CN111620983A - Acrylate emulsion for moisture-resistant rubbing water-based ink and preparation method thereof - Google Patents
Acrylate emulsion for moisture-resistant rubbing water-based ink and preparation method thereof Download PDFInfo
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- CN111620983A CN111620983A CN202010541285.5A CN202010541285A CN111620983A CN 111620983 A CN111620983 A CN 111620983A CN 202010541285 A CN202010541285 A CN 202010541285A CN 111620983 A CN111620983 A CN 111620983A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
Abstract
The invention relates to an acrylate emulsion for moisture-resistant rubbing water-based ink and a preparation method thereof, wherein the acrylate emulsion comprises the following components: 8-12% of water-based acrylic resin, 0.9-1.7% of emulsifier, 52-58% of deionized water, 1-5% of functional monomer, 20-27% of soft monomer and 7-14% of hard monomer. The acrylic ester emulsion prepared by the invention has excellent performances of good stability, good flexibility, high adhesive force and the like, has good compatibility with color paste ground by the company, and the prepared water-based ink has high adhesive force, is water-resistant and moisture-resistant and rubs, effectively improves the application performance of the water-based ink and has lower cost.
Description
Technical Field
The invention belongs to the technical field of emulsion polymerization, and particularly relates to an acrylate emulsion for moisture-resistant rubbing water-based ink and a preparation method thereof.
Background
The water-based ink is prepared by using water as a solvent. The water-based ink mainly comprises a water-based binder, a pigment and related auxiliaries, and compared with the traditional solvent-based ink, the water-based ink does not contain volatile toxic organic solvents, has no adverse effect on the health of printer operators in the printing process, has no pollution to the atmospheric environment, and has no pollution to printed matters. The common resin of the water-based ink binder is water-based acrylate resin, amino resin, rosin modified maleic acid resin, polyester resin, water-based silicone resin, epoxy resin, alkyd resin, phenolic resin, water-based polyurethane and the like, and compared with the water-based acrylate resin and the modified product thereof, the water-based acrylate resin has incomparable advantages in the aspects of weather resistance, heat resistance, ink stability, printability and the like, and is the resin with the most wide application. However, water-based inks containing water-based acrylate resins as a binder also have problems such as poor water resistance and poor adhesion to low-polarity films. The water resistance of the water ink has important significance for the use of the water ink, because the water ink is often applied to packaging printing products, some products can be soaked in water for a long time or frozen in a refrigerator for a long time, if the water ink has poor water resistance and poor friction resistance, the water ink can be emulsified in water to lose luster, and can be completely faded in serious cases, so that the image of the product is influenced.
Disclosure of Invention
1. Technical problem to be solved by the invention
The invention aims to solve the problems of poor water resistance and poor rubbing resistance of the existing water-based ink emulsion.
2. Technical scheme
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention relates to an acrylate emulsion for moisture-resistant rubbing water-based ink, which comprises the following components: 8-12% of water-based acrylic resin, 0.9-1.7% of emulsifier, 52-58% of deionized water, 1-5% of functional monomer, 20-27% of soft monomer and 7-14% of hard monomer.
Preferably, the water-based acrylic resin is at least one of acrylic resins Solury 70, Solury 90, Solury 120, Joncryl67 and Joncryl 678.
Preferably, the emulsifier comprises an anionic emulsifier, a nonionic emulsifier and a reactive emulsifier, the anionic emulsifier is fatty alcohol ether sodium sulfate or alkylaryl polyoxyethylene ether ammonium sulfate, the nonionic emulsifier is isomeric tridecanol polyoxyethylene ether, and the reactive emulsifier is one of environment-friendly reactive emulsifiers SR-10 and ER-10.
Preferably, the functional monomer is at least one of acrylic acid, methacrylic acid, glycidyl methacrylate, self-crosslinking monomer diacetone acrylamide (DAAM), adipic Acid Dihydrazide (ADH), acetoacetoxyethyl methacrylate (AAEM) and silane coupling agent monomer, and the silane coupling agent monomer is one of vinyl trimethoxy silane, vinyl triethoxy silane, vinyl tri (beta-methoxyethoxy) silane and gamma- (methacryloyloxy) propyl trimethoxy silane.
Preferably, the soft monomer is at least one of n-butyl acrylate, isooctyl acrylate, lauryl methacrylate, beta-hydroxyethyl acrylate, beta-hydroxypropyl acrylate and stearyl acrylate; the hard monomer is methyl methacrylate or styrene.
A preparation method of acrylate emulsion for moisture-resistant rubbing water-based ink comprises the following steps:
s100, dissolving, namely dissolving the water-based acrylic resin in a reaction kettle at a high temperature;
s200, preparing a monomer pre-emulsion, and pre-emulsifying a part of emulsifier and all monomers;
s300, carrying out polymerization reaction, namely adding the rest of emulsifier and half of deionized water into a reaction kettle, adding the resin liquid prepared in the step one, introducing condensed water, introducing nitrogen, stirring and heating, adding 30-42.8% of initiator solution, simultaneously adding 5-20% of monomer pre-emulsion, stirring and reacting for 15min to form blue-phase seed emulsion, heating, controlling the temperature to be 80-90 ℃, simultaneously dropwise adding the rest of monomer pre-emulsion and initiator, reacting for 4h, cooling to 60-70 ℃, respectively adding redox initiator for removing residual monomer, and carrying out heat preservation reaction for 0.5 h;
s400, adjusting the pH value, cooling to 40 ℃, and adjusting the pH value to about 8.5;
s500, filtering and discharging, and filtering the feed liquid with the pH value adjusted to obtain the required emulsion.
Preferably, the initiator in step S300 is one of ammonium persulfate, potassium persulfate, and sodium persulfate.
Preferably, the redox initiator in step S300 is one of ammonium persulfate-sodium bisulfite, potassium persulfate-sodium bisulfite, tert-butyl hydroperoxide-sodium formaldehyde sulfoxylate, tert-butyl hydroperoxide-sodium bisulfite, and tert-butyl hydroperoxide-iso-ascorbic acid.
Preferably, the preparing of the monomer pre-emulsion in step S200 is to weigh 50-80% of the total amount of the emulsifier, 20-40% of the total amount of the deionized water, and pre-emulsify all the monomers to obtain the monomer pre-emulsion.
Preferably, the dissolving in the step S100 is to weigh 30% of aqueous solid acrylic resin, 8-12% of ammonia water, and 58-62% of deionized water, add into the reaction kettle, and heat up to 70-85 ℃ until the resin is completely dissolved, so as to obtain a light yellow clear solution.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
the invention relates to an acrylate emulsion for moisture-resistant rubbing water-based ink and a preparation method thereof, wherein the acrylate emulsion comprises the following components: 8-12% of water-based acrylic resin, 0.9-1.7% of emulsifier, 52-58% of deionized water, 1-5% of functional monomer, 20-27% of soft monomer and 7-14% of hard monomer. The acrylic ester emulsion prepared by the invention has excellent performances of good stability, good flexibility, high adhesive force and the like, has good compatibility with color paste ground by the company, and the prepared water-based ink has high adhesive force, is water-resistant and moisture-resistant and rubs, effectively improves the application performance of the water-based ink and has lower cost.
Drawings
FIG. 1 is a flow chart of a preparation method of an acrylate emulsion for wet rubbing resistant water-based ink according to the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in many different forms and are not limited to the embodiments described herein, but rather are provided for the purpose of providing a more thorough disclosure of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
Referring to the attached FIG. 1, the acrylate emulsion for wet rubbing resistant water-based ink of this embodiment comprises the following components: 8-12% of water-based acrylic resin, 0.9-1.7% of emulsifier, 52-58% of deionized water, 1-5% of functional monomer, 20-27% of soft monomer and 7-14% of hard monomer.
Wherein the water-based acrylic resin is at least one of acrylic resins Solury 70, Solury 90, Solury 120, Joncryl67 and Joncryl 678.
The emulsifier comprises an anionic emulsifier, a nonionic emulsifier and a reactive emulsifier, wherein the anionic emulsifier is fatty alcohol ether sodium sulfate or alkylaryl polyoxyethylene ether ammonium sulfate, