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Patent 1093257 Summary

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Claims and Abstract availability

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(12) Patent: (11) CA 1093257
(21) Application Number: 1093257
(54) English Title: FABRIC DECORATION TRANSFERS AND INKS THEREFOR
(54) French Title: DECALQUES ET ENCRES DECORATIFS POUR TISSUS
Status: Term Expired - Post Grant
Bibliographic Data
(51) International Patent Classification (IPC):
  • D06P 5/15 (2006.01)
(72) Inventors :
  • LEWIS, EDWARD J. (United Kingdom)
  • RATTEE, IAN D. (United Kingdom)
(73) Owners :
  • LEWIS, EDWARD J.
  • RATTEE, IAN D.
(71) Applicants :
  • LEWIS, EDWARD J.
  • RATTEE, IAN D.
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Associate agent:
(45) Issued: 1981-01-13
(22) Filed Date: 1977-03-02
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data: None

Abstracts

English Abstract


ABSTRACT OF THE DISCLOSURE
Decoration materials, e.g. for decorating fabrics,
are made of removable design layer on a flexible sub-
strate. The layer comprises a base of thermoplastic
film-forming polymeric material, a pigment, a cross-linking
agent capable of cross-linking the thermoplastic polymer,
a thermally activated catalyst promoting the cross-linking
reaction, and a high temperature plasticiser. If the layer
is formulated correctly, transfer and fixing of a pre-
printed design on fabric may be effected by passing the
fabric an decoration material between heated calender
rolls.


Claims

Note: Claims are shown in the official language in which they were submitted.


- 24 -
CLAIMS
1. A decoration material consisting essentially of a
flexible substrate having at least one removable dry ink layer
thereon, the at least one layer comprising a base of thermo-
plastic film-forming polymeric material, a pigment, a cross-
linking agent capable of cross-linking the thermoplastic
polymer, a thermally activated catalyst for promoting the
cross-linking reaction selected from the class consisting of
amine and ammonium salts of strong acids and mixtures thereof,
and a high temperature plasticiser, the polymeric material being
chosen and the at least one removable layer being formulated
so that when the layer is transferred to a material to be
decorated and subjected to heat and pressure in the transfer
operation, and any necessary heat fixation treatment, the layer
breaks down to provide a discontinuous non-superficial residual
matrix capable of holding the pigment to the material, which
does not significantly modify the properties of the material
after decoration.
2. The decoration material of claim 1 wherein the remov-
able layer contains at least one pigment capable of reacting
with the polymer.
3. The decoration material of claim 1 wherein the remov-
able layer contains at least one pigment capable of reacting
with the cross-linking agent.
4. The decoration material of claim 1 wherein the
thermoplastic film-forming polymer material is a polyvinylbutyral.
5. The decoration material of claim 1 wherein the
thermoplastics film-forming polymer material comprises a mixture
of a polyvinylacetal and at least one component selected from

- 25 -
the class consisting of acrylic polymers, polyamides,
polyvinyl acetate and polyvinyl alcohol.
6. The decoration material of claim 1 wherein the
cross-linking agent is at least one dialdehyde.
7. The decoration material of claim 1 wherein the
cross-linking agent is a methylolated aminoplast monomer.
8. The decoration material of claim 7 wherein the
cross-linking agent is selected from the class consisting
of dimethylolurea, dimethyloldihydroxy ethylene urea,
dimethylolcyclic ethylene urea, methylolated melamine
and trimethoxy methyl melamine.
9. The decoration material of claim 1 wherein the
catalyst is selected from the class consisting of amine salts
of strong acids.
10. The decoration material of claim 1 wherein the
catalyst is an amine salt of p-toluene sulphonic acid.
11. The decoration material of claim 1 wherein the
high temperature plasticiser is selected from the class
consisting of high molecular weight fatty acids, esters
of high molecular weight fatty acids with polyethylene,
glycol, esters of high molecular weight fatty acids with
glycerol, paraffin wax, stearamide and finely dispersed
polyethylene.
12. The decoration material of claim 1 wherein the
removable layer is present on the flexible substrate as
a number of discrete areas.
13. The decoration material of claim 1 wherein the
removable layer is present as a continuous coating over

- 26 -
the whole of the flexible substrate.
14. The decoration material of claim 1 wherein the
removable layer is made up of a plurality of sublayers.
15. The decoration material of claim 1 wherein the
removable layer is made up of a first sublayer containing
the components listed in claim 1 with the exception of
the pigment, a lithographic image printed thereon in
at least one colour and printed from pigment containing
inks and a second sublayer over the lithographic image
and of composition similar to the first sublayer.
16. The decoration material of claim 1 wherein the
flexible substrate is selected from the class consisting
of cellulose acetate films, nitrocellulose films, aluminium
foils and surface treated papers.
17. The decoration material of claim 1 wherein the
flexible substrate is a silicone release coated paper.

