CN116694142A - Pigment with good coloring effect for printing transfer printing film and preparation method thereof - Google Patents

Pigment with good coloring effect for printing transfer printing film and preparation method thereof Download PDF

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Publication number
CN116694142A
CN116694142A CN202310981765.7A CN202310981765A CN116694142A CN 116694142 A CN116694142 A CN 116694142A CN 202310981765 A CN202310981765 A CN 202310981765A CN 116694142 A CN116694142 A CN 116694142A
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parts
pigment
printing
coloring effect
preparing
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CN202310981765.7A
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Inventor
吴行正
闫小菊
林美招
胡永玲
汤政锋
曾维香
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Jinjiang Houde Printing Co ltd
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Jinjiang Houde Printing Co ltd
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Priority to CN202310981765.7A priority Critical patent/CN116694142A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00Pigment pastes, e.g. for mixing in paints

Abstract

The invention relates to a pigment with good coloring effect for printing a transfer printing film and a preparation method thereof, belonging to the field of pigments, wherein the pigment with good coloring effect for printing the transfer printing film comprises the following components in parts by weight: 50-60 parts of composite emulsion, 5-8 parts of calcium stearate, 20-25 parts of colorant, 1-3 parts of silane coupling agent, 3-6 parts of light calcium carbonate, 5-8 parts of diluent, 1-3 parts of paraffin and 2-4 parts of polydimethylsiloxane. The pigment obtained by the invention has good tinting strength and tinting strength.

Description

Pigment with good coloring effect for printing transfer printing film and preparation method thereof
Technical Field
The invention relates to the field of pigments, in particular to a pigment with good coloring effect for printing a transfer film and a preparation method thereof.
Background
The transfer film is an intermediate carrier, present on a transfer paper or plastic substrate, carrying the printed or printed pattern for transfer to a layer of chemoelastic film on the printed article. The existing transfer film generally adopts a soluble pigment as a colorant, which is the most main colorant, because the pigment can be directly dissolved in a solvent, and is very convenient to use, however, due to the chemical property and physical property of the pigment, there are a plurality of defects such as: the general pigment has unsatisfactory light resistance, is easy to fade under the action of ultraviolet rays, and has poor light resistance; the pigment is highly transparent and has poor hiding power and tinting strength; the pigment is easy to be in a solvent, so that the solvent resistance of the pigment is often poor, and the problems of difficult transfer printing and uneven coloring can occur, so that the quality problems of grey and dullness of the color of a transfer printing film, incomplete transfer printing patterns (with defects) and the like are caused.
Disclosure of Invention
Accordingly, the present invention has an object to provide a pigment for printing a transfer film having a good coloring effect and having a good coloring power and a good coloring fastness, and a method for producing the same.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the pigment for printing the transfer film with good coloring effect comprises the following components in parts by weight: 50-60 parts of composite emulsion, 5-8 parts of calcium stearate, 20-25 parts of colorant, 1-3 parts of silane coupling agent, 3-6 parts of light calcium carbonate, 5-8 parts of diluent, 1-3 parts of paraffin and 2-4 parts of polydimethylsiloxane.
Preferably, the composition comprises the following components in parts by weight: 60 parts of composite emulsion, 8 parts of calcium stearate, 25 parts of colorant, 3 parts of silane coupling agent, 6 parts of light calcium carbonate, 8 parts of diluent, 3 parts of paraffin and 4 parts of polydimethylsiloxane.
A preparation method of a pigment with good coloring effect for printing a transfer film comprises the following steps:
50-60 parts of composite emulsion, 5-8 parts of calcium stearate, 20-25 parts of colorant, 1-3 parts of silane coupling agent, 3-6 parts of light calcium carbonate, 5-8 parts of diluent, 1-3 parts of paraffin and 2-4 parts of polydimethylsiloxane are uniformly mixed and stirred according to parts by weight, and the pigment with good coloring effect for printing transfer printing films is obtained.
