Document g3w03Lq0gEVXRxXxBXXEYQGL
E. I.'DO PONT DE'NEMOURS k COMPANY Pigments .Department
cc: W. S. Struve
E. F. Klenke/
R. F. White
R. Gedd/
>
-E.^W, Koslosky
-X H. Dunn/
<?R.dB, Morton
' R. M Saleml
A. E* Andrejko (7)
W;-oc Hoffman (7)
F. N. Odell
J . ,C, Chaney
/f, P. Bruce
*-^7 J i, J> Adams
// R. H. Wetzel
// J. W. Minnich
f I Newport Library
Newark
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Newport
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Newport, Delaware April 27, 1973
CP NEWPORT ` -* j EXPERIMENTAL OPERATING PROCEDURE NO.
--!N" --: .
Title: .
BT-H76-D, N-8730-A, Monastral Blue G
Objective:
Demonstration of plant-scale manufacture by preparation of 2,000# of BT-476-D.
.Background:
Sales has requested a Blue G pigment which can be ' dispersed by a Cowles milling, followed by one pass
on a three-roll mill, Ciba-Geigy1s Irgalite Blue LGLD has been promoted for oil-based inks on this basis.
BT-476-D prepared in the laboratory and inr the Newark semiworks has been superior versus LGLD in dispersi bility, transparency, gloss and viscosity in heat-set inks* A previous attempt to manufacture BT-476-D under XOP-424 in December of 1972 failed to produce acceptable material. Contamination with Arquad 16-50 resulted in a product of extremely poor~d'ispersibility. In-process sampling indicated two major sources of contamination: (1) insufficient cleanout of the dispersion mill and (2) use of tote bins which contained substantial amounts of standard BGD mill powder.. Several modifications of-the procedure have been made to reduce the threat of contamina tion by Arquad 16-50 during the execution of this XOP.
Number of Tests: Ten (IQ) Dispersion Millings Two (2) Extractions
Starting Date;
April-rMay 1973
* N35374
XOP No. 428
; -2-
fibril 27, 1973
Procedure:
This operation including cleanout should have special supervisory coverage on a 24-hour basis.- No equipment is to be used without approval from supervision. - BT-476-D should follow a BT-436-P campaign which utilized vinyl pyrmni-^Anobut no Arquad 16-50. The details for equipment cleanout and for the process are attached.
Testing:
Research will evaluate by Cowles milling in Thermex A6E
heat-set vehicle.
;.
Newport Disposition: To be shipped to Newark for drying and pulverization!
Samples:
1 gallon of each mill^ig at completion (10)
'1 gallon of 4-hour milling from.#6 milling (1)
1 gallon vat contents on route to filter
(each extration)
:
1 gallon tote bin. press cake (each extraction) (2)
i
..
.. :
\;
Safety Aspects: No new hazards Involved.
Responsibilities: ,
Scheduling & Batch Cards:
Samples:
Testing:
Closing Report:
5
Production Control Operations Research Research, E, W. Gillow
EWG/mja
DUP050109369
XOP No. 428
APPENDIX "A"
April 27, 1973
CLEANOUT PROCEDURE FOR DISPERSION MILLING ___N-8730-A, BT-476rD
(Use only mills'cleaned as follows)
1. Flush with water until flushes are clear, probably 8-10 hours.
2. Dry mill with low water alum 2 or 3 flushes at 400 lbs, each until dry. About 1-2 hours required for this step.
K- *^Ai*oAs
This cleanout method was suggested by W. G. Hoffman, CPC
Area II Supervisor. He should be consulted if clarification is needed
..
i
The mill or mills used should be selected from those just
completing an Arquad 16-50 free campaign of BT-436-P.
4
'*
*
EWGi1low/mja
DUP050109370
XOP No. 428
. APPENDIX "B"
April 27, 1973
CLEANOUT PROCEDURE FOR MILL DISCHARGE, EXTRACTION, FILTRATION, PACKOUT. . N>8730-A, BT-476-D
TOTE BINS FOR MILL POWDER*-- -
,1, Select 10.tote bins for mill powder discharge.
2, Chop out any encrusted mill powder, particularly in
corners.
_
3. Flush profusely with water until foam is no longer detectable.
PUMPING STATION; VAT 4 7C
1. Fill 47C vat and empty several times. .<
'
2. Pass vat contents through lines to rotary filter.
;
3. Send water flush from clean tote bin through lines to 47C.
ROTARY FILTER
1.. Drain bowls
2. Flush cloths and bowl with water until free of pigment - from previous batches.. A thorough job will take one shift.
TOTE BINS FOR PRESSCARE*
1. Select four (4) tote bins.
2. Turn on side and flush with high pressure hose until no presscake clings to surfaces,
,
* If new tote bins are used, they must be cleaned and inspected in the same manner,
EWGiliow/mja
DUP050109371
OPR.
f - *r'""
,:u
. u- '
BT-H 76-P
mu
Chg #
. DATE TIME OPR.
;
. s1 ,u-`- './ - '
.................................
INSTRUCTIONS
J. "IJEecITnlTI----------- -------- ----------~---- ; q .\ tirade set tightly. W Stop rod in place.
c) Pali empty.
1 QUANTITY STD--.---- * RECOP ' '
,
*'. ' / . ..... m ..
internal mill temperature previous batch
65C or below. If not, cool mill until temperature is 40C j
or below.
j
' .
.' C. .
2. Add .aluminum sulfate.
..
3. Add C.P-LC blue crudedfcot No.
Lot No,
............. "
1100# . 220#
*4. Add
'% L .
fa) perclene (b) h/Azir 20*6
30# j
i.
Vi?' ' ` -"< '
. ` _ .* '
* . /f
' 7: ' ` V-
.. \
* * V '
-.
' ..
. .... _ . 1
6. Install grinding heyd - make sure cooling water i
is on full to mill '.jacket,
.{
_:Remove...stop .rod.,..unlock, brake.,...and. .start,.milling; . Record HoO outlet terrro. after milling for 2 hrs.i
If temp,"'13 above 20^0 notify Supv,
j
Record i-i^O outlet temp, immediately before dumpii hg.
. Tf fcemn is above 20C not ifv Suw ,
1
P' Milling finished (actual milling).
! 5 hrs.
_Stop..miil/.._set. .brake, .insert .stop., rod. Remove 1
grinding head, and install dumping head.
ao. Start dust collector,
j j
ax* Remove stop rod., unlock brake and start dumping
charge by rotating mill for 17 min. If dischargi
weight is under 1350# min. inform s u p v .
12*. Clean scale face and Platform.
113^ Drum charge to clean, dry
Tote Bin
Take 1 at. sample during drum out.
$
j =/3n
.
14. Shut.off dust collector, 15. Position mill, set brake, insert stop rod and
remove dumping head.
j 1
i
' . r*
i
4
...... Record..:. ..... ...........................Sampled, by: ... ,
Total Net Height- ' Stencil.: Code, Lot, Net and Tare 'weights | < on each container - Solids
>. .Net Solids | MAKS OUT PACK&JT CAP!)
Record interns! mill temperature,. (Record this' temo. on next Charge - Item ' ?r.)
Same
1357#
i
' 65C Ma;- :
i 11
(
DUP050109372
H*
Ui EE f TIME
* V.
, VM<MU
I.M
AW
7/ ' BCD EXTRACTION ,,
' i.' / : ..
r L. i
. BT~<rK~Q.
M~%7 '0-/1
7" > 47C r ROTARY FILTERS
t * * ; "
...... <--
.- !.
c
WMVWWAIWM
A-4 t'toUt
. " .
?*:b a t c h h o .
i *1,
w%. --
Select: 5
INSTRUCTIONS'
. r
'loti
tor extraction
store in area east of unloading station.
and Hold
ji-i QUANTITY STD. If EEC O'
j>
** * '
-f:Y .i -> j
!
t.