- 27 -
18. The decoration material of claim 1 wherein the
flexible substrate is a wax coated paper.
19. The decoration material of claim 1 wherein the
flexible substrate is a paper coated with a thermoplastic
coating formed of a mixture of unsaturated esters of an acid
selected from the class consisting of acrylic acid and
methacrylic acid, cross-linked by ultraviolet irradiation.
20. The method of decorating a substrate which comprises
applying the decoration material of claim 1 thereto under the
action of heat and pressure, and subjecting the removable
layer of such decoration material on the substrate to heat
treatment to fix the decoration on the substrate, whereby
the at least one layer breaks down to provide a discontin-
uous non-superficial residual matrix holding the pigment to
the substrate, which does not significantly modify the
properties of the substrate after decoration.
21. The method of decorating a substrate according to
claim 20 wherein the substrate is a textile fabric.
22. The method of decorating a substrate according to
claim 20 wherein the flexible substrate is removed from the
substrate prior to the fixing treatment.
23. The method of claim 20 wherein the decoration material
and the substrate to be decorated are brought together between
heated calender rolls under a line pressure of 40 to 200 lbs/
linear inch of roller width.
24. The method of claim 20 wherein the substrate to be
decorated is a textile fabric and the fabric and the decoration
material are passed through heated calender rolls at a speed
of at least 5 m/minute.

- 28 -
25. The method of claim 20 wherein the heat and pressure
are sufficient to activate the catalyst and initiate
the fixation reaction.
26. A printing ink for use in the manufacture of
decoration materials and comprising a liquid carrier medium,
an ink vehicle of a thermoplastic polymeric film-forming
material capable of being cross-linked, a cross-linking agent
capable of cross-linking the polymeric film-forming material,
at least one pigment, a thermally activated catalyst for pro-
moting the cross-linking reaction between the thermoplastic
polymeric film-forming material and the cross-linking agent
selected from the class consisting of amine and ammonium salts
of strong acids and mixtures thereof, and a high temperature
plasticiser, the polymeric material being chosen and the ink
being formulated so that when applied to a flexible substrate
to provide at least one removable dry ink layer thereon and
the at least one layer is transferred to a material to be
decorated and subjected to heat and pressure in the transfer
operation, and any necessary heat fixation treatment, the layer
breaks down to provide a discontinuous non-superficial re-
sidual matrix capable of holding the pigment to the material,
which does not significantly modify the properties of the
material after decoration.
27. The ink of claim 26 wherein the thermoplastic
polymeric film-forming material is polyvinylbutyral.
28. The ink of claim 26 wherein the cross-linking agent
is a dialdehyde.
29. The ink of claim 26 wherein the cross-linking agent
is a methylolated aminoplast monomer.

- 29 -
30. The ink of claim 29 wherein the cross-linking agent
it selected from the class consisting of dimethylolurea,
dimethyloldihydroxyethyleneurea, dimethylolcyclic ethylene
urea, methylolated melamine and trimethoxymethylmelamine.
31. The ink of claim 26 wherein the catalyst is
selected from the class consisting of an amine salts of
strong acids.
32. The ink of claim 26 wherein the catalyst is an
amine salt of p-toluene sulphonic acid.
33. The ink of claim 26 wherein the high temperature
plasticiser is selected from the class consisting of high
molecular weight fatty acids, esters of high molecular
weight fatty acids with polyethylene glycol, esters of
high molecular weight fatty-acids with glycerol, paraffin
waxes, stearamide and finely dispersed polyethylene waxes.

Description

Note: Descriptions are shown in the official language in which they were submitted.