Preferably, the preparation method of the composite emulsion specifically comprises the following steps:
s1: preparing hollow silicon dioxide, a polyacrylic acid solution and polyurethane emulsion;
s2: mixing the hollow silicon dioxide obtained in the step S1, the polyacrylic acid solution and the polyurethane emulsion according to the weight ratio of 1:2:2, stirring for 20-30min, heating to 90-95 ℃, and reacting for 1-2h to obtain the composite emulsion.
Preferably, the preparation method of the hollow silica in the step S1 specifically includes the following steps:
s11: mixing polystyrene, cetyl trimethyl ammonium bromide, ammonia water solution with the volume fraction of 50% and ethanol solution with the volume fraction of 75%, and stirring for 30-50min to obtain polystyrene mixed solution;
s12: and (3) adding tetraethoxysilane into the polystyrene mixed solution obtained in the step (S11), continuously stirring for 48-72h, filtering, and drying to obtain the hollow silicon dioxide.
Preferably, the weight ratio of the polystyrene to the hexadecyl trimethyl ammonium bromide to the ammonia solution to the ethanol solution is 2:1:4:6, and the weight ratio of the polystyrene mixed solution to the tetraethoxysilane is 3:1.
Preferably, the preparation method of the polyacrylic acid solution in the step S1 specifically includes the following steps: mixing and stirring ammonium persulfate, acrylic acid, isopropanol and water according to the weight ratio of 1:5:4:3 for 20-30min, and then carrying out heat preservation reaction for 10-20min at 60-70 ℃ to obtain a polyacrylic acid solution.
Preferably, the preparation method of the polyurethane emulsion in the step S1 specifically includes the following steps:
mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 1-2 hours at 80-85 ℃, adding triethylamine, and continuing to react for 20-30 minutes to obtain polyurethane emulsion.
Preferably, the weight ratio of the 2, 4-toluene diisocyanate, the polypropylene glycol, the 2, 2-dimethylolpropionic acid and the triethylamine is 3:3:3:4.
Preferably, the preparation method of the diluent comprises the following steps: PVB resin, n-butanol and methanol were mixed according to 1:8:10, stirring for 24-36h to obtain a softened mixture, and mixing n-butanol, methanol and the softened mixture according to the weight ratio of 1:1:20, adding n-butanol and methanol into the softened mixture for the second time, and continuously stirring for 24-48 hours to obtain a refined mixture, wherein the weight ratio of the methanol to the refined mixture is 1:10, adding methanol into the refined mixture for the third time, and continuously stirring for 12-18h to obtain the diluent.
The molecular chains of the polymer emulsion in the composite emulsion are mutually entangled, a network structure with high surface energy can be formed, the addition of the hollow silicon dioxide further increases the active center of the network structure, so that the gaps among the molecular chains are reduced, ordered chain segments are increased, and cohesive force is increased, therefore, the emulsion has good steric hindrance and stability through electrostatic repulsive force existing between the molecular chains and the solution in the emulsion and the activity of the hollow silicon dioxide, and the tinting strength and color fastness of the pigment are improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The colorant is an inorganic or organic pigment powder, and it is specifically described that the raw materials and the equipment of the present invention are commercially available, and are not specifically exemplified, wherein the raw materials of the present invention are commercially available and are well known to those skilled in the art.
Example 1
The pigment for printing the transfer film with good coloring effect comprises the following components in parts by weight: 60 parts of composite emulsion, 8 parts of calcium stearate, 25 parts of colorant, 3 parts of silane coupling agent, 6 parts of light calcium carbonate, 8 parts of diluent, 3 parts of paraffin and 4 parts of polydimethylsiloxane.
A preparation method of a pigment with good coloring effect for printing a transfer film comprises the following steps:
and mixing and stirring the composite emulsion, the calcium stearate, the colorant, the silane coupling agent, the light calcium carbonate, the diluent 8 parts, the paraffin and the polydimethylsiloxane uniformly to obtain the pigment with good coloring effect for printing the transfer printing film.
