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Патент USA US2101887

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Patented
14, 1937
2,101,887 _
UNITED I STATES
PATENT OFFICE
2,101,887
PRODUCTION OF EFFECTS ON MATERIALS
John Allan and James Arthur Wainwright,
Spomion, near Derby, England, assignors to
Celanese Corporation of America, a corpora
tion oi’ Delaware
No Drawing. Application October 5, 1935, Serial
No. 43,780. In Great Britain October 17, 1934
5 Claims. (C1. 91—88)
This invention relates to the production oi‘ oi’
on exposure to light; compositions containing
i'ects on materials and more particularly to the ?lm-forming substances of this nature give et
production of e?ects on textile materials, ?lms, fects of especial brightness, particularly when the,
i'oils, plastics and the like made of or containing
cellulose acetate or other cellulose ester or ether.
In producing effects on cellulose ester and ether
materials with the aid of pigments, powdered
metals and the like, diiliculty is often experi
enced in obtaining bright e?ects which are fast
Ill to rubbing. Moreover many of the compositions
which have been employed in the production of
5
eifect material is a powdered metal such for ex
ample as powdered bronze or powdered alumin
ium.
When the ?lm-forming substance is a cellulose ‘
derivative it is advantageously the same cellu
lose derivative as is present in the material
treated. Nitrocellulose is less desirable than cel 10
lulose acetate in that nitrocellulose tends to de
these effects tend to gelatinize and/or discolor
velop color‘ on exposure to light whereas cellulose
on storage and have therefore to be employed
acetate does not.
while comparatively freshly prepared.
The proportion of ?lm-forming substance em
ployed will vary with its “viscosity characteris 15
tics” and the method by which the composition
is to be applied. A low viscosity cellulose acetate
may form 4, i0, 20% or more of the total weight
According to the present invention effects are
produced on textile materials, ?lms, foils, plas
tics and the like made of or containing cellulose
esters or ethers by applying thereto a suspension
of a comminuted e?ect material in a solution of
20 a ?lm-forming substance in a medium contain
ing a substantial proportion of a volatile solvent
for the cellulose ester or ether of the material
treated, and a volatile non-‘solvent for said cellu
lose ester or ether. Both the compositions em
25 ployed and their use in the production of effects
on cellulose ester and ether materials form im
portant features of the present invention.
By means 01' the invention it has been found
possible to obtain a large variety of di?erent ef
30 fects, of high quality and good fastness to rub
bing, on cellulose ester and ether materials. The
eil'ect materials which may be employed may be
inorganic or organic in nature, and as examples
of suitable e?ect materials may be mentioned
35 titanium oxide, barium sulphate, zinc oxide, di
acetyl or dibenzoyl benzidine, powdered metals,
?sh scales and insoluble dyestuiIs. The effect
material is employed in comminuted form and
preferably in a very ?ne state of division, ex
40 cept in cases where the eifect to be produced
precludes this, as may be the case when, for
oi.’ the composition.
'
In general a composition
designed‘for application by printing and which _
contains. about 15% of powdered effect material
should contain from 742%, e. g. 8-9% or an
acetone-soluble cellulose acetate 01’ the viscosity
commonly employed in lacquers.
~
The e?ect compositions of the present inven-}
tion, as has been indicated, contain a substan—
tial proportion of volatile solvent for the cellulose
derivative of the material treated. Where the
material contains cellulose acetate, acetone or
methyl ethyl ketone is conveniently employed. _
The proportion of volatile solvent should form
not less than ‘about 25%, and may with advan
tage constitute more than 35%, for example 40
50%, of the total liquid constituents in the ef
fect composition.
In addition to the volatile solvent a volatile
diluent exercising little or no solvent action on
the cellulose derivative in the material treated.
is also incorporated in the composition. Exam
ples of diluents suitable for use in compositions 40
for application to materials containing an ace
instance, fish scales form the effect material. '
tone-soluble cellulose acetate are methyl, ethyl
A considerable variety of ?lm-forming sub
stances may be employed. As examples of such
and butyl alcohols, benzene, toluene, xylene, butyl
45 substances there may be mentioned cellulose ace
tate and other water-insoluble esters and ethers
of cellulose, e. g. cellulose nitrate, cellulose for
acetate or mixture thereof.
If desired, in addition to the volatile solvent, 45
less volatile solvents may also be incorporated
in the composition, particularly such as boil at
mate, cellulose propionate, cellulose butyrate,
temperatures of 100 to 200° C., and especially
ethyl cellulose or benzyl cellulose and chlorinated
50 rubber and resinous substances such for exam
ple as polyvinyl or polyacrylic resins, e. g. a poly
corporated in the e?ect composition ethyl lactate,
diacetone alcohol or dioxane.
vinyl acetate or polymerized styrol. The ?lm
iorming substances employed are preferably such
as yield, on evaporation of their solutions, color
" less,.transparent ?lms which do not develop color
preferably employed in proportions of less than
50% of volatile solvent employed, proportions
of about 20-30%, e. g. 25%, of the volatile sol
vent giving very good results. It is, moreover, 55
130 to 170° C.