~093Z57
This invention relates to materials for the decoration
of fabrics used as textile materials and ink compositions for
making the same.
Our French Patent Specification No. 2 261 138, laid
open to public inspection on September 12, 1975, describes and
claims a method of decorating textile fabrics which comprises
taking a flexible substrate having a removable layer thereon
containing a dye and/or pigment and a film forming polymeric
base which on heating becomes sufficiently adhesive to adhere
under the effect of pressure to the textile fabric more strongly
than the layer adheres to the fle~ ble substrate, pressing the
layer onto a textile fabric while heating, removing the
flexible substrate to leave the layer adhering to the textile
fabric and subjecting the fabric to a fixation process which
fixes the dye or the pigment to give a fast result and causes a
thermal breakdown of the film so that the presence of its
residues does not affect the textile properties of the fabric
or the fastness of the coloured result.
As indicated in the aforesaid published French patent
2~ specification, within that general process a wide variety of
materials may be used for the layer which is applied to the
textile to be decorated.
According to the present invention there is provided a
decoration material primarily for use in decorating textile
--2--

~0~3257
fabrics which has the advantage of giving an efficient
transfer of the removable layer with very short contact
times and which consists essentially of a flexible substrate
having at least one removable dry ink layer thereon, the
at least one layer comprising a base of thermoplastic film-
forming polymeric material, a pigment, a cross-linking agent
capable of cross-linking the thermoplastic polymer, a thermal-
ly acti~ated catalyst for promoting the cross-linking reaction
selected from the class consisting of amine and ammonium
salts of strong acids and mixtures thereof, and a high temper-
ature plasticiser, the polymer material being chosen and the
at least one removable layer being formulated so that when
the layer is transferred to a matexial to be decorated and
subjected to heat and pressure in the transfer operation, and
any necessary heat fixation treatment, the layer breaks down
to provide a discontinuous non-superficial residual matrix
capable of holding the pigment to the material, which does
not significantly modify the properties of the material after
decoration.
The re vable layer may contain more than one pig-
ment and the pigment(s) may be inert or capable of reacting
with the polymer and/or the cross.linking agent.
Such a material is used by bringing it into contact
under heat and pressure with the material to ~e decorated,
usually a textile fabric, in order to adhere together the
removable pigment-containing layer and the material to be
decorated and thereafter subjecting the material to a fixation
. . ~

1093257
treatment which fixes the pigme~t to the material and nor- -
mally breaks do~m the tra~sferred layer so that the properties
of the material are not significantly ~odified by the presence
of its residues. The use of a thermally acti~ated catalyst
makRs lt possible, using the techDlques described in more
detail below~ to use heat and pressure su$$icient to ~nitiate
the ~xing which can then be all~Yed to go to co3pletion in
time, e.g. a rew days, while the material to be decorated is
- 3a -
~.

10932S7
simply stored. The flexible substrate may be removed prior
to the fixing treatment or afterwards. Generally if it is to
be removed after the fi~ing treatment a higher combination of
temperature and pressure is required in the initial contacting
treatment than if the flexible substrate is removed prior to
the fixing treatment. In certain circumstances it is ad-
vantageous to remove the flexible substrate after the fixing
treatment to minimise the risk of contamination of parts
of the machinery by pigment and removable layer materials.
10 The initial heat and pressure contacting may be of a very
short duration making it possible to achieve transfer and
optionally fixation also by a single passage through heated
nip rollers i.e. an application of heat and pressure of the
order of 10 2 or 10 3 seconds.
Polymers which are preferred as forming the basis
of the removable layer are the polyvinylacetals such as
polyvinylbutyrals and polyvinylformals. They may be used
alone or in mixture with other polymers including acrylic
polymers, polyamides, polyvinylacetate or polyvinyl alcohol.
~uitable cross linking agents which can be used
include dialdehydes e.g. glyoxal, epoxy resin monomers and
aminoplasts. Of particular value are the methylolated
aminoplast monomers e.g. dimethylolurea, dimethylol-
dihydroxy ethylene urea, dimethylolcyclic ethylene urea
or methylolated melamine and their methyl esters such as
trimethoxy methyl melamine.
~s noted above, the catalysts used to promote the cross
linking action are thermally activated. This means that they
-4-