The preparation method of the composite emulsion specifically comprises the following steps:
s1: preparation of hollow silica:
s11: mixing polystyrene, cetyl trimethyl ammonium bromide, ammonia water solution with the volume fraction of 50% and ethanol solution with the volume fraction of 75% according to the weight ratio of 2:1:4:6, and stirring for 50min to obtain polystyrene mixed solution;
s12: adding ethyl orthosilicate into the polystyrene mixed solution obtained in the step S11, continuously stirring for 72 hours, filtering, and drying to obtain hollow silicon dioxide, wherein the weight ratio of the polystyrene mixed solution to the ethyl orthosilicate is 3:1;
preparing a polyacrylic acid solution: mixing and stirring ammonium persulfate, acrylic acid, isopropanol and water according to the weight ratio of 1:5:4:3 for 30min, and then carrying out heat preservation reaction for 20min at 70 ℃ to obtain a polyacrylic acid solution;
preparing polyurethane emulsion: mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 2 hours at 85 ℃, adding triethylamine, and continuing to react for 30 minutes to obtain polyurethane emulsion, wherein the weight ratio of the 2, 4-toluene diisocyanate to the polypropylene glycol to the 2, 2-dimethylolpropionic acid to the triethylamine is 3:3:3:4;
s2: and (2) mixing the hollow silica, the polyurethane emulsion and the polyacrylic acid solution obtained in the step (S1) according to the weight ratio of 1:2:2, stirring for 30min, heating to 95 ℃, and reacting for 2h to obtain the composite emulsion.
The preparation method of the diluent comprises the following steps: PVB resin, n-butanol and methanol were mixed according to 1:8:10, stirring for 36h to obtain a softened mixture, and mixing n-butanol, methanol and the softened mixture according to the weight ratio of 1:1:20, adding n-butanol and methanol into the softened mixture for the second time, and continuously stirring for 48 hours to obtain a refined mixture, wherein the weight ratio of the methanol to the refined mixture is 1:10, adding methanol into the refined mixture for the third time, and continuously stirring for 18 hours to obtain the diluent.
Example 2
The pigment for printing the transfer film with good coloring effect comprises the following components in parts by weight: 50 parts of composite emulsion, 5 parts of calcium stearate, 20 parts of colorant, 1 part of silane coupling agent, 3 parts of light calcium carbonate, 5 parts of diluent, 1 part of paraffin and 2 parts of polydimethylsiloxane.
A preparation method of a pigment with good coloring effect for printing a transfer film comprises the following steps:
and mixing and stirring the composite emulsion, calcium stearate, a colorant, a silane coupling agent, light calcium carbonate, 5 parts of a diluent, paraffin and polydimethylsiloxane uniformly to obtain the pigment with good coloring effect for printing the transfer printing film.
The preparation method of the composite emulsion specifically comprises the following steps:
s1: preparation of hollow silica:
s11: mixing polystyrene, cetyl trimethyl ammonium bromide, ammonia water solution with the volume fraction of 50% and ethanol solution with the volume fraction of 75% according to the weight ratio of 2:1:4:6, and stirring for 30min to obtain polystyrene mixed solution;
s12: adding ethyl orthosilicate into the polystyrene mixed solution obtained in the step S11, continuously stirring for 48 hours, filtering, and drying to obtain hollow silicon dioxide, wherein the weight ratio of the polystyrene mixed solution to the ethyl orthosilicate is 3:1;
preparing a polyacrylic acid solution: mixing and stirring ammonium persulfate, acrylic acid, isopropanol and water according to the weight ratio of 1:5:4:3 for 20min, and then carrying out heat preservation reaction at 60 ℃ for 10min to obtain a polyacrylic acid solution;
preparing polyurethane emulsion: mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 1h at 80 ℃, adding triethylamine, and continuing to react for 20min to obtain polyurethane emulsion, wherein the weight ratio of the 2, 4-toluene diisocyanate to the polypropylene glycol to the 2, 2-dimethylolpropionic acid to the triethylamine is 3:3:3:4;
s2: and (2) mixing the hollow silica, the polyurethane emulsion and the polyacrylic acid solution obtained in the step (S1) according to the weight ratio of 1:2:2, stirring for 20min, heating to 90 ℃, and reacting for 1h to obtain the composite emulsion.
The preparation method of the diluent comprises the following steps: PVB resin, n-butanol and methanol were mixed according to 1:8:10, stirring for 24 hours to obtain a softened mixture, and mixing n-butanol, methanol and the softened mixture according to the weight ratio of 1:1:20, adding n-butanol and methanol into the softened mixture for the second time, and continuously stirring for 24 hours to obtain a refined mixture, wherein the weight ratio of the methanol to the refined mixture is 1:10, adding methanol into the refined mixture for the third time, and continuously stirring for 12 hours to obtain the diluent.
Example 3
The pigment for printing the transfer film with good coloring effect comprises the following components in parts by weight: 55 parts of composite emulsion, 6 parts of calcium stearate, 23 parts of colorant, 2 parts of silane coupling agent, 4 parts of light calcium carbonate, 6 parts of diluent, 2 parts of paraffin and 3 parts of polydimethylsiloxane.
A preparation method of a pigment with good coloring effect for printing a transfer film comprises the following steps:
and mixing and stirring the composite emulsion, calcium stearate, a colorant, a silane coupling agent, light calcium carbonate, 6 parts of a diluent, paraffin and polydimethylsiloxane uniformly to obtain the pigment with good coloring effect for printing the transfer printing film.
The preparation method of the composite emulsion specifically comprises the following steps:
s1: preparation of hollow silica:
s11: mixing polystyrene, cetyl trimethyl ammonium bromide, ammonia water solution with the volume fraction of 50% and ethanol solution with the volume fraction of 75% according to the weight ratio of 2:1:4:6, and stirring for 40min to obtain polystyrene mixed solution;
s12: adding ethyl orthosilicate into the polystyrene mixed solution obtained in the step S11, continuously stirring for 60 hours, filtering, and drying to obtain hollow silicon dioxide, wherein the weight ratio of the polystyrene mixed solution to the ethyl orthosilicate is 3:1;
preparing a polyacrylic acid solution: mixing and stirring ammonium persulfate, acrylic acid, isopropanol and water according to the weight ratio of 1:5:4:3 for 25min, and then carrying out heat preservation reaction for 15min at 65 ℃ to obtain a polyacrylic acid solution;
preparing polyurethane emulsion: mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 1.5 hours at 82 ℃, adding triethylamine, and continuing to react for 25 minutes to obtain polyurethane emulsion, wherein the weight ratio of the 2, 4-toluene diisocyanate to the polypropylene glycol to the 2, 2-dimethylolpropionic acid to the triethylamine is 3:3:3:4;
s2: and (2) mixing the hollow silica, the polyurethane emulsion and the polyacrylic acid solution obtained in the step (S1) according to the weight ratio of 1:2:2, stirring for 25min, heating to 92 ℃, and reacting for 1.5h to obtain the composite emulsion.
The preparation method of the diluent comprises the following steps: PVB resin, n-butanol and methanol were mixed according to 1:8:10, stirring for 28 hours to obtain a softened mixture, and mixing n-butanol, methanol and the softened mixture according to the weight ratio of 1:1:20, adding n-butanol and methanol into the softened mixture for the second time, and continuously stirring for 36 hours to obtain a refined mixture, wherein the weight ratio of the methanol to the refined mixture is 1:10, adding methanol into the refined mixture for the third time, and continuously stirring for 16 hours to obtain the diluent.
