Document 8RJKGqMy2dddO2xRaxvyQNxK
E, I, DU PONT HDE NEMOURS & COMPANY KREBS PIGMENTS DEPARTMENT 256 YANDERPOOl STREET NEWARK, NEW JERSEY
Serial No,
KB-50-40
Copy No, #1, Humericai FIX
NEWARK PLANT PIGMENT COLOR RESEARCH REPORT
Pi'OC'X'csa Repor t FLUID FUliRGY GHIKDISG. (II) D3IHBIH0 rtB02! REDS15' AE:D CHROME
YDLLQDB Hi THE C.n. \IJEKLBR w FLUID PWEROY RliDUUJIOU DILL"
Period Covered
SJ3PTSISBER - NOmiBliR, 1950
FILE: DATE:
MR~X14 *4 Uoy, 28, 1950
NJ 379?
copy tot
01 * Numerical Pile 2 - ioeearbb Office (114*4) 5 - Library Pile (114*4) 4 - V* Chalupski - Plant Filee 6 * D. B* Klllian/A. Siegel 6 * C* B* Bridie * E*S*D* * Wilm* 7 - L*r B* Magruder * Newark
4 - Extra m- *
Serial Ho* KH-60-40 Copy Ho* #1. Numerical Pile
NEWARK p l a n t PIGMENT COLOR RESEARCH RBPORT
PROGRESS REPORT FLUID e n e r g y GRINDING (II) GRINDING "BOH REDS" AND CHROME YELLOWS IN TUB C*B* WHEELER "FLUID ENERGY REDUCTION KILL*
SEPTEMBER * NOVEMBER, 19S0
charge ! A~IC~3, 36
SUBMITTED BY* 8* APPROVED 83ft Q
BATE SUBMITTED* Not* 17, 1460
DATE ISSUED*
Nov, 28, 1950
DUP050068483
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The work covered in this report is a continuation of the tody reviewed In KH-SO-7 which abeuldlba consulted far detail# concerning the operation of the "Fluid shiergy Hill* and a die* oussicn of general Objectives* Briefly* the purpose wae to develop were information on the offeet |f this special type of grinding an tho dl#peral<m proparfciaa of\pig*et#* The prev'te v o t k ooverec awe rwn ir--w an wap\ weau a I, G-S52-D. The present study covered the taro "BOB Reds", m I* (S 8 AO BOE-iin) and RT-535-B (PCAHSA-BOH-Ba) and Hpdlian Cbrowe Ydloir. Y-469-D.
The result# Obtained
generally \eiwllar to thoee
obtained with F*S*8 and G-S52-D*
"Fluid Energy Hilling" gives material which le finer
and more unifora (dry fineness) than our present sdkropulverised products*
A marked iaprovement In Texture uae obtained with the "BOH Bede", B5WMBH9 aBd aWee** Product# nade by
a wlx*in" technique approach enamel fineness and
gloss but would probably not be acceptable far this
application* However, roller will ground products appear substantially equal to ball mill onamela and should be acceptable*
Theae Bed# develop their tinting strength ina paint grind slowly but the rate of strength development Is greats with the fluid energy material. pletely ground the latter la weaker end a little bluer than the mikropulveriaed pigment* Sh the ease of
RT~S53*Dtfce difference le very alight} with RT-825-1) it Is of the order of 10
me various
ile wpr. ewpared frow nlkr..op_u...l.v..e...r..l.s._ed....a..n..d
fluid energy ground red pi its s*howed cn"ly re*latively
flight differences in nassfons, solar* At complete
t*isper#*on, an# issuer are vs/s mssnse# mo
C&X9jpVsNMtCK* jjpMHI9 '99991RI9V :&/BrmwJr PJrwClIliw* IsHEI
conditions * -the ******t-ft free the fluid energy wars lighter then the## **<<* iron the control pulverised) pigmente*
5*. in increase tea* two-fold) in dry bulk le obtained with the red plgssate upon "fluid energy" willing*
An **>p*ayfliiiiWt in df *p*r*^
sties was
obtained with' Chrome Yellow, fluid energy material'
DUP050068484
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were unacceptable because of grit* However a single pass over the roller mill gave texture eng gXose of the same order as that Obtained by the conventional three passes or by ball mill grindings. Strength difference* were very slight) they indicated n advan* tone of ea. %% for the fluid energy sample. The natter of dry balk in the ease of Chrome Yellow is still an open question* (See bodr of report;
Further work, If any* will be guided by Managerial deelslon based on the facts presented above and a study of the economies of fluid energy
See eomnsnfca In previous report* KH-50-7* There have been no new developments*
The grinding work was carried out in a commercial type' of Fluid Energy mill, the "0405* model, rather than the experimental nodal used in the previous work. While saaller In size then the latter* the operating capacity was nueh larger* As Indicated in Table I, the feed rates used were 500-400 pounds per hour* The amount of the samples available precluded any study of variables and ths operating conditions used wars based simply on the anperieaoe and judgment of the Wheeler technical ataff It was their opinion that a factor rate could bo achieved In practical use; this opinion was the basis for their coat estimate of April 6* 1950*