10932S7
are ineffective at normal ambient temperature, and so do not
tend to cross-link the polymer compound of the decoration
material during its manufacture or storage, giving that material
a good shelf-life. The temperature at which the catalyst may
be activated may vary, but is preferably greater than 100C.
Activation may take place by a heating treatment subsequent
to transfer of the removable layer to the material to be
decorated or simultaneously therewith.
The thermally activated catalysts used in the present
invention, so-called "blocked" catalysts, are selected from
amine and ammonium salts of strong acids and mixtures thereof,
e.g. the ethanolamine or diethanolamine salts of mineral acids,
and ammonium salts such as ammonium chloride, nitrate, phos-
phate and sulphate. The activity of the amine or ammonium
salt depends upon the disassociation of the salt. Until a
critical temperature is reached the catalyst has no significant
effect in the removable film. The catalysts suggested in our
patent referred to above are acid or acid generating catalysts
such as zinc nitrate as optional ingredients in order to pro-
mote superior washing fastness. Acid catalysts and acidgenerating catalysts such as zinc nitrate show initiation at
~uite low temperatures, e.g. 50 to 60C or even lower, and
there is no suggestion that by using thermally activated
catalysts as proposed herein the threshold temperature can be
raised with corresponding advantages as discussed below. The
amine salts of p-toluene sulphonic acid (PKa = <2) are of
especial value in this connection enabling the critical
initiating temperature to be raised to as high as 120C with

10932S7
corresponding advantages in the heat stability of the
releasable layer, the flow of the layer during transfer and
the extent of thermal breakdown of the removable film during
transfer and heat fixation. Suitable amine compounds for
combination with p-toluene sulphonic acid include S-carbazide,
mono- and di-ethanolamine.
It is particularly desirable to utilise a catalyst/cross
linking agent combination that gives a precise temperature
threshold for cross linking. Since during the course of
forming the removable layer on the flexible substrate by
coating or printing, for example, it may be necessary to heat
the paper in order to remove solvents; it is important that
no cross linking reactions are initiated by such heating.
During the transfer process, when heat and pressure are
applied, they should initially be sufficient only to ensure
that the materials of the removable layer flow readily without
the development of the viscosity which is characteristic of
the onset of cross linking; however, at the end of the
transfer process, the heat and pressure may rise to activate
2Q the catalyst.
--6--

1(;~93Z57
High temperature plasticisers constitute a special
sub-group of plasticisers and have the property of lowering
the temperature of the rubber/melt transition. They may
or may not also possess the property of normal plasticisers
i.e. lower the temperature of the glass/rubber transition
to give a softer more pliable film. Since the process of
decoration requires that the continuous nature of the
transferred film does not survive the fixation process
normal plasticisers have no significant role to play. How-
ever high temperature plasticisation improves the extentof penetration of the releasable film into the receiving
substrate during transfer and the continuation of that
process during the subsequent fixation treatment. Suitable
materials for use as high temperature plasticisers include
fatty acids such as palmitic or stearic acid, esters of
stearic acid or palmitic acid with polyethylene glycol or
glycerol, paraffin wax, stearamide or finely dispersed poly-
ethylene.
The removable layer may be a continuous layer of one
colour or may be a discrete layer in the form of a
decorative pattern or the like. Such a discrete layer is
conveniently produced by printing and in a further aspect
-7-

1093ZS7
the present in~ention provides printing inks comprising the
ingredients of the layer as set forth above dissolved or
dispersed in an appropriate solvent.
In another aspect, then, the present invention resides
in a printing ink for use in the manufacture of decoration
materials and comprising a liquid carrier medium, an ink
vehicle of a thermoplastic polymer film-forming material
capable of being cross-linked, a cross-linking agent capable
of cross-linking the polymeric film-forming material, at least
one pigment, a thermally activated catalyst for promoting
the cross-linking reaction between the thermoplastic polymer
film-forming material and the cross-linking agent selected
from the class consisting of amine and ammonium salts of
strong acids and mixtures thereof, and a high temperature
plasticiser, the polymeric material being chosen and the ink
being formulated so that when applied to a flexible substrate
to provide at least one removable dry ink layer thereon and
the at least one layer is transferred to a material to be
decorated and subjected to heat and pressure in the transfer
operation, and any necessary heat fixation treatment, the layer
breaks down to provide a discontinuous non-superficial residual
matrix capable of holding the pigment to the material, which
does not significantly modify the properties of the material
after decoration.
Such inks can be formulated according to normal
ink making practice and can be adjusted in their consi-
stency to the particular method of application required.
- 8 -
B