Comparative example 1
Comparative example 1 was prepared in substantially the same manner as in example 1, except that a polyurethane emulsion and a diluent were directly used, specifically:
the pigment for printing the transfer film comprises the following components in parts by weight: 60 parts of polyurethane emulsion, 8 parts of calcium stearate, 25 parts of colorant, 3 parts of silane coupling agent, 6 parts of light calcium carbonate, 3 parts of paraffin and 4 parts of polydimethylsiloxane.
A method for preparing a pigment for printing a transfer film, comprising the steps of:
and mixing and stirring the polyurethane emulsion, the calcium stearate, the colorant, the silane coupling agent, the light calcium carbonate, the paraffin wax and the polydimethylsiloxane uniformly in parts by weight to obtain the pigment with good coloring effect for printing the transfer printing film.
Preparing polyurethane emulsion: mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 2 hours at 85 ℃, adding triethylamine, and continuing to react for 30 minutes to obtain polyurethane emulsion, wherein the weight ratio of the 2, 4-toluene diisocyanate to the polypropylene glycol to the 2, 2-dimethylolpropionic acid to the triethylamine is 3:3:3:4.
The pigments obtained in examples 1 to 3 and comparative example 1 were each tested, and the test results are shown in Table 1.
Relative tinting strength test: testing the relative tinting strength change of pigment paste according to the method B (instrumental method) described in HG/T3951-2007 appendix B after 1 day and 180 days of storage at 25 ℃ just after preparation, taking the paste of each example and comparative example just after 1 day of preparation as standard paste, the tinting strength of the paste is 100%, and testing the relative tinting strength of the corresponding paste after 180 days of storage at normal temperature;
color difference test: placing the pigment at 35 ℃ and 80% humidity for 3 months, and measuring the color difference delta E1; placing for 3 months at 100deg.C under 50% humidity, and measuring its color difference delta E2;
stability test: the pigment paste is placed for 180 days at 25 ℃, and the stability of the pigment paste is judged by visually observing whether obvious pigment particle precipitation, flocculation, layering and caking stability occur or not.
Table 1 test data for pigments of examples 1-3 and comparative example 1
As can be seen from the above table, the pigments of examples 1 to 3 have good stability with respect to the pigment paste obtained in comparative example 1, and the coloring power is kept good.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The pigment for printing the transfer film with good coloring effect is characterized by comprising the following components in parts by weight: 50-60 parts of composite emulsion, 5-8 parts of calcium stearate, 20-25 parts of colorant, 1-3 parts of silane coupling agent, 3-6 parts of light calcium carbonate, 5-8 parts of diluent, 1-3 parts of paraffin and 2-4 parts of polydimethylsiloxane.
2. The pigment for printing a transfer film having a good coloring effect according to claim 1, comprising the following components in parts by weight: 60 parts of composite emulsion, 8 parts of calcium stearate, 25 parts of colorant, 3 parts of silane coupling agent, 6 parts of light calcium carbonate, 8 parts of diluent, 3 parts of paraffin and 4 parts of polydimethylsiloxane.
3. The preparation method of the pigment for printing the transfer film with good coloring effect is characterized by comprising the following steps of:
50-60 parts of composite emulsion, 5-8 parts of calcium stearate, 20-25 parts of colorant, 1-3 parts of silane coupling agent, 3-6 parts of light calcium carbonate, 5-8 parts of diluent, 1-3 parts of paraffin and 2-4 parts of polydimethylsiloxane are uniformly mixed and stirred according to parts by weight, and the pigment with good coloring effect for printing transfer printing films is obtained.
4. The method for preparing a pigment for printing on a transfer film with good coloring effect according to claim 3, wherein the method for preparing the composite emulsion specifically comprises the following steps:
s1: preparing hollow silicon dioxide, a polyacrylic acid solution and polyurethane emulsion;
s2: mixing the hollow silicon dioxide obtained in the step S1, the polyacrylic acid solution and the polyurethane emulsion according to the weight ratio of 1:2:2, stirring for 20-30min, heating to 90-95 ℃, and reacting for 1-2h to obtain the composite emulsion.
