Document vVXdbyyo21zQopoxdkeRqKqKb
E. !. DU PONT DE NEMOURS & COMPANY KREPS PIGMENTS DEPARTMENT 256 VANDERPOOL STREET NEWARK, NEW JERSEY
Serial No. KN--5l--8
Copy- No.
-1
Numerical File
S NEWARK PLANT PIGMENT COLOR RESEARCH REPORT
Y) Final Report
CONTROL OF DUSTING OF MHX-CAP" PIGMENTS GRANULAR MILORI BLUE B-278-D
Period Covered
1944 - 1950
%
Hi 9797
FILE: DATE-.
213 2/9/51
Serial Ho, KH-51-8 Copy Ho, 1
Copy to* #3. * Hnoerical File
2 * Research Office 3 library file 4 V, Chalupskl - Plant Files
i D. B, Killian - W. F, Spengoman/J.B.Callaway/P.J.Monahan 7 * Extra
HEWARK PLAHT PIGMBHT COLOR RESEARCH REPORT
Final Report COHTROL OF DUSTIHG OF "HY-CAPrt PIGHEHTS
GRABULAR HILORI BLUE B-278-B 1944 - 1950
CHARGE I A-II-C-214 a *x -c ~5
SUBMITTED BY* J. 0. Morrison APPROVED BY* B. H, Perkins
x'
BATE SO
V
BATE ISSUED*
1/12/51. 2/9/51
DUP050068565
1.
wmmmm*
this report covers study directed toward development of economical methods for reducing the dusting of colored pigments, particularly wHy-Cap" iron blues and chrome greens, conducted under Project A-II-C-214, and application of these principles to the development and standardization of B-27S-D.
study of the principles involved in controlling the dusting of these pigments has been completed. An improvement in dusting behavior is effected by micro-pulverizing the lump pigment coarsely, at the same time treating the coarsely ground powder with a high* boiling petroleum-solvent, and subsequently pelletising the treated pigment by mixing it in a standard color blending mixer such as is normally used in the regular bag packing operation.
Development study has included preparation of sizable quantities of the desired reduced dusting super-texture iron blue, ami Chrome greens at four standard shades of the G-550-D line*
Laboratory testing methods have been developed for the evaluation of dusting tendencies and roller mill grinding properties (freedom from separation and tailings). The results obtained with these testing procedures have been corroborated by practical evalua tion of a few of the semi-works products*
Experimental evidence Indicates that the incorporation of the anti-dusting oily agent is an essential step in the proposed procedure. The preferred procedure has been cleared by the legal Department as free from domination by the Cabot "spheronizing" patents.
To date the experimental process has been applied only to iron blue. A product suitable only for ball mill use, comprising treated B-216-D type pigment and coded B-278-D, is regularly manufactured and sold to Xntag. The attached B-278-D<A) making and processing instructions and notes describe the process completely.
The softer texture product required for satisfactory roller mill grinding has not been manufactured* Release of any suchproduet for roller mill application must he governed by adequate large scale pretesting to provide assurance of satisfactory roller mill performahce.
The preferred procedure effecting the Improvement in dusting behavior has been cleared by the Legal Department as free from domination by the Cabot "Spheronizing" patents* It appears that we are free to operate our process*
moil
DUP050068566
_m
380 i
Cost Group - 5 ........ ........ ... -.........-1313D.
Cods* B-278-D W (A)
Goal* 4292# Dlazo Vats Coupling Vat*
Approved by* JOB* 12-5-49 HA* 12-12-49 CWOs 12-15-49
Strike Vat* l8l, 280, 232 JESj 3-2-50
,8.Mi
_____8.3--_____ ___
wmujmaajm________
CTSIBPCIIOIIB MS. COBB 1M.`
! Pump intoseale tank 380
Aik* , & Cites
T
Aik. ZZS ClteS
t
A. Start water Into scale tank 3oT
B. Turn on agitator and steam.
C. D.
AHdeijguhstantod
d7u7m*' p(3in053G.)
at
104-106?.