Material for the work was obtained from regular plant pro duction on ths three codes in the form of lump color which was coarsely pulverised (semi-works will without screen) before, shipping to Wheeler* Some minor difficulties (especially with the Yellow) were encountered in feeding the pigment to the Fluid Energy mill at sn even ante; ft is believed that these could be overcome*
Uniting during operation, while not bad, than when ths brown and groan pigacat* were grounds Such of the dust sross from a previous run on hlthol Rod which was scattered throughout ths area* However the greater feed rats soaparsn tS that used with ths experimental mill was probably a contributing factor* In any sins# sufficient contamination was obtained with ths Yellow to make conclusions regarding odor meaningless*
' Yields are indicated in 'Table I* Sums of tho material :: "unaccounted far" was probably left in tho aystomj this should be reduced la commercial operation* Only relatively small percentage*
DUP050068485
*3
passed through to the collecting sleeve (l*e. fines from the cyclone collector). Composites for the evaluation study vex* made of this sleeve material with the mala collection*
Sub-sieve analyser tests (Fisher apparatus) made at tbs Wheeler pleat .ere reported la Table I* ' Various samples were also examined microscopically* Tbs "fluid energy11 material appeared to be more uniform sad to contain fever aggregates thaa tbe mliasNapulverl UePSe'--VrS sonnies-V*
Tests at Rework comprised tbe following t
1. VemisbrDrler - Rubouts* 1 x 50 and 3 x 80 (Tablee IX* mu
% Ousting* Limited to observations during dispersion tests* (Tables IV, V, VI).
8* Moisture content of BOH Reds (Table XII)*
4. Dry bulb (weight of 1 inch cube) (Table X&
5* Dispersion* Preliminary teste characteristics by comparing enamels made from (heavy consistency) mix-la bases with the asms enamels ball willed over night. (Tables IV, V, VI, V7XIXI]) In view of the favorable results obtained with the fluid energy samples* tbe tests wars repeated and extended by grind ing the paste one?* and three passes on tbs thros roll will d comparing the final enamels with 78 hour ball will grinds, (Tables VIII, XX, X)* A comparison mas also wade of one hour and 24 how ball will grinds. (Tables IV, V, VI, VXX)
The results obtained are presented in Tables XI to XII and are discussed below* The *C* (composite) samples are the west significant* However sene tests were also run on the oyoloae end sleeve components of the composite as a matter of interest*
mzmm
The wlkropulveriaed control was slightly dark end vs/s weak against standard 8T-525-D* Compared with this control, energy composito was slightly dark* weak (ea. 110) and
slightly blue* Comparison of 1 x SO and 3 x 50 mulls Indicated the fluid energy sample to bo superior both in respect to rate of strength development and elimination of grit*
Improvement In dispersion Characteristics mas shorn clearly in the other tests* (See especially Tables VIIIII, XX, X> Three jafsoa^owor' the roller millgevs^ substantially as god Persian (grit mad gloss) as a 72 hour ball mlll win'i. pass aaspl* va* only vary slightly Inferior* An omens
DUP050068486
*4
directly from the mixerpaste was ve*y slightly inferior to the one pass product bub definitely better than Hie mlkropulverised control ground three passes*
'The effect of improved texture obtained by fluid energy grinding on color le to giro a lighter (more intense) maastone end more rapid strength development thm the control* At Hie mixer paste stage or after one peer the fluid energy enamels mere strong! additional strength mas developed at three passes and on ban mil* n-wg be^ those letter (ball milled) *00**1# mere masher S^ooi tbs corresponding ones from the control* ' This effect might here been predicted from the rubout tests*
Urn bettor texture of the fluid energy sample was also shown by a wry short (1 hour) bell mill grind* However* it mas not sufficiently dispersed under these conditions to bo rated as satisfactory for enamel use* (The sleeve sample* comprising very fine materiel met someShat better* as would be expected)*
