . . . . . . . . . . ". . . . . . . . . . . . . . . . . . .
... . . . . . . . . . . . . .
Sprinkle ip slowly
..........
so as not toexdeed 59*F.
With. steam pipe t heat water, bath.
rr
Raise tamo/ of slumv to 113*F(A5*Cl
Hold at 111*? tfor 1 hour.
*aivMM
;
A00
i/ater Ice
'$$
a.-. . . . . .
, &
468 Spdium Sulfate anFij d.
To Vat 11, ;?t4. fridge add (20 inches)* Have available
.
Add ice to vatP with agitation, till
excess ice As present. ~
h
Move acid container to 11 Vat platfo *Bl.,--
nnrrcnr sulfonate
IT Vat
'l"V); .
hours t keeping excess ice In Vat* , (Use glass Jar and two l/Zf.'LTygon
tubes as svphons.)
Heat slurry to 160P with steam Hold atl55*-l60*F. for 1/12 hrs.
Ileasure and record volume Add bv sifting
2 IbaV per* inch of volume Stir i/2 hour, qftar adding M-IOA
mg
Filter, in 16 frames, hronse press,.
Wash, with I!108 solution, 21 1hw.tper 5.0 sallons of water.'to
, -`
negative test on Congo Red papert
Dump press;
*
. .. . . . . . . . . . . . . -
.....................
Wold as pwssMlfA, Weigh nrasseake.
---------------- ------------------------
JOOSV GROUP-________SIONATOSK--
DUP050069951
FORMULA SHEET
couowcooa
d are
tMUMat*..,.-t
-------- ------ -------- -----
BASES on.................... ..............PAGE 2
mm
,-... ....................
tc.
. . .. .
- . t, -f
_______.
+9 *'
WnGM)
mjfvr* Mb
LBSn
tfefcer ............ .. ....................
BT-309-P............................ ....5k.
m-n-m
MM
60
Su^fousted Dirotasir e ........
Violet Oroide
6
30
Caustic Sodaf SO# ... A.g .5..
';
34
. c.
WUUWOUttWN
Analyse bv KlelriShl method and calculate to Dioxazina Violet-
PART Bt To 9 Vat (CPC Semiwworks J aM'
7 inches
Add........................................... . Stir to hrek down pasta*
......
Make to
...........
(20 inches )aud hold-
....................... 4
To a30 cation.stainless steel dram
Add
......................................V.
. Frnrn Part, A - Ifalce. to . withwater. ..... Add immediately' to. a p H of 11.5. Should makea
clear solution* . Slake, to.................... ..................... .
; 7- t
yflth water......... .
......................
Record bH of solution in dram:......... .
Add contents of drum to A. Vat,........... .. Stir to mix and take pH of slurry in 9 Vat* Record: oH; .. > -- .
tfater Alum * :,G
''
......... .
12
13
To Add . Stir to dissolve,................................... Strike alum solution into. 9 Vat in 30 minutes.
1?
stir ?n minutes.
.,
Rennrd! Rinal rW
*.
Filter In two press loads, 16 frame each, in bronze press-. -1
- - {
Hash practically sulfate-fyee-
Dump press- Drv in Qordon-Davis dryer at 14Q*F.
Pulvey} m regular speed-,
V -
---
PACKAOC--. GOAL YIELD.
Jug. PER
JCO0T GROUP,, , 52,. BICWATQWB ...Q ,,.J,i-CA.. Rlgfo, DU P050069952
PROCESS NOTES
(A)BT~376-D
(A)BT-376-D is a flocculation-resistant lake of "Dioxazine Violet'*, composed of 90 mol percent of Dioxazine Violet {BT-309-P) on
which is precipitated 10 mol percent of the aluminum salt of a sulfonated Dioxazine Violet* The ''A*1 formula gives the Serai-works method of preparing both the sulfonated component and the lake.
Two sulfonations and one laking have been made in the Semi-
works, as lots 3355, 3357 and 34-63 respectively. la- flocculation resistance, the product (lot 3463) was close to the original laboratory preparation, KS-520b, in tinctorial properties and resistance to flocculation.
The composition and yields given below are calculated, based on components charged, and the Semi-works yield.
COMPOSITION?
CALCULATED YIELD?
Dioxazine Violet Toner A1 salt of sulfonated toner Moisture Total
4
7.0 11.2 l.J 2.4
1TO
62.5 lbs. "as is". 61.0 lbs. anhydrous
References KN~54-'27
/y.Signed; J. Klein
Approved!^J. H, Cooper S/24/54
ic
DUP050069953
DUP050069954