For- example, there may be in
Such solvents are
2
2,101,887
usually advantageous to employ in the composi
tion a solvent of even lower volatility than those
or 'the treated ‘materials ‘may be subjected to a
mentioned aboveand in addition thereto, since
The compositions maybe applied to materials
calendering operation. ;
not only is the rate of evaporation of the solvent
mixture thereby retarded, but the settlement of
?nely divided pigments and other eifect ‘mate
rials is also retarded. Incorporation'in the com
positions of plasticizers for the ?lm-formingsub
.
'_
,made of or containin‘g‘cellulo'se esters whether '
those‘ materials arein'the form of ‘filaments, yarn,
straw or like form, but the invention is or particu
lar importance inconnection with the production
of e?ects on such materials in the form of sheets,
?lms, or fabrics; in the treatment of fabrics bet
stances therein isalso frequently advantageous
10 especially where the material to be treated is
_ ter results are obtainable in general on materials 10
a fabric or other product liable to be subjected
‘having a close structure than on materials having '
to ?exing and when it p is desired to apply
the composition to the whole surface of the ma- ,
an open structure.
terlal, or in bold designs. .Where‘?ne designs,
examples are given‘ solely by way of illustration
ence of plasticizer in the composition applied _is
not generally necessary.
Examples of solvents of low volatility and of
and are not in any way 1imitative:—'
plasticizers for cellulose esters or ethers which
A cellulose acetate solution is prepared from
the‘ following ingredients-,
and diethyl phthalates, triacetin, the aromatic
.
tricresyl '
-
Parts by weight
Methylated spirits ____ _'_ ________________ __ 185
Benzyl
dispersed in' 85 parts by weight of a solution con- '
v30 taining 100 parts of acetone-soluble cellulose ace- .
40
'
Ethyl lactate___1____’____‘ __________ ___ ____ __ 150
Xylene_____'___-__; _____ __' __________ __' ____ _; 200
eral preferable that it should be employed in low
proportions. For example, while a composition
containing 15 parts by weight of bronze powder
35
-
Acetone _____________ ___. ________________ ___ 350
vent of very low volatility or a plasticizer is in
25 corporated in the effect composition it is in gen
cohol and will give very excellent results ‘when
printed on a cellulose acetate woven fabric, it is
.
Cellulose acetate ___________ __. ___________ __ 100
phosphate, and ‘dibutyl‘ tartrate. Where a sol-'
tate, 350 parts of acetone, 150 parts of ethyl-lac
tate 200 parts of xylene and 185 parts of meth
ylated spirits maycontain 15 parts of benzyl al
-
Example 1 I
20 may be employed are benzyl alcohol, dimethyl
phosphate,
.
invention but it is to be understood that these
15 e. g. dotted or line designs are desired, the pres;
sulphonamides, triphenyl
_
The following examples serve to illustrate the
alcohol-___“; _____ __v___-___.__‘- _____ _, 15
1,000
30"
A fabric composed of cellulose acetateyarns is
dyed a black ground color and is printed with a
composition made by incorporating a bronze
powder in the cellulose acetate'solution in the
proportion of 15 parts by weight of bronze pow
der to-85 parts by weight of the solution. The 35
generally inadvisable that the proportion of such
a relatively non-volatile solvent, in the composi-_ . fabric is dried after printing and a bright metallic
tion should exceed more than about 25% of the print on ablack ground is obtained.
?lm-forming constitutents of the composition.
,
_ Example 2
Any other desired ingredients, e. g. ?re-retard
ants or compounds adapted to ‘prevent discolora
tion of the effects produced on the materials. may
be incorporated in the e?ect compositions.
The compositions may be prepared by simple
solution or dispersion of the ?lm-‘forming sub
stance in the liquid medium and dispersion there
in of the e?ect material,e. g. by mixing the liq
‘uid-mediumZ ?lm-forming substance, and eifect
material in a mechanical mixer.
Where the
40
A cellulose acetate'solution is prepared from
the following ingredie_nts:—.
.
Parts by weight
Cellulose ' acetate_ ______ _____-______________..,100
Acetone _______ __--_'__, _____ _-_ ___________ __
.Ethyl lactate
__-_-
___-
350
45
150
Xylene ________ __' ____ _>___, ______________ __ 200
spirits____"_ __________ ___ _____ __
185
I‘Benzyl alcohol_____'_____’ _______________ __
Methylated
15
eifect material is unlikely to be damaged by such
a step it is advantageous to knead it with the I,
,
'
.