5. The method for preparing a pigment for printing on a transfer film having a good coloring effect according to claim 4, wherein the method for preparing hollow silica in step S1 comprises the steps of:
s11: mixing polystyrene, cetyl trimethyl ammonium bromide, ammonia water solution with the volume fraction of 50% and ethanol solution with the volume fraction of 75%, and stirring for 30-50min to obtain polystyrene mixed solution;
s12: and (3) adding tetraethoxysilane into the polystyrene mixed solution obtained in the step (S11), continuously stirring for 48-72h, filtering, and drying to obtain the hollow silicon dioxide.
6. The method for preparing a pigment for printing on a transfer film with good coloring effect according to claim 5, wherein the weight ratio of the polystyrene to the cetyltrimethylammonium bromide to the aqueous ammonia solution to the ethanol solution is 2:1:4:6, and the weight ratio of the polystyrene mixed solution to the tetraethyl orthosilicate is 3:1.
7. The method for preparing a pigment for printing on a transfer film having a good coloring effect according to claim 5, wherein the method for preparing the polyacrylic acid solution in step S1 specifically comprises the steps of: mixing and stirring ammonium persulfate, acrylic acid, isopropanol and water according to the weight ratio of 1:5:4:3 for 20-30min, and then carrying out heat preservation reaction for 10-20min at 60-70 ℃ to obtain a polyacrylic acid solution.
8. The method for preparing a pigment for printing on a transfer film having a good coloring effect according to claim 4, wherein the method for preparing the polyurethane emulsion in step S1 specifically comprises the steps of:
mixing 2, 4-toluene diisocyanate, polypropylene glycol and 2, 2-dimethylolpropionic acid, reacting for 1-2 hours at 80-85 ℃, adding triethylamine, and continuing to react for 20-30 minutes to obtain polyurethane emulsion.
9. The method for producing a pigment for printing on a transfer film having a good coloring effect according to claim 8, wherein the weight ratio of 2, 4-toluene diisocyanate, polypropylene glycol, 2-dimethylolpropionic acid and triethylamine is 3:3:3:4.
10. The method for preparing a pigment for printing on a transfer film having a good coloring effect according to claim 3, wherein the method for preparing the diluent comprises: PVB resin, n-butanol and methanol were mixed according to 1:8:10, stirring for 24-36h to obtain a softened mixture, and mixing n-butanol, methanol and the softened mixture according to the weight ratio of 1:1:20, adding n-butanol and methanol into the softened mixture for the second time, and continuously stirring for 24-48 hours to obtain a refined mixture, wherein the weight ratio of the methanol to the refined mixture is 1:10, adding methanol into the refined mixture for the third time, and continuously stirring for 12-18h to obtain the diluent.
CN202310981765.7A 2023-08-07 2023-08-07 Pigment with good coloring effect for printing transfer printing film and preparation method thereof Pending CN116694142A (en)

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CN115701386A (en) * 2021-08-02 2023-02-10 绍兴雅兰烫印箔膜有限公司 Preparation method of bright digital ink-jet printing thermal transfer printing film

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US4503172A (en) * 1983-05-20 1985-03-05 Allied Colloids Limited Water soluble polymers
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CN103384840A (en) * 2010-12-22 2013-11-06 三菱丽阳株式会社 Transfer film and method for producing same, and laminate and method for producing same
CN102992334A (en) * 2011-09-08 2013-03-27 江南大学 Hollow nano-grade silica particles and preparation method of heat-insulation paint thereof
KR20130083516A (en) * 2012-01-13 2013-07-23 한양잉크 주식회사 Water based foaming-ink composite for gravure printing and manufacturing method of non-woven fabrics wallpaper using the water based foaming-ink composite
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CN115701386A (en) * 2021-08-02 2023-02-10 绍兴雅兰烫印箔膜有限公司 Preparation method of bright digital ink-jet printing thermal transfer printing film

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