B. Stir 20 minutes or longer to dissolve*
%
504 589? 5*4
4
lilac* 2, Heigh and hold at vat 383 for step 5
3T~ ' 3. Run 15-20" (+2450.) water into vat 383 3 4. Turn on agitator and steam. 5. Pump in H-340 weighed in step 2. 6. Adjust to 40" (4900.) at 70-75** 7. stir 20 minutes or longer to dissolve.
1700 340 1?00
OT 4
8. Remove steam vent seal in strike vat. 9. Oet inside strike vat and hose top, wall,
agitator etc. thoroughly clean* 10. Bun 20-25" (+26250.) water into strike vat
with agitation* 11. Blow steam lines* 12. Run wash water to sewer with agitation. 13* Oet agitator at 16 RPM.
W Heigh and dump into vat 389* 5 Adjust to 24" (400.). Heat to 120-140? to dissolve.
226 12 226 ' 12 "-'>i
W
35F 7
o:
17. Run Into scale tank 387 from vat 343 MT8
18, Adjust t 24" (400). 19. Stir to uniform solution.
' ...20 Heigh and pour into vat 388
21 Start agitator. 22 Adjust to 30" (860.) by adding water slowly.
243
Stir 3-5 minutes to emulsify*
Heigh and pour in 2-3 minutes
65
Stir 5 minutes.
Check and Record* Solution .-
Tmust ha dark
and clear.
.27. When strike vat runs empty hose top, wall, agitator, etc. from outside of vat and run to sewer. 28 Run 5-15" (+1050G.) water into strike vat*
399 122
M 243
65
DUP050068567
VAT PAGE* 2
CODS* H-278-DCA) Lbs* 4292#
29. Pump into strike vat from Vat 382
d H Pe If
_........*
p h v . p .... _ h
'
30
into strike vat through screen.
3X Install chart in temperature controller.
32 Adjust to 39" (40950.) at 74-76?.
"Tr-- LBS. CODE EBB..
24 38** 24
3Bc T s??T
IQ
33. Adjust scale tank 380 to 77 (30530.) at
104-106?
34. Strike vat 380 at 104-106? into strike vat
at 74-76?. on the surface in 40-45 aIn.
35* Hun in from scale tank in 5-10 minutes.
MT
4
36. If U-594 alkalinity jSri^p*TT^xoeedsro735^
calculate and run into strike vat from Scale
(jlk-0.35)
*x(u39 lbs H-594) f 100 *
acct. ibs, 1-27
37* Stir 5 minutes. 38. Check and Record* ._______ F. 39. Test and Record* Copperas IS
,
.Must be
40. Heat at once to 169-171? in 57-63 minutes. Record* Time started,
41. Check and Record accuracy of controller*
Lear* Thermometer
F Controller
f.
H--ig0h~* T--h--e--r-m--o-m---e--te--r . _.,.B...o? Controller _ or.
42. Stir 30 minutes at l69-171s?. Record* Time started
.
43. Run vat 389 into strike vat in 2-4 minutes.
44. Stir 15 minutes* 45. Run vat 387 into strike vat in 2-4 minutes. 46. Stir 15 minutes. 47* Run vat 388 into strike vat. 48. Stir 2 hours. Record* Time Started
49. Record* pH
Normal 1.5-2.2. If above pH 2.5
Adjust downward only to 2.0-2.5 with H-27.
Do mt make upward adjustment* Record* pH
50. Shut off agitator.
51* Air cool for 8 hours or less to 140-145?. Record* Time started
Record* Time stopped
.
Becord* ............ .
: : ?.
52. 3 hours after start of air cooling, turn on
agitator for 3-5 minutes. 53. 6 hours after start of air cooling, turn on
agitator for 3-5 minutes* 54. Before recording final temperature in step 51,
Stir 3*5 minutes,
55* Check and record*. normal 77(8o85G.).
56* If necessary, flood to 140-145?.
. Records
F.
Record*
,
57. Press with agitation. GRIND WITH **
(440 Cu.Pt.)
0 0
TIME START. n t
*??***.
JIM PIS..
..,...... .
,,0PTH,
........... ......................
27 2349 27
172 440
DUP050068568
Codei B-278-D
42921 or * Grind
Process* (A)QDate*4HA*^iSf12*1!"^
JttKHI0 AREA NOTES JE&t 3-2-SO
PRESSING AREA INSTRUCTIONS
Vat
Bata
Tima
Released by
Press So. 32,33,36,37,38,39)for each
No.of Cakes 60,60 $0 60 60 60)1/3 of batch
Press with
Agitation
Nash to 20 hours or 1800 ohms*
Bake first test after 15 hrs.
Load on 7 cars for each 1/3 of batch.
Special Instructions Non-Bleeding.
Wash with 100-140F water.
Leave top 4 pans empty on each car.
Samples Deliver to
DRYING AREA INSTRUCTIONS
Type L.V. H.V. Hurricane Hours 10 9 ---- 10 + 9 Temp.200 *140 ---- 200 140
Lump container See Chart. Special instructions Non-Bleeding
PRESSING AREA NOTES DRYING AREA NOTES
5
Samples Deliver to
GRINDING AREA INSTRUCTIONS
Grinder No. 3 L.S.p. 5/8* screen Special instructions Non-Bleeding. Follow special directions on back
of card. Samples* 2 envelopes & 1 Qt.Jar 1/2 full.
Deliver to* Control Laboratory Mix before sampling 60 Kin.
No. 1 Conical Blender. Packaging* See chart.
GRINDING AREA NOTES 2nd,Split entirely consumed, per
scheduling table.
DUP050068569
.
See Job Breakdown for Details.
1. Check mill and N-621 pump speed (180 BPil).
Adjust spray t 40-50# oil pressure.
2. Pill N-621 supply tank.
3* Crush lump and load lu hopper. 4. When starting grind, ALWAXBi
A. Turn on 8 lbs. nitrogen
B* Start Grinding
C. Open N-621 Valve,
D. Start N-621 Pump.
I:
Record accurate time Immediately check spray
Starting from gun.
1st
Drum.
7* When stopping grind, ALWATS* A. Stop N-621 Futtp.
B. Close H-621 Voire.
0. Stop Mill, D. Torn Nitrogen valve 1BFT.
.8 Frequently Inspect color for uniform appearance
9* Frequently inspect spray from gun.
.10 Record aeourate time first drum is filled
.11 Continue grinding Into second drum.
.12 Record net weight of first drum.... ......... #.
13* Divide lbs. minutes * .......' # per
If less than 8 or more than 10
min.
multiply by 19.2 and correct N-621
pump speed.
14. Continue grinding batch,per instructions 4,7,
8,9*
.15. Open and dean mill whenever sludge appears
in product*
16 Weigh total batch. Recordi
# Grind.
17.
Subtract*
# lump.
* Lbs. N-621
majiisiaiis,
A. Divide middle batch of 3 batch family( 1 strike), to obtain 2 equal mixes from the 3 twitches*
B. Record following on CARD FOB aSf.BASGB Bill'*
1st.Lot#
. Drumsf ........ Drums from 2nd. '
2nd.'Lot#,, __vDrumsy Divide between 1st and 3*t
3rd. Lot#.. _ .T Drums, +______ Dramsfrom 2nd.
Total Drums.......... 2m.. ....... J. Drums each mix.
C. Tumble each mix 60 minutes, inspect dusting. Continue tumbling if necessary until satis*
factory., D. Submit samples to Lab, B. Hold in blender for disposition. F. When OX, pack in 50 lb. bags*
Handle carefully to avoid breaking granules.
DUP050068570
Newark, Hew Jersey December 15, 1949
B-278-D(A) STAITDA.RD FORMULA HOTES
B"278"D is & green toned Miles*! Blue in dustless, fro* flowing granular form*, Dump pigment is manufactured by the B-271-D
WB'B process* then coarsely pulverised and simultaneously treated, in the pulverizer, with 4i of high "boiling hydrocarbon oil (Mentor 28}*, and finally- converted to the granular form by tumbling in a conical
mix-tank*
tactical evaluations conducted during tbs Chemical Division
process development study (Project 314} demonstrated that, while
B-S78-D as manufactured by the ''A*1 process can be employed in ball**
mill dispersion applications with considerable advantage because of
its freedom from the objectionable dusting which characterises the
use of conventional powdered pigments, its use In roller "mill dig"
pension operations cannot be generally reoommaadsd because of adverse
tendencies toward partteXe-elaasifioation and pigment separation on
the roller-mill, resulting from incomplete wetting of the pigment with
vehicle in the pregrind mixing process. Although the latter diffi
culties are greatly minimised by use of the experimental (B) B-278HD
process (inert atmosphere strike), the
has not been standardized
to date because of cost considerations*
A-fc the insistence of the Xntag Division of Interchemical .
Corporation, which cooperated in practical ball-mill evaluation phases of the development study, ~278~D(A) has recently been .standardized and released* Sale of the pigment is temporarily re stricted to Jjntag*
MAliXFO- s
The making process is identical with B-271-D WBW*
All stepwise making Instructions must be followed ex plicitly. Particularly critical are the weights of H-594 (Step 1} and li-340 (Step 2), and the time and temperature specifications in Steps 40 and 42,
The process responds tiro tori ally to .normal iron blue control variables. It should not be necessary to us any variable other than weight of H-340, with suggested limits of 1800 and 1875 lbs*
In the unexpected event that the process should Hgo1! out of control it would be desirable to institute lump rub outs (9$
lump, 4$ 1-621, versus ,sas is" standard) as a screening test for diversion of unsatisfactory batches to other channels, such as
B-216-D, prior to grinding.
DUP050068571
-2" ALTERNATE PRODUCTION:
When desired, lump cole, fox* conversion to B-27S-D may be selected from existing stock of B-27'X~B on the basis of rubout of a representative sample of the B~271~D, in which 4$ of the standard rubout weight of the lump sample is replaced with N-621*
PRESSING AND WASHING; In conformance with current operating practice the
parent batch is pressed in three sash presses under separate lot mashers. Maintenance of standard texture requires uniform and thorough washing*
DRYING i Assured maintenance of .tine quality, particularly texture,
demands that no portion of the lump pigment be overdried* ' This req^SreieSa^j{*
1* Dryer pans must be uniformly loaded, 2* Deformed pans, which prevent air cir
culation, must not be used* 3* The specified h:.gh-temparature drying
period must neTer he-'e^>'eecS3r\)y the Drying Room*
The specified drying cycle, 10 hoars at 200F fol lowed by 9 hours at X40F* 9 produced uniformly excellent results, during winter months, with B-269-D, a very similar product but with unusually exacting texture requirements* The cycle may require seasonal change to avoid excessive moisture during the summer* All such changes must be dominated by the first paragraph in this section. The writerfs experience has indicated that the high-temperature period should probably never exceed 14 hours.
DUP050068572
QRIHPIHQ \WD MIXING %
A General %
A relatively coarse grind Is essential since the quantity of ST-631 (Mentor 23 oil), required for subsequent elimination of the dust formed during grinding, must be kept at a minimum to avoid excessive dilution of the pigment tinting strength. . Pulverizer Ho, 3, with 5/8" round perforated screen. must be used as specified,
The H-621 is continuously injected into the pulverizer rotor chamber, vhiXo grinding, by means of a spray gun to nhich the oil is metered through a variable-speed gear pump The specified pump speed (192 RPM) provides the desired 4?1 treatment for the color grinding rate experienced to date but must be adjusted to compensate for any change in. grinding rat, as detailed below.
The three 1431 lb, sisner-batches of ground color obtained from a single 4292 lb, trike are combined into two 2146 lb, lots for the final granulation and duat removal operation in conical mixer .Ho, 1, The specified 60 minute tumbling period has been ade quate in the majority of batches to date. In the two unsatisfactory oases, an additional 90 minute tumbling period was arbitrarily employed with fully satisfactory results,
B, Safety;
Ho tendency toward increased inflammability as a result of Mentor treatment was detected in a careful examination of semiworks B-278-0 treated with 7$ of the agent.
At the suggestion of the Safety and Fire Protection Division of the Service Departme5.it, oomjrasaed nitrogen is employed as the Mentor atomising medium, It is recognized that the quantity of nitrogen employed is much less than would be needed to maintain am Inert atmosphere inside the pulverizer,
SAFETY PRECAUTIONS SPECIFIED FOR BLEKDIKG OF IRON BLUE XH SEALED BLEEDERS MUST EE OBSERVED.
''Always Be Careful".
0, Equipment Preparation;
1, Check interior of #3 mill. If necessary, remove sludge or install 6/8" HP Screen.
3, Cheek 1-631 supply. Three batches (4292#) require 25 gallons.
3, Check N-6.23 supply, %ree batches require 2 cylinders (440 on*ft,}.
DUP050068573
-4"
4. With spray gw removed fro mill and diroetod into a huoket,
A* Set JM522 pressure at 8 lbs*
B Clamp gum trigger open, start and
adjust W-621 pump to 192 BPM*, then
adjust gun trigger to provide
Lbs
H-621 line pressure
Gc If spray is not satisfactory, hay gun cleaned by qualified expert.
P 'When spray has been Satisfactorily
adjusted, do not disturb trigger adjustment, but shut off H-621 supply, then shut off H-622 gas supply
5 Install spray gun on supporting rods on side of #3 mill with nosale 3/4 r outside of open mill port
6 Pill N-621 supply can to top
Hopes;
a). The N-621 oil reservoir calibration is 3.86 lbs N-621 per inch
b) The gear pump assembly is quipped with two pumps* The smaller one has been used exclusively to date, The larger one will be needed In the future as noted under (e) below
*::e). At 192 RPM the small puitp will deliver 24 lbs of N-621 per hour, equivalent to 4$ treatment at a grinding rate
of 600 lbs* per hour Actual grinding rates have varied between 500 and 600 lbs* per hour. Experience has indisated that the 192 RBI rat may be safely used between these limits, insofar as quality is concerned. Because
of the low cost of Jf-621 and the minor effects of such variations on total pigment yield, there is no need for
acourate batchwise revision of the standard 4/ treatment quantities as charged out on the individual making cards; periodic adjustment of if-621 (as trail as N-622 Nitrogen) accounts csh be made, based on actual inventory*
d)* Daily spot checks of actual grinding rate (accurate time
for one barrel) are recommended, with appropriate adjust ment of N-621 pump speed if grinding rate is slower than 500 or faster than 600 lbs per hour* The following formula applies for calculating correct speeds for the small pumps
8J# for 4$
192
x
60
y lbs* ground SoiSut,esrrtlL,jusI
S3
19*2 X
lbs. mins*
DUP050068574
-5 **
} It is expected that projected replacement of the lump color feed hopper trill Increase the grinding rat to approximately 1000 lbs* per hour, which was regularly obtained with a similar semi-works mill* Tills will necessitate use of the larger pump and determination of the correct EPM to deliver 4fo 1-821 based on actual grinding rate*
D, Grinding:
lo To obtain satisfactorily mi form grinding rate and uniform H-62X treatment, it is necessary to thoroughly crush each drum of lump color before dumping l/2 of eonients.into feed hopper* Repeat crushing before dumping last 1/2 of contents,
2, ALWAYS observe following sequence when starting to grind?
A, Turn on nitrogen supply and adjust to 8 lbs# pressure,
B, Start mill#
C* When color is discharging, but HOT BEFORE, open N-62X valve and start 1-621 pump,
3, Immediately check to be sure spray is functioning properly,
4, Check constantly to be sure color continues t grind at /normal rate,
5, Whenever mill is stopped for ARY reason, ALWAYS observe following sequence j
A, Shut off K-821 pump and close 1-621 valve,
B* Let mill run 1 to 2 minutes (except in emergency), ther stop mill*
0, Stop nitrogen flow, (TURB GAUGE VALVE TO LEFT.)
S, Check each drum of ground color fcr uniform appearance. If oily sludge is present in. color, the mill must be opened and cleaned,
7. Periodically cheek appearance of spray while grinding. Keep port hole open and cleasj by locking out mill and scraping away accumulated sludge as necessary,
8, Open mill and remove sludge and cake* when necessitated . either by presence of sludge in discharged color or by excessive squealing of drive pulley.
9# Record number of drums ground, see instruction 1 below#
DUP050068575
E* Mixing
Mote % Record following data fop each thpae-batch family oh first batch oapd oni?/c
l* When all throe lots of a three "batch family (single strike) have been ground, record number of drums in each lot# Distribute ALL of 2nd lot between 1st and 3rd to obtain two equal sise mixes# Records
1st lot No#
# drums +
dr-urns from 2nd lot#
2nd lot No#
* .......... drums to be divided between Lots 1 & 3#
3rd lot No#
drums.4-
drums from 2nd lot#
Total drum in 3 lots __-~2
drums for each mix#
2, Tumble each mix 60 minutes in No. X oonioal blender, sample^ and inspect dusting# Continue tumbling until dusting appears satisfactory* Then submit laboratory samples and hold in
blender for disposition*
5. When OK, pack and handle carefully to avoid breaking granules*
PACKAGING s
No evidence of oil-staining of bags was obtained in a 29 month storage test in the semi "works#
No information is aval lable concerning degree of granule breakdown and dust formation resulting from transportation of the
color, either in bags or in rigid containers# Bags should be used exclusively in the absence of speoific requests to the contrary#
TESTING;
Routine control tests are limited to dust inspection and rubout evaluation.
The dust inspection consists of visual examination of a pint sample in a quart glass jar. No more than an extremely slight amount of suspended color should be visible immediately after the jar is moderately shaken.
Suggested rubout shipping limits ares
Masstone; Undertone(Trans.)
Strength: Tint; Tint:
dark - s * light vs,green - vs.red 95 - 105 s.green - a.red vs.intense - vs.dull
DUP050068576
Because of the nature of the product non-represent atlv sampling for th rubout test is occasionally experienced* Wo batch should be rejected until substandard color results are adequately confirmed by now samples*
QUALITY PERFOBIMTGE;
Experience to date indicates that no roblending of granulated pigment should be necessary inasmuch as the color performance of the basic process (B-300-D, B-27X-D) is remarkably consistent*
In the rent that reblending should be required. It amsfc be done in conical mixer #1* Ribbon mixers disintegrate the granules
almost instantaneously*
YIELD PERffPRMMCEi
Experience to date supports the assumption that all of the 1-621 is retained in the product.
CALCULATED COMPOS IT IQH (IB. 951-147)
Anhydrous Cyanoferrate Complex Organic Treating Agents
Moisture
3719 lbs* 318 " 255 !t
lbs,
86*65$
7*40 5*95
CALCULATED GOAL YIELD (MB. 951-1,7)
Anhydrous Lump As Is Lump (S*2j Hs0) Anhydrous Grind As Is Grind (5 * 955* HgO)
3865 lbs* 4120
4037 n 4292 "
PREPARED BYi 3.10* MORRIS01 12-14-49
APPROVED BYj B. ARHOUL
12-14-49
APPROVED BY: B. J HUGEES 12-14-49
RMK
DUP050068577