I
_
1,000
?lm-forming substance prior to addition of the . A fabric composed of cellulose acetate yarns
main body of the liquid medium. The desirabil-_ _ is dyed a medium blue‘ ground shade and is print
ity of employing a composition from which the ed with a composition made by incorporating an
55 ‘?lm-forming substance will deposit as a clear - aluminium powder'in the cellulose acetate solu~
transparent ?lm has already been referred to, and
_tion in the proportion of 15 parts by weight of
it should be noted that the selection of the liquid _ aluminium powder to 85 parts by weight'of the
constituents of the compositions, and the choice
of proportions in which they are to be employed,
are important in this'connection.
v
_‘
The compositions of the invention may be apé
I plied to the materialsby any convenient method
and the materials then subjected to a drying or
steaming or other treatment to ?x the eiTect
65 materials thereon.
For example the composié
tions may be applied locally to the materials by
- printing, or by brushing, smearing or spraying
through stencils. They may also be applied to
the whole surface of the material, for. example
70 by padding, brushing, spraying or all-over print
ing. The material may be subjected to any de
_ sired treatment before or after the application _of
solution. The fabric is dried after printing and
a bright aluminiumprint on ‘a blue ground is ob
tained.
_
-
~
-
1'
on
"
Example 3.
‘
A‘ polymerized vinyl acetate solution'is- prepared "
"from the following ingredients:
.
1.
.
v
_
_
Parts by weight
Polymerizedvinyl acetate ______ ___ ________ __ 500
Xylene____'__; _____________ _.___- _____ __'____ 350
Acetone_v__‘ ____ -7 ____ _v__1 _______________ -_ 150‘
'
'
1,000
A fabric composedof cellulose acetate yarns is
'
70
dyed a brightgreen ground shade and is printed
the eifect composition. For example the mate-v with avcomposition made by‘incorporating ethyl
rial may be dyed or delustred or'otherwise treated . lactate and a bronze powder in the polymerized
prior to the application of the effect composition
vinylacetate solution inthe proportion of 109mg 75
3
2,101,887
by weight of ethyl lactate and 30 parts by weight
of bronze powder to 80 parts by weight of the
solution. The fabric is dried after printing and
a bright print on a bright green ground is ob
tained.
,
What we claim and desired to secure by Letters
Patent is:—
1. Method of producing e?'ects on ?laments,
yarns, fabrics, straws or the like, consisting sub
10 stantially of a water-insoluble organic acid ester
of cellulose or cellulose ether, which comprises
printing thereon a suspension of a comminuted
effect material in a solution of a ?lm forming sub
stance in a medium containing 25 to 50% of a
15 volatile solvent for the cellulose derivative of the
material treated, and a volatile non-solvent
therefor, so as to bond the effect material to said
cellulose derivative, said suspension having no
solvent action on the cellulose derivative.
2. Method of producing effects on ?laments,
20
yarns, fabrics, straws or the like consisting sub
stantially of a water-insoluble organic acid ester
of cellulose or cellulose ether, which comprises
printing thereon a suspension of a comminuted
25 'e?ect‘material in a solution of cellulose acetate
in a medium containing 25 to 50% of 'a volatile
solvent for the cellulose derivative of the material
treated, and a volatile non-solvent therefor, so
as to bond the effect material to the cellulose
printing thereon a suspension of a comminuted
e?'ect material in a solution of polymerized vinyl
acetate in a medium containing 25 to 50% ot a
volatile solvent for the cellulose derivative of the
material treated, and a. volatile non-solvent
therefor, so as to bond the effect material to said
cellulose derivative, said suspension having ,no
solvent action on the cellulose derivative.
4. Method of producing e?ects on ?laments,
yarns, fabrics, straws or the like consisting sub 10
stantially of cellulose acetate, which comprises
printing thereon a suspension of a metal powder
material in a solution of cellulose acetate in a
medium containing 30-40% of a volatile solvent
for the cellulose acetate, a less volatile solvent 15
present in a portion of less than 50% of the vola
tile solvent, and a volatile non-solvent therefor,
so as to bond the e?ect material to the cellulose
acetate of the material treated, said suspension
having no solvent action on the cellulose acetate 20
in the material treated.
5. Method of producing effects on ?laments,
yarns, fabrics, straws or the like consisting sub
stantially of cellulose acetate, which comprises
printing thereon a suspension of a metal powder 25
material in a solution of a polymerized vinyl ace
tate in a medium containing 30-40% of a volatile
solvent for the cellulose acetate, a less volatile
solvent present in a proportion of less than 50%
of the volatile solvent, and a volatile non-solvent 30
sion having no solvent action on the cellulose therefor, so as to bond the effect material to said
cellulose acetate, said suspension having no sol
derivative.
