Document 91Y8V3jdDDZO0xgnEz3od25LV
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TO IWSLL
smmmm KEMOKAKDtM REPOST HO. F-93
J B. Bullitt, Wilmington
R. B. Davis, Marshall *b.
3, D. Pickens, flint
Mp. R. E. Pike, Mr. y. R. Matthew,
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Mr. W. P. Kingsley, Mr. R, j. fniiBer,
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Filet iSlO
Flint 2, Michigan May 25, 1953
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PRELIMIMRT W& fXOH OP CHROMIUM HYDROXIDE
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0" AMD ^DUXiUi"
H:
Chromium Hydroxide (0I-734-D) 1 a pale green trans-
extender pigment currently under development by the
tS Department. It le considerably more transparent than
chromium tetrahydroxld (w-701) but 1 not a color! a
Polymer K (nickel hydroxide). Chromium hydroxide has been ex
amined for possible utility in the formulation Of bright metal
lic..., .
!
In *Dco" metallic. ,it .has been'considered principally as:
I* A replacement for chromium tetrahydroxide (W-701) to upgrade exterior durability.
2. Placement for clear base to upgrade- exterior lity and/or working properties.
In considered fis a durability of it p/i f
chromium for Po
tions,
de is being r K to improve
This report summarises the results and present status of the evaluation and development of chromium hydroaide i both ''Bac" and nDulux". The lots of chromium hydroxide pigment investigated are referred to bydesignations, defined in Table 1, that are descriptive of the reaction used to prepare the pigment
r AHD OOHCLUSIPKS.
ragsg1. "Ducon tinting lacquer formulated from ''chloride"
pinrnreottceeeggsrsitycchu.r.op..m.O..n.iu...me...x..ph_oy..sd..ur..or.e.x..i.d.iI.n.e mp,,praiiaggg,,smsst*etonntewta.o.s....ts.i.un..p.t.i.en. rgiorf"oinrmcu-olalto.erd!-anf-rdomfilm ^ssuulfate" process pigment. However, even the "chloride" tinting
)
checked severely on exposure in masston, being inferior to Polymer K in this respect after one year in Florid (Table it).
2* Formulation of "Due" metallics sing either ''chloride" or "sulfate" process chromium hydroxide pigment offered no durability advantage over controls prepared on existing practices.
A. Formulations prepared using "sulfate" process
chromium hydroxide were inferior to matches based on Polymer K, Argent drey or complementary blending in film integrity And/or polish back at twelve months Florida exposure (Tablb il)
B. Formulations based on chromium hydroxide , (either "sulfate" or "chloride5' process pigment)
were intermediate in gloss retention* polish back or film integrity between matches prepared using a W-701 pigmentation (best) and by extension of a W-785 pig* mentation with clear base to equal hiding (Table 111), Ho significant advantages in blister resistance over W-701 could be demonstrated for either chromium hydroxide pigment In "Puce* lacquers on either one year Florida exposure (Table III) or by accelerated
testsvover a body undercoat (Table v), ,
3. Harking properties of bright metallics wepe not improved by replacing clear base with chromium hydroxide {Table VI),
A. wea, excellent
P(Taackbalegevsixta).bility
of
chromium
hydroxide
in
"buc''
zmw "
1. The only durability background available to date involves "sulfate" process dry pigment ball milled or flushed in a "Dulux" vehicle system. The result# of these exposures shpmed*
A. Ball mill dispersions of the dry pigment were ' superior in blister resistance oh exposure to the
flushed samples prepared by the Pigments department (Table IV), Ho advantage in initial color Was shown by the flushed sample,
B. in mAsstone* at optimum P/B ratio (15/100) s "Sulfate" process pigment ball milled gave durability after, eihht monJB Florida exposure intermediate between Polymer K and chromium tetrahydrOxide, W-701. It shewed blister resistance superior tc w-76land no evidence of checking* It was inferior to Polymer K in gloss retention* (Table IV) '
2* "Dulux" enamels formulated with plant or s ami-works production lots of either "sulfate" or "modified chloride" process pigments showed satisfactory Viscosity stability and freedom from settling after two months shelf storage* However., mill bases
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formulated from the "modified chloride" process pigment bodied severely after.two weeks at 110P and showed surface livering after two months shelf storage* Mill bases of "sulfate" process pigment were satisfactory, > . ACT!OH TAKEN CM PROPOSED;
1. Further valuation of chromium hydroxide in "Due" has been discontinued in view of lack of durability or working property advantages over existing practices. Surveillance of panels now on exposure is the only action proposed in "Due".
2. in "Dulux", preliminary exposures of chromium hydroxide have yielded encouraging, but limited, durability re sults for the ball mill dispersion. further development in "DuXux" will be delayed pending return of extensive exposures of ball mill dispersions of plant and semi-works scale "sulfate" process and semi-works scale "modified chloride" process'pigment. Should these exposures continue6 to show durability advantages for chromium hydroxide over existing metallic formulating practices * the preferred pigment process will be selected, the cost picture , will be developed and plant alignment undertaken in preparation for release of the ball mill dispersion of chromium hydroxide in ^bulux". EXPERIMENTAL DETAILS:
*
Pigment Samples - The samples of chromium hydroxide received from the Pigments7 Department and the process reactions involved are listed in fable 1, "Sulfate" process pigment was preferred by the Pigments Department on the basis of ease of manufacture. The "modifled sulfate" process was a commercially impractical vari ation of the sulfate reaction. The "chloride" process was not considered desirable for large scale production because of the corrosive free chlorine by-product. Evaluation of free chlorine in the chloride process was eliminated in the "modified chloride" process by the introduction of formaldehyde as a reactant. The two samples of "modified chloride" process pigment differed only in that lot 1579 baa heat developed while lot 1578 was cold struck, "Chloride" and "modified chloride" pigment will be more expensive than "sulfate" process pigment according to Pigments Department estimates,
Durability - Significant Florida durability results for exposures of experimental/scale "sulfate", "modified sulfate" and "chloride" process chromium hydroxide pigment in "Due T are presented in Tables XX and 111, Table XI lists results comparing the experimental process samples with other transparent extenders in masstene and a bright metallic. Table 111 Illustrates the effect on Florida durability of the replacement of M-701 or clear base by chromium hydroxide in bright "Duco" metallios. Four months Florida exposure results for plant and semi-works production lots of chromium hydroxide in "Duco" will be available 7A5/53 .
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Durability results in "Dulux" m&aston of plant seal "sulfate'' process chromium hydroxide &r presented oh Table IV. Pour months Florida exposures of semi-works "sulfate" and "modi fied chloride" process chromium hydroxide in "Dulux" will be available 8/15/53 *
Pigsment Dispersion and Initial Properties - In "spuoo" a pulp procl^PX dispersion Was usedV Attempts to utilise adry pigment modified pulp process mere unsuccessful because of excess ive grit and poor color. "Dulux" dispersions mere prepared by ball mill grinding.
in "Due" lacquers. Clarity (on flowout) of experimental scale "chloride" process pigment was superior to all other lots. Experimental "sulfate" process pigment Was cloudy. , The plant and semi-works pigments were equal in clarity, being intermediate in this respect between experimental "chloride" process and experimental "sulfate" process pigBenb. Ho differences were noted between flowout clarity of ehnomiura hydroxid.e. pigment samples evaluated in "' DuluVx"
Accelerated blistering results are tabulated on Table V for plant and semi-works production of chromium hydroxide in unexpoaed "Dulux" and "Duo" masstones, and for panels of "Due" exposure series TX-5W after one months Florida exposure. Accel erated blistering results on these pigments in "Dulux" after one month Florida exposure (series TX-5193) will be available 6/15/53.
The accelerated blistering test consisted of immersing the panels in distilled water at 98"? for a period of one week. The panels were periodically examined to note the,time of initial blistering as well as the severity of blistering at one week* A body undercoat system was used ("Due", *75-1195 primer; 683-1717 surf4eer - "Dulux" t 765-1676 primer-swcfacer)^
The effect on "Duoo" waking properties of the replace ment of dear base by chromium hydroxide in a bright high aluminum content metallic is presented on Table 71. Hiding was measured by cryptemeter. Scaling, mottling and patching where determined by spraying, buffing and patching 12" x*36" panels in the laboratory. The effect of chromium hydroxide on "Dulux" working properties was net determined.
Package Stability - Viscosity stability (two weeks 110*F and also two months shelf storage) and settling results (two months shelf storage) for plant and semi-works lets of chromium hydroxide in "Due" and "Dulux" are presented on Table 711. Viscosities were measured by a Brookfield viscosimeter; average of reading at spindle speeds of 10 and 20 rpm are recorded. Samples were stored in 3/# full closed cans. Degree of settling was determined by applying a tapered spatula perpendicularly to the pigment cake.
FLXMT LABORATORY
ji- F
R. Jv Fulmer
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TABULATION OF CHROMIUM HYDROXIDE SAMPLES RECEIVED FROM THE PIGMENTS DEPARTMENT
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COMPARISON OF FLORIDA DURABILITY OF CHROMIUM HYDROXIDE WISH OTHER EXTENDER PIGMENTS IN "DU
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CHROMXOM HYDROXIDE ACCELERATED9 BLISTER TESTS PLMtT AMP SEMI-WORKS PIGMBW? EAMPTJRR
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TABLE V I
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