1093257
It is important to avoid excessi~e heat during ink formula-
tion 80 that no initiatio~ of cross linking occ~rs and also
to a~oid the use of acidic materials as additi~es for the
same reason.
The remo~able layer may be a simple single layer or
may be made up of a plurality of sub-layers. The essential
feature of the removable layer is that it should contain,
either throughout or in at least one of its sub-layers or in
the combination of such sub-la~ers, the components previously
described as ~ecessary compone~ts of the removable ; layer.
~he use Or a plurality of sub-layers may in certain cir-
cumstances offer particular a~vantages when it is de-
sirea to use particular printing methods. For example
- 8a -

~0~3;~S7
printing by lithography requires inks to possess particular
properties in relation to their physical reactions with the
lithographic plate. To achieve a satisfactory balance of
such properties is not easy when the inks also require to
possess properties and contain substances such as have been
discussed. However by coating or printing the flexible sub-
strate using any appropriate means with a releasable film
comprising all of the ingredients necessary to the present
invention, drying the coated substrate and then printing the
decoration using a normal lithographic ink, a suitable decor-
ation material can be built up. It may be advantageous with
some lighographic inks to apply over the printed decoration a
further coating similar in composition to the first in order
to achieve the best transfer properties and fastness. It
is particularly advantageous when lithographic inks are
printed to use a thermoplastic base material such as is
provided by ultra violet cured inks based on glycidyl
methacrylate. Similarly in gravure printing good image
production is dependent upon the acceptance of the ink re-
ceiving surface of the ink in the engraved cells and theability of printed dots to flow together to give overall
coverage. To assist in this process with the removable
layer system of the present invention it may be advantageous
previously to coat the flexible support with an overall
removable coating of similar composition.
_g_

10932S7
In the production of the decoration materials by
any conventional mode of printing, the formation of a
plurality of layers is in any case inevitable in multi-
colour printing processes since the coloured decoration
is built up by successive printing with different colours,
mixture shades being produced by laying one printed coat
on another.
It is important in printing by any method and par-
ticularly when a plurality of layers is involved to avoid the
use of drying temperatures which may initiate the cross
linking reaction or cause the high temperature plasticiser
to become operative~ The first will give papers of poor
storage stability as cross linking may proceed for a period
of time after heating ceases and the second will give rise
to a tacky paper which cannot be stacked without adherence
of separate sheets or layers in a roll of printed paper.
The flexible substrate may be chosen from a wide
variety of materials the surface of which is either such that
it inherently possesses the necessary release properties
between it and the removable layer or which surface may
have been treated to give the desired effect. Self-
supporting films of cellulose acetate and nitrocellulose
or aluminium and other metal foils may be used as such or
paper may be used, e.g., coated with a surface having ap-
propriate release properties such as wax, nitrocellulose,
silicone or a rubbery coating e.g. comprising polybutadiene.
Silicone release coated paper, wax coated paper or paper
"~ -10-

~093257
coated with a thermoplastic coating such as are provided
by unsaturated esters of acrylic or methacrylic acid cross-
linked by ultraviolet irradiation in the presence of
appropriate catalysts are the preferred flexible substrates.
Certain paper types are usable as such, i.e. without the
provision of an applied release coating.
When the decoration materials of the present invention
are used, the removable layer should first be transferred to
the fabric to be decorated. This is done using the thermo-
plastic properties of that removable layer, whereafter thelayer is subjected to an appropriate fixing treatment which
serves to cross link the thermoplastic material to form a
discontinuous matrix firmly holding the pigments to the
material to be decorated.
Clearly if the removable layer remained during such
processing as a layer, it would severely affect adversely
the handle and appearance of the fabric after decoration.
It is accordingly essential to use a removable layer
formulation which will break up on heating to give a
discontinuous non-superficial layer and to employ transfer
conditions which enable this process to occur. Accordingly
the preferred transfer conditions are such that the high
temperature plasticiser in the removable layer becomes oper-
ative and the pressure employed promotes adequate flow of
the fluid layer into the fabric to be decorated. The
temperature to which the removable layer is raised during
the transfer process may be such that
~r -11-
r~

-` 10932S'7 - i t
the cross l~nking reactio~ is initiated by activating tne
catalyst, and i~ this is done, th~re is no need ~or any
~ubsequent heat treatment to fix the pigment, ~ixing to
iull fastness taking place automatically over a period
e,g,~o~ lO to 200 hours.
~ We ha~e fou~d that by choosing appropriate pressures
and temperatures for the initial application of the de-
coratio~ materials according to the present i~ve~tion o~to
the fabric to be decorated,sufficient assimilation of the
10 removable layer into the material of the fabric can be
achieved so that little or no adhesion remains between the
fabric and the flexible substrate. I~ these circumstances
it may be advantageous when using certain machine types for the
fixatio~ treatme~t to lea~e the composite unsepPrated
during fixation thus protecting parts of the machine from
co~tamination. Normally satisfactor~ trausfer of the re-
movable layer to the fabric to be decorated is obtai~ed
using a calender with one or both rollers heated, We have
iound temperatures from 80 to 102C and pressures be~leen
20 40 and 200 lbs per linear inch of the roller w~dth to give
Ratis~actory results, The best results are obtained ~hen the
transfer paper reaches a-temperature in the n~p such tha~ ~he
high temperature plasticiser becomes operative, ~Jormally
such plasticisers are selected so that operati~g roller
temperatures lie betwee~ 80C aud 120C. ~lnning speeds
can be slow e.g. 5-10 metres per minute or faster consi-
stent with the fact that co~tact times will be of the
order of 10 2 seconds or less and it is desirable to achie~e
an appropriate traDsfer paper temperature i~ that short
- 12 -

- ` ) 1093257 ~ . ~
time. If higher pressures are used the degree of transfer
into the interstices of the fabric is ~ery high so that the
considerations discussed above apply. The conditio~s
cannot be strictly defined since the properties of the
material to be decorated affect the tra~sfer conditions si~ce
the thickness, density, compressibility etc. of the fabric all
affect the extent of heat film transfer into the fabric
under the hot high pressure conditions.
Although transfer using a very short duration heat/
pressure treatment for example, in a calender, is preferred
it i8 possible to use a static press. Normal~y this will
involve the application Or high pressures e.g. 800 psi
to achieve satisfactory results and although the duration
o* the transfer treatment will be longer than when a
calender is used it will be much shorter than is ~ormally
the case when static presses are used to produce transferred
de¢orations. Normally a static pressure of 5-8 seconds
will be required when the materials of the present inven-
tion are used. ~is may be contrasted with periods Or
60 seconds used in,for example,sublimation transfer
printing c.f.Defago et al ~.S. Pate~t Specification
3782896.
~he rabrics which may be decorated using the materials
-of the prese~t inve~tion may be cellulosic e~g. cotton,viscose
rayon, polynosic ra~Jon, cuprammonium, rayon, polyamide
e.g. Nylon 66 or ~ylon 6, polyester, mixtures of fibres e.g.
polyester/cotton or wool/cotton blends, coated fabrics e.g.
pol~vinylchloride coated cotton fabrics, aluminium coated
fabrics.
B - 13 -

1093257
The following Examples will serYe to illustrate the
invention:
EXAMPLE 1
A paper coated with a silicone release layer is
printed to a dry film thickness of 3 microns with an ink
containing in each 100 gms
2 gms of a copper phthalocyanine pigment
15 gms of polyvinyl butyral ("Butvar 98" - Monsanto Co.)
6 gms of stearylalcohol-ethylene oxide condensate
3 gms of a 20% aqueous solution of dimethylol
dihydroxy cyclic ethylene urea
1 gm of ammonium nitrate
73 gms of 64 O.P. ethanol.
The printed paper is brought into contact with a
mercerised cotton fabric and passed between two rollers set
so as to give a pressure of 100 lbs per linear inch of nip.
The upper roller is made of steel and heated to 110C and
the fabric paper composite is passed through the nip at 6
yards per minute. The composite is then passed over an
oil heated drum at 165C under a felt blanket used to assist
contact. The fabric is in contact with the heated surface
and the contact time is 30 seconds. After the heat treatment
the paper is removed and the fabric is printed with a brilliant
blue design of high fastness to washing and light. Its ap-
pearance and handle are substantially those of the unprinted
fabric.
*Trademark.
"Butvar" is a registered trademark of Monsanto Company
-14-