' 3. Method’ of producing effects on ?laments,‘ vent action on‘the cellulose acetate.
yarns, fabrics, straws or the like consisting sub
35
JOHN ALLAN.
35 stantially 01' a water-insoluble organic acid ester
JAMES ARTHUR WAINWRIGHT.
30 derivative of the material treated, said suspen
of cellulose or cellulose ether, which comprises
(CERTIFICATE ' 0F ‘commoner.
Patent, No. 2,101,887. \
December 114., i957.
. JOHll- AILAN, “ET AL‘.
It 'is‘hereby certified that error appears in‘ thatrinted specification
of the above numbered patent requiring correction as follows: l’age 5 , second
_ column, line 16', claimh, for the word "portion" read proportion; and that
the said‘Lett‘ers Patent s‘houldbe read with: this correction therein that
the same may conform to the record of the case in the Patent Office.
,Signedand sealed this 22nd day orrebmm, A. p; 1958.
'
Henry Van' Arsdale,
(Seal)
Acting Commissioner of Patents.
3
2,101,887
by weight of ethyl lactate and 30 parts by weight
of bronze powder to 80 parts by weight of the
solution. The fabric is dried after printing and
a bright print on a bright green ground is ob
tained.
,
What we claim and desired to secure by Letters
Patent is:—
1. Method of producing e?'ects on ?laments,
yarns, fabrics, straws or the like, consisting sub
10 stantially of a water-insoluble organic acid ester
of cellulose or cellulose ether, which comprises
printing thereon a suspension of a comminuted
effect material in a solution of a ?lm forming sub
stance in a medium containing 25 to 50% of a
15 volatile solvent for the cellulose derivative of the
material treated, and a volatile non-solvent
therefor, so as to bond the effect material to said
cellulose derivative, said suspension having no
solvent action on the cellulose derivative.
2. Method of producing effects on ?laments,
20
yarns, fabrics, straws or the like consisting sub
stantially of a water-insoluble organic acid ester
of cellulose or cellulose ether, which comprises
printing thereon a suspension of a comminuted
25 'e?ect‘material in a solution of cellulose acetate
in a medium containing 25 to 50% of 'a volatile
solvent for the cellulose derivative of the material
treated, and a volatile non-solvent therefor, so
as to bond the effect material to the cellulose
printing thereon a suspension of a comminuted
e?'ect material in a solution of polymerized vinyl
acetate in a medium containing 25 to 50% ot a
volatile solvent for the cellulose derivative of the
material treated, and a. volatile non-solvent
therefor, so as to bond the effect material to said
cellulose derivative, said suspension having ,no
solvent action on the cellulose derivative.
4. Method of producing e?ects on ?laments,
yarns, fabrics, straws or the like consisting sub 10
stantially of cellulose acetate, which comprises
printing thereon a suspension of a metal powder
material in a solution of cellulose acetate in a
medium containing 30-40% of a volatile solvent
for the cellulose acetate, a less volatile solvent 15
present in a portion of less than 50% of the vola
tile solvent, and a volatile non-solvent therefor,
so as to bond the e?ect material to the cellulose
acetate of the material treated, said suspension
having no solvent action on the cellulose acetate 20
in the material treated.
5. Method of producing effects on ?laments,
yarns, fabrics, straws or the like consisting sub
stantially of cellulose acetate, which comprises
printing thereon a suspension of a metal powder 25
material in a solution of a polymerized vinyl ace
tate in a medium containing 30-40% of a volatile
solvent for the cellulose acetate, a less volatile
solvent present in a proportion of less than 50%
of the volatile solvent, and a volatile non-solvent 30
sion having no solvent action on the cellulose therefor, so as to bond the effect material to said
cellulose acetate, said suspension having no sol
derivative.
' 3. Method’ of producing effects on ?laments,‘ vent action on‘the cellulose acetate.
yarns, fabrics, straws or the like consisting sub
35
JOHN ALLAN.
35 stantially 01' a water-insoluble organic acid ester
JAMES ARTHUR WAINWRIGHT.
30 derivative of the material treated, said suspen
of cellulose or cellulose ether, which comprises
(CERTIFICATE ' 0F ‘commoner.
Patent, No. 2,101,887. \
December 114., i957.
. JOHll- AILAN, “ET AL‘.
It 'is‘hereby certified that error appears in‘ thatrinted specification
of the above numbered patent requiring correction as follows: l’age 5 , second
_ column, line 16', claimh, for the word "portion" read proportion; and that
the said‘Lett‘ers Patent s‘houldbe read with: this correction therein that
the same may conform to the record of the case in the Patent Office.
,Signedand sealed this 22nd day orrebmm, A. p; 1958.
'
Henry Van' Arsdale,
(Seal)
Acting Commissioner of Patents.
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