The fluid energy sample mas about twice as bully as tbs control! no difference in dusting mas obvious in the laboratory tests*
Baas
By rubout against standard RT-6S3-D, His control sample was light* weak and vs/s blue* Compared with this control* the fluid energy composite mas vs intense* vs week and vs bins* As in the ease of RT-625-D* it mas superior in rate of strength develop* meat but the difference mss lass marted*
Texture results were generally similar to those obtained with RT*825-r>. The fluid energy simple mas superior (grit and gluts) to the control throughout althou^i His difference after throe passes over the mill was only slight* After 72 hours hall* milling the difference mas very slight but still favorable to the fluid energy sample. Substantially ooaplete dispersion mss obtained after cue- pass over the mill end the enamel mads in this way mas practically equal to the AX and bull mill grinds in grit ratings and in gloss* The control sample showed the expected difference as grinding progressed* Three passes mere required to reach a texture (Hegman gauge ) of *9** Ball milling gave a texture of *10* and a vs'a further improvement in glees.
The color differences between the fluid energy and mlkropulverised samples mere lass then with RT-82S* After one pass* mm the fluid energy sample was mere completely dispersed* it mas slightly lighter In masstone Hum the control. After three psesee or after ballmllliag* the differences were *v*e** mod chiefly in Intensity, Tinting strength of the enamels showed a fairly regular increase as grinding progressed? in both esses* the bell mill pro ducts were etreager than the roller mill preduete* The fluid energy
DUP050068487
sample showed m adivantage la strength at the mixer paste stage end after one pass* After three passes* It was "o.k. vs time* and after bailmilling, "vs weak*, i similar to the rubout results*
Short ball mill grinds gate rather irregular results but were In qfualitative agreement with the above tests.
Building properties mere similar to those obtained with RT-528. Busting characteristics were also similar.
iaas&
Beeause of contamination with red pigment* no firm sen* elusion oould be drawn as to the effect of fluid energy milling m color, there was an Indication of a very slight tea S$0 increase in tinting strength*
A sample of Sherwtn Williams wAtomized" Medium Yellow, 0*53786 was included in some of the Texture tests* This product is dull and weak compared with Y-469-D but Is alleged to be good In texture*
The fluid energy sample was superior to the control In respect to grit and gloss throughout the tests* It -was hot a *mlx In" pigment and was somewhat inferior to the BOH Bods at this stage* However* only one pass over the roller mill was required to give satisfactory freedom from grit md gloss] this was not ha* proved by additional roller mill grinding or ball milling* The control sample required three passe# over the mill*
The amount of sample available precluded any extensive tests cm the Sherwin Williams yellow* it appeared to bo similar in grinding characteristics to the fluid energy samples.
The "control* wee lump color (some batch) from 18 Building mikropulverized in the Semi-Works. It was considerably more bulky than the standard and aetually more bulky then the fluid energy sample which. In turn, was about equal to stsi dard in bulk* The differences may have been the result of packing down during ship ment of the drum from Jfciladelphia* This matter of dry bra; must be considered unsettled In the ease of Chrome Yellow] however* it would seem probable that the effsst of pulverisation may only be slight*
Differencea In dusting were small and probably of doubtful significance.
Sines it was suspsctsd that some of the color differences noted* eapeelally with Aurie Brown (see KH-SO-7), slight have hems due to loss of water from the very fine pigment during grinding, the red pigments investigated In the present study were analysed for water* The results are given In Table XIIj the difference* are small m d probably not significant.
DU P050068488
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Weight Sample feed sate Manifold Temperature Partiole else (Da) (1)
(sioFoni} Control Cyelomo Coll* Sleeve
Distribution (Percent) Initial Main run Sleeve Sloe off (end) ttoacoouated
wtm&: 150# 308#/a*.
140?
1B0# 3S8#/far.
Id0?
#tfct 13#
S65#/hr* ISO0?
1*30 0.68 0,51
0.89 0.67 0.38
0.46 0.43 0.3?
mM 31.4
8.7 16.0 10.6
. SS.4# 46.6 3*3 8.0 18.7
33.1 32.8
8.9 19,0 10.8
(1) Flaher Sub Slav# Analyze***
DUP050068489
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1373-15C s 166 <
161 *
Hold Me. . ___
,.
Std. HT-52S-D (lot mmm
Mlkroptilverlsod Control Lot 16066
(Ssnplas C & I mulled lx and 6 x 66}
Extenalon (l/50>
OSx vs 1 3x Glx VB E lx
Clx V8 0 5X
Six VO 1 SX
1* dark sidark t lot, lass grit
v si light ok grit v si It gritty
soak (os 116) yn*tr vsak
C3x vti D3x
dark sit dark
waak s/s weak
1S75-14C ** Hold saorgy Composite saaplo 146 * Std. B2-653 (Lot 440) 141 * Mlkropulvertsed Control. Lot 18593.
(Semples C & E mulled lx and 3 x 60}
C3x vo E5x Clx va Six Glx VO CSX Blx vs E3x
mx vo mx m$vo *
Maastone
vs int vs int. si loss grit Praot. equal vs light, si gritty-
light light
vo v'kp vo bins vs vkp vo him ws/vs ink si istk/sosk
waak vo/o bins **
DUP050068490
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mmm
*w*o IKH3 60-S
Plaid lne*gy Coapoalte mm Lot 650 (Chipping Standard) Btkropnlverlsaa Control, lot A-1623
C V8 E
c v# a **
Maaatoae
Dark, rod (1)
Bark, rod (1) va daife ire groan
Sit *1 rad 3* si rod
(1) Sample apparently contaminated with RT-655-D
| DUP050068491
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DUP050068494
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Comparison of
mu en&aele
(Color, Hiding end Oloou)
un
13&/%to 13 B/14B 13 C/14C 13 wl4D 13 E/14E
Cyelons Coll* )
Sleave
, ) Fluid Kneefe? Gromd
Composite a /b ;
Sid* Y-S25-D (lot S9633) , im RY-S33-D, lot 440}
Control (mlkropulverised) RT-S2S, lei 18908 Jm
BM33 lot 10303}
W a C*W>
1 how Grinds A 78 B
A 78 C
B 78 C 78 E
78 0
SSrMzg ColorAiding Close
el dk el tr 0*K.
os* equal
O.K.
el It* el op* 0*K.
78 li si op* totter
It op
totter
it 78 op* totter
78 A dk*
tetter
7 die vs tn el tetter
ttK Close
dk tr.
Oft equftl 8 It Op*
0*K*
0*K* 0*K*
78 It 78 op* o*K*
8 It op*
0*K*
Oft 00881
O.K.
8 It At Op* o.x*
78 It Op*
O.K.
WCJQ5
0Q Bow n Onj-ai^
el dk el trsns el <& el trane el dk el trane el dk/dk irons dork, trim**
0*K*
O.K.
0*K* l*worse 1.worse
V el 8
* 0.K* O.K. O.K*
Me
DUP050068495
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DUP050068496
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DUP050068497
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DUP050068498
Bulk Tests (weight of 1 lush oube)
sample 1S73-13C
IS
X3S
Code ET-525-D
e
-
Description ~ F, E* Composite
gbtJL
2.035 8*050
Std* RT-S25HD ($2853) $225 8*800
Control (Bot 18288)
4.325 4.350
810 65
100
1575-14-C 14-D 14-E
RT-533-D 9
*
F. E. Composite Std* RT-533-D (440) Control (Bot 18523)
1*700 8*580 3*500
1.725 2,585 5*500
198 (1) 54 (1)
IPO ft)
1554-60*0 60- 80--E
Y-469-D
F* B# Composite Std. Y-469-D (441) Octroi (hot A-1823)
2.375 9.125 5.575
9 *550 8,17$ 5,750
38 62 100 <1M*>
lots (1) These figures sere ra-ohecked with substantially the ease results*
(2) Bee comments in tody of report*
DUP050068499
** or nuid
BOH Beds
1S73-13C Rj?-52SDt 18986
1898-146 RT-553-D, 18888
tfcnortptlon Fluid Energy Ground MikTopulverlzed Control
Moisture (Toluene Plat.) 4.80# S.68*
Fluid Energy Ground Mikrpulverised Control
1*40* 9.40$g
DUP050068500