~0932S7
If the nip pressure is reduced to 10 lbs per linear
inch of nip and the same procedure adopted then the trans-
ferred design is clearly present on the fabric surface.
Similarly if the paper is removed before passage round the
oil heated drum, then the transferred film is observed to
mark the blanket during fixation although the design is no
longer fixed in a superficial way.
EXAMPLE 2
A paper coated with a silicone release layer is printed
to a dry film thickness of 6 microns by screen printing with
an ink containing in each 100 gms,
2 gms of Colour Index Pigment Yellow 1
15 gms of polyvinyl butyral ("Butvar 98" - Monsanto Co.)
8 gms of stearyl alcohol - ethylene oxide condensate
2 gms of a 20% solution in water of trimethylol
melamine
1 gm of ammonium sulphate
40 gms of "Cellosolve"
33 gms of 64 O.P. ethanol.
The printed paper is brought into contact with cotton
interlock fabric and passed between two rollers set so as
to give a pressure of lS0 lbs per linear inch of nip. The
upper (steel) roller is heated to 125C and the fabric/
paper composite is passed through the nip at 5 yards/minute.
The composite is then pressed in a garment press set at a
temperature of 165C for 30 seconds and the paper subsequently
removed.
The fabric is printed to a well penetrated yellow shade
of high fastness to washing and to light. The handle of the
*Registered Trademark for ethylene glycol monoethyl ether.
v~ -15-

~093257
the fabric is excellent and the textile characteristics
unimpaired.
EXAMPLE 3
The paper of Example l was used to print fabrics
made of 67/33 polyester-cotton blends, 50/50 cotton-polyamide
blends and viscose fabrics: similar results were obtained .
EXAMPLE 4
A paper coated with a silicone release layer is given
a second overall coating to a dry layer thickness of 6 microns
using a solution which contains in each lO0 gms,
16 gms polyvinyl butyral ("Butvar 98" - Monsanto Co.)
8 gms stearyl alcohol-ethylene oxide condensate
3 gms of a 20% aqueous solution of dimethylol di-
hydroxy cyclic ethylene urea
l gm ammonium nitrate
72 gms 64 O.P. ethanol.
To the doubly coated paper is applied a design with
for example a brush or felt pad using an ink containing in
each lO0 gms,
5 gms Colour Index Pigment Red 6
10 gms polyvinyl alcohol
85 gms water.
After drying the paper is contacted with a 50/50 cotton/
polyester blended fabric and subsequently treated as in
Example 2.
The design is found to be transferred completely to the
fabric to give a red decoration of excellent fastness to wet
treatments and to light.
-16-

~093257
EXAMPLE 5
An ink is prepared containing in each lQ0 parts,
5 parts of a pigment selected from the list given below
10 parts of stearyl alcohol-ethylene oxide condensate
2 parts of trimethoxy methyl melamine (40~ aqueous
solution)
1.5 parts of ammonium sulphate
1.5 parts of polyvinyl butyral
33.5 parts of 64 OP ethanol
33.0 parts of toluene.
The ink is printed onto silicone release paper or wax
release paper by screen printing and dried.
The design may be transferred to a cotton-polyester
or cotton fabric by contacting the printed side of the paper
with the cloth and heating the composite under pressure
(400 lbs per square inch) at 125C for 0.03 seconds. The
composite may then be heated under light or no pressure for
30 seconds at 165C. The paper may then be removed leaving
the printed design on the fabric providing a decoration
which is fast to washing.
Alternatively the paper may be removed from the
fabric after the first and before the second heat treatment.
Some pigments which may be used in the ink in this
example are listed below,
-17-

10932S7
Copper phthalocyanine (blue shade)
Carbon black (grey shade)
Cl OH CONH
N = N ~
~ ~ (red shade)
Cl ~ ~)
CH3
C - OH
NH.CO.C N = N ~ Cl
(yellow shade)
- OH Cl
IH3
-18-

109~2S7
(violet shade)
-19-

` 10932S7
E~AM~,E 6
2 gm8 of a finely divided carbo~ blac~ pigme~t
15 gms of polyvinyl but~ral (n~utvar 98" - Monsanto Co.)
10 gms of stearyl alcohol - eth~le~e oxide conde~sate
2 gms Or trimethox~ meth~lmelami~e
1 gm of the monoethanolamine sal~ of p-toluene
sulphonic acid
2 gms of Bentonite
are dispersed in a mixture of 50 parts of pol~eth~le~e glycol
10 200 with 18 parts of diaceto~e alcohol to form a screeu
pri~ti~g ink. A silico~e coated paper aS used i~ Example 1
is printed with the ink by screen printi~g and dried at
s 75C. ~he pri~ted paper i8 then used to decorate a
cotton fabric by passing the paper i~ contact with the
fabric throug~ heated ~alender rollers operating at a pres-
sure o~ 70 lbs per li~ear inch of ~ip with one roller
heated to a temperature of 95C. ~he speed of passage is
20 metres p~r mi~ute. ~he paper is then peeled from the
; cotto~ fabric leaYing the pri~ted.desig~ thereo~. ~he
20 fabric i5 the~ heated f-or 30 seco~ds i~ an ove~ at 140C.
After the heat treatme~t the fabric is d~orat~ with a
fast black desig~. The fast~ess is found to improve on
- 20 -
B

109 325 7
standiDg to an eve~ higher sta~dard givi~g excellent
fastness to the I.SØ No. 4 washiDg test.
E~A~PIE 7
If in ~xample 6, the carbo~ black pigment i8 replaced
by a red pigme~t (a.I. Pigment Red 6) and the design i~
printed by screen printi~g onto a wax coated paper. An
excellent trans~er o~ the design onto a rayo~ ~abric is
~chieved by increasing the calender pressure to 115 lbs
per li~ear inch and the temperature of the heated roller
to 110C. ~he fastne~s of the decoration a~ter heat
treatment as described in ~xample 6 i8 excellent.
E3AnPIE 8
~ n ink made up as sh~ in Eæample 6 is applied by
screen prin~ing to a wax coated paper which is then used
to decorate a cotto~ ~abric by passing the paper in contact
~ith the fabric between heated calender rollers at a pressure
o~ 100 lbs per l~near inch of n~p with o~e roller heated to
a tempe~ature of 190C and with a ru~ni~g speed o~ 1 yard
per minute. The paper is then peeled from the fabric. After
storage for 7 days the fastness of the decoration is greatly
improved over ~hat whlch may be observed lmmediately af~er
the paper is peeled a~d is eq~al to that observed of the
pattern i5 produced by the transfer and fixation conditions
employed in Example 5.
- 21 -
. ~

f .) . ~-
10932S~
E~PTE 9
A coating solution of 15 parts of polyviDylbutyral
dissolved in 85 parts o~ n-propanol is applied to a paper
- coated with an ultra~iolet radiation cured butylmethacrylate
composition containing a suitable photochemical initiator
and dried. The polyvin~lbutyral coating is applied at a
wet thickness of 6 ~.
$he coated paper is printed with a conventional
lithographic ink containing a copper phthalocyamine pigment
using normal procedures and then coated again with a solution
containing
- 15 parts of pol~in~l butyral
10 partæ of stearyl alcohol
2 parts of trimethoxy uethyl melamine
1 part of the diethanol2mine salt of p. tolue~e sulphonic acid
dissol~ed 72 parts of n-propanol and dried at 50C. The
wet thicknesg of the second coating is 6~.
~ he printed paper i8 then used to decorate a
cotton/polyester blended ~hirting fabrio by bringing it
into contact with the fabric and passing the composit~
through a heated calender set at a pressure Or 70 lbs per
linear inch and the temperature of the heated roller at
~00C. After passage through the calender the paper is
remo~ed leaviDg the decorating deæign on the fabric. ~he
latter is then heated for 45 seconds at 135C to gi~e a
blue decoration of ~ery high fastness to seYere washing
a~d to light.
. , . ~
~ -- 22 --

109325'7
EXAMPLE 10
8 parts of a copper phthalocyanine pigment
15 parts of polyvinyl butyral
12 parts of stearyl alcohol - ethylene oxide condensate
2 parts of trimethylolmelamine
2 parts of ammonium nitrate
are dispersed in 61 parts of 64 O.P. ethanol to form a
gravure printing ink. A design is then applied to an
ultraviolet radiation cured butylmethacrylate coated paper
as used in Example 8 by gravure printing using a force of
9 Kg cm 1 and a running speed of 20 cm sec 1.
The printed paper is then used to decorate a
cotton fabric by the procedure described in Example 6.
The fabric is thus decorated with a blue design of very
high washing and dry cleaning fastness.
-23-

Representative Drawing

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Administrative Status

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Event History

Description Date
Inactive: Expired (old Act Patent) latest possible expiry date 1998-01-13
Grant by Issuance 1981-01-13

Abandonment History

There is no abandonment history.

Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
LEWIS, EDWARD J.
RATTEE, IAN D.
Past Owners on Record
EDWARD J. LEWIS
IAN D. RATTEE
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Claims 1994-03-04 6 186
Cover Page 1994-03-04 1 8
Abstract 1994-03-04 1 16
Drawings 1994-03-04 1 5
Descriptions 1994-03-04 24 696