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Патент USA US2132869

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Patented Oct. 11, 1938
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2,132,869
PATENT. ‘OFFICE
UNITED
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21132369.
'CELLULO-SE ACETATE LACQUERS ‘CONTAIN- .
ING‘OXIDIZE‘D CEIJJULOSE ACETATE’
5' Charles‘R. Fordyceva'nd Martti" Salo', ‘Rochester,
. N.‘-Y., assignors to Eastman Kodak Company,
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Rochester, ZN.’ Y.,ga. corporation. of ,lflew Jett
Application December 15, 1936,
Serial No. 115,971
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Claims. ,(01. 134.49)
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bylour preferred method, were dissolved in
' This invention relates to celluloseacetate lac-~ pared
10
parts
by ‘weight of a solvent mixture com
quers, and has as its objectjto provide a cellulose
acetate lacquer which will adhere ?rmly to metal
and other surfaces which it is desired to coat." ,
5;; ' The use of cellulose‘ acetate ' inflacquers ‘has
been greatly restricted by the insuf?cient adhesion
of cellulose acetate lacquer" ?lms to surfaces to
which they are, ap=plied.~ In the case of cellulose ,
posed fcf
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Auetnne
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Percentiby weight
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Ethylene glycol \monomethyl ether acetate__ 20
Toluene__;-;__'__‘_' ______________________ _-__ 15
Methyl acetate"; ______ __- _______ __'_Y____.;_‘ 15
nitrate lacquers, adhesion‘ can be improved by . and the solution was» coated on a strip of cold
Very rolled steel. Stripping .tests were carriedout by
few resins,rhowever, are compatible with cellulose theGardner Laboratory adhesion method, de
acetate, and even those which are compatible do scribed on page 217 of the 6th edition of “Physi
10 the incorporation of resins in the lacquer.
not always confer the property of good. adhesion
on cellulose acetate lacquers in which they are
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incorporated.
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We have discovered that the adhesion of cellu
lose acetate lacquers to metal and other surfaces
can be improved by the incorporationof oxidized
cellulose acetate in the cellulose acetate lacquer.v
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‘cal and Chemical Examination of Paints, Var
nishes, Lacquers and Colors”, by H. A. Gardner.‘
A stripping load of over 600 grams was necessary
to remove the ?lm from the metal,‘ as compared
to a load of only 50 grams necessary to remove
a ?lm of a cellulose acetate lacquer made in the
same way except for the omission of the oxidized
The method by which we prefer toi prepare ' cellulose acetate. The load required for strip
ping the cellulose acetate lacquer containing oxi
oxidized cellulose acetate is as follows: A sus;
pension of 100 parts of cellulose acetate'of 38%
acetyl content in a solution of 10 parts of po
tassium permanganate, 13.5 parts of sulfuric acid,
N). U1 and 1500 parts of distilled water is held at 25° C.
until the permanganate color, hasentirely ‘dis
appeared, which requires approximately three
hours. The suspended, oxidized cellulose acetate
is then treated with water vcontaining sulfur
30 dioxide to remove the manganese dioxide ad
dized cellulose acetate was approximately the
same as that required for stripping a typical,
commercial cellulose nitrate lacquer.
The ratio of the Weight of oxidized cellulose 2-5
acetate to cellulose acetate in 'a lacquer may
range from 1:4 to 3:1. Proportions much less
than 1:4-v do not give satisfactory adhesion, while
proportions much greater than 3:1 do not give
satisfactory ?exibility or stability upon aging. 30
hering to it, and ?nally is washed with distilled ' In most cases, it is desirable to use a cellulose
acetate plasticizer.v in the lacquer. The lower
water and dried.
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The preparation of oxidized‘cellulose acetate alkyl phthalates, such as dimethyl, diethyl and
is described in U. S. Patent 1,976,758 of George dibutyl phthalates are very satisfactory, as are
tripropionin, tributyl phosphate, and dibutyl '
35 B. Watkins and Joseph D. Ryan, which shows
its use as an adhesive layer between cellulose tartrate. The quantity of plasticizer may vary
‘widely, but best results are obtained if the weight
acetate sheeting and glass sheeting in the manu
facture of safety glass. Oxidized celluloseace-r of plasticizer is from 40% to 60% of the com
tate, however, is too water-absorbent vandf the bined weight of ‘cellulose acetate and oxidized 40
cellulose acetate.