, .
i .
T
.t
/ r
--
Lot No. Lot No, Lot No, Lot No. Lot No,
;
Lbs. LbS * Lbs. Lbs.
ld>* .^
Ca l Ions I!p0
}!
Calions HpO . Gallons IM>
! i|
Gallons 11,-0- '
!
Gallons H?>0
ti
Record Total pounds ;
Lbs,
ih .VS?,; . ' >
v* %
*
, V* *
*Use water to mill powder chart.,for correct gallons HaO, .
1
-y 2. Check 47C 'tank empty.
'|
MT
a
ft! **-r
J *. *
;*?**>< *.V*
U:
*.'* **
. *i *. * , T
i.r r
*3, Close 47C tank discharge valve - Very important;
.TZKOtOI
that valve.is closed* Acid solution will corro d1 e*mmi. maJgt n* ei t'Hilal rI id Mpil umpMl 1i.1.nterna.lL1 part.isr^j,
4, Add 2.SO' gallons water to 47C tank *
t / !ic. *
J Cals
5. ' Record tine started water addition..
^11.
t.vujwi.mI --m
6. Start agitator. Fume scrubber must
" ....... ....................................
' - ----------------- ----
------------------------
------------ ----------------------- - ~~
ting before agitator will start ._
be
J opera- i!
M
_______ li
H
zsrTki Yj/'F
* **
^wmmmrn****
* . m 'V >*.*
% Heat 47CXT-- ~ /. T/- t-tank to 94-96Cr\f. _ n / -o /i
at 95C.
^
* --. i.-- . m in,
- set control_ ^
_________ ______^
L_.:. i
' ' iwi'i ' ij.
oojin__ c_
... ;i
it `
/ .n /
' *
94.rS6 j
Slurry and pump 5 charges mill powder via tote
i *_
VJ.U uu j
io".oTSf lbs. JL.11/V, k3 V-.OS L j
(f HOP lbs, 100!, CPC).__Check 47C tank .tespcrr.i
acure before each tote bin unloading.
Extracticn/tank :*t5r,!peratu.re...t?.usc..'o.e 35C or
ji-
above before proceeding. If 47C .tank is below '
|}
S5"C. contact supervisox.'
ij 85C <]_
17?. Record time completed core, bin unloading,
DUP050109373
V i
Y ;
.pMX'bsAt-S730'/? 47G * ROTARY FILTERS
INSTRUCTIONS
1 BATCH HO. >. J'JilAIH I I f
. Sfo. /HifCfS ! - 'V-l
* . 92C minimum.
il 92 1
4^-t,
--
Agitate 2 hours at S3C. Set control point at j
88C.
Start
a .ra.
i P .Cl.
. ..End
a.ta. O .til. _i
i
ft ;
-.
*-Ph*
--n
Record A7C temperature at end of 2 hour
agitation. oeried.
'9
Record time at end *ftf 2 hour hold.
1 i
f i i
IS ~ The rotary,vacuum,_ilterlhg^pneraticn. must be li
_____started .and the-orooer operntiht:conditicns__
set before proceeding to next -steo.
Min.
Iiwa> in ,W .! IIIW .1 --1 ^1. .
for, i ! I
r^.1 f
'
~fj~*
47C Jjenperscure msc be mainrair.ed at S6~90qC ; "SurCng pvHpiniTy^xa~set control paint at 88*C
Start pumping; to #.I rc-carv vacuum filter bool. ;
Record t.line at start. of Dumping.
____
JlLf Finish pumping. Slurry pump discharge pressure*. ~~ should read ^ero.
.I
,! i
IS * t
uI
eon tv. ;............ .
.... ........ ..... . , _
j j
- Flush 4 / C tenh.pith...75... cals....cold..pater pith i , Gals.
-- *
acitaticn
and.
pum.p.--.cneracitig..................... ............ . .
*!i
__ luspeat.-s.^c A ?*6t......... ..............' ..................... #
i^eckil^Leitptv. .
. . -1 i
.l11
1
*>R. Record,__tft:e 47C chocked empty.
IV'HMII* .
"1 .. I
.1 0 I
*a>
DU P050109374
FILTRATION 'WASHING -PACK! NG
// -8730-/}
ST- <+76 -b
BATE TIME CPR, ii
srcf>
i*
2,
h~
' __
INSTRUCTIONS
. Start...rotarv vacuurn filter.,and auxi.liary equipment.
-4 The following operating condition must be set
before slurry, from 47G is to be pumped to
rotary vacuum filter howl.
!!
a. Drum speed set^gt
RPM.
Numbers
on dial selector*
b. Vacuum to drum
Inches Kg,
c, Waterflow cover drum
#1 wash line
gpm Valve setting
#2 wash line
Jtpm__V a^l_ve_se tting
#3 wash__l_in.
aive setting
* Wash water temperature 90-95
d. Primary filtrate receiver vacuum
inches
&, Secondary filtrate receiver vacuum
inches Hg,
Air to drum > adiust as needed.
-f -a
QUANTITY STD, PREC:
3> St art filling #1 rotary vacuum filter bowl. Record time bcv?ls starts filling__ ||
' 4 Check, i-lt rotary. vacuum^filter , primary,, and
J
ri -- !' 1fir `
secondary filtrate pumps for effluent color If color is present, stop filtration and invveessttiigr.ate cause and make the necessary correct!
-4-J
L5 second ary.._fi It ra t.e.. ovr-PS--e fflue n t_. hour! 'r -Color*.
i 6. Fill repuloer with water manually.
! 7. i 8,
Set. . water low_to ...renulpar on. automatic contro 1
Record time v2 bowl starts filtering
Mlili , I
..*.
,! .
n.i
.mi -
ptm Win'S*, ,--n
Start irl .rotarv vacuum filter and auxiliary
equipment when level, in bowl covers rake agitator,
L-- The following opera ring ^condition .reuse be set on the secondary rotary vacuum filterT
DUP050109375
FILYRATIGN-WASKING-PACKING N-8730-A eT-i4.76~D
INSERTION'S
b.' Vacuum to drum,,
inches Hp O. ......
, d.
Hp O temoerature .----- ------------iff T-t II
Turn ori NHq 'flow ~tbv2' wash line
QUANTITY 1 STD. iJRECC
--| -SEHii
Water flow to.#3 wash line
gum
jf
Hp O temperature e. Primary filtrate receiver vacuum
1
inches HpO.
: t. Secondary filtrate receiver vacuum
! I1
inches H?0.
S
i: !
Air to drum * adlust as needed.
'
-- --
1 .t
____,f .....-r . \ j
- ............_...............................
4 ti
10. Chock #2 rotary vacuum filtgg.p_rlTgary_a.nd
.secondary filtrate receiver.pumps effluent o:
co 3. or. If color is ore sent, stop .gilt ration,,
_and Investigate cause and make necessary
corrections,
. I, Check #2-Trptarv vacuum, filter primary and secondary filtrate pumps. effluent hourly for
!} ij
color. Record on cheek sheet.:
.-.!{
IX^Pac kou t press cake i n Drums or.. Tote B1ris_.
f Take a 2 oz, oresscake samale every 15 minutes
from conveyer before dumping to shippingcon*
tainers. Make composite sarnole of all 2 oz.
samples taken during packing out lot.
m .h i, i^< iru a w m
imri'i i n nmm
11 ..in in --11 > *>.
!
3. Record Lot No. No. CofcMInH tain ers
Sampled by Net Weights
Opr i
1 A, Identify each container with following
N-Code Lot No, Gross Wt. Tare Wt. Net Wts,
}I" Make "6u"*packovit" curd arid deliver co Aron"
|J--**
DUP050109376