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40 ?lms it forms are too brittle to permit of its use
In lacquer compositions to be applied by spray
as the sole ?lm forming; component of a lacquer
which is to form the surface layer of an object. ing, solvent combinations already known for use
We have found that oxidized ‘cellulose acetate 7 with cellulose acetate may be employed. We have
is compatible in all proportions with cellulose ace- - found the following mixtures very satisfactory:
tate, and that lacquers made .from mixtures, in
Per cent
suitable‘ porportions, of cellulose acetate, oxi
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by weight
dized cellulose acetate, and a plasticizer, are very
(A) Acetone ________ -4 ________________ __V_
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satisfactory with respect to adhesion, ?exibility
Ethylene glycol monomethyl ether_-____ 20
Methyl acetate_________________ _;____
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As an illustration of the effect of an’admix'ture
of oxidized cellulose acetate on the adhesion of
vToluene ___________________________ __
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cellulose acetate, we give thefollowing examples:
(B) Acetone ___________________________ __
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Example I .—10 parts by weight of low-viscosity
cellulose .acetate of 40%, acetyl-content and 2
parts by weight of oxidized cellulose acetate pre
. Ethyl lactate ____________ ___ _________ __
20
and water resistance.
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Ethyl ‘acetate ___________________ _'____
Toluene ____' __________________ _'___._‘__
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2,132,869
The concentration of the lacquer solution will
vary somewhat, depending upon the viscosity de
sired, but ordinarily the combined weight of cel
lulose acetate and oxidized cellulose acetate will
Cl be from 6% to 9% of the combined weight of
cellulose acetate, oxidized cellulose acetate, and
solvent mixture. Pigments may be incorporated
if 'desired.
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acetate of high acetyl content were, dissolved im
a mixture of 2500 parts of ethylene chloride and;
500 parts of ethyl alcohol. All parts are expressed
by weight. By means of a suitable coating ma
chine this solution was applied
a thin surface 5
coating to paper. The resulting coated paper
exhibited good appearance and ?rm adhesion of
Example II.—400 parts, of low;viscosity; ace-'1 the applied coating to the paper. .
10 tone-soluble cellulose acetate and 400. partslofz ‘ 'lWhat we claiin as our invention and desire to’
oxidized celluloseiacetate‘ were dissolved in a .be secured by Letters. Patent of the United States 10
mixture of 5000 parts of acetone, 2000 parts. of
1. A cellulose acetate lacquer comprising oxii=
ethylene glycol mcn‘ometh'yl ether, 1500 parts of
cellulose acetate in the proportion of from
methyl acetate and 1500 parts of toluene. 400 dized
15 parts of diethyl phthalate' was then adde'gl as a' 1' to ‘12 parts of‘oxidized cellulose acetate per 4
pliasticizer; All parts are expressed by weight. parts of cellulose acetate, the lacquer having the 15
property of adhering ?rmly to ‘metal and other
Panels of polished steel were coated by spraying surfaces
to which'it is. applied, and of continuing
this solution under standard spraying conditions. to adhere when the lacquered surface is bent.
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When thoroughly dry, the lacquerjcoatings were
90 found to adhere very tenaciously to the metal.
For uses which'require coatingfrom heavy so- '
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2. A ?exible ‘article of manufacture having a
closely adhering coating of a cellulose acetate 20
lacquer comprising oxidized cellulose acetate
lutions, ordinary celluloseeacetate solvents, such the proportion of from 1 to 12 parts oi oxidized
vas acetone, ethylene chloride-methyl ‘alcohol, cellulose acetate per 4 parts of cellulose acetate,
mixtures, methyl acetate, etc., may be employed the, lacquer forming the surface layer of the
25 without diluents, and the concentration in the ?nished article, and maintaining its adhesion to 25
sclution adjusted’ to give the required viscosity. the article when, the article is bent.
' Example, [IL-400 parts of oxidized cellulose
acetateand 600, parts of, low-viscosity cellulose
CHARLES R. FORDYCE.
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MART'I'I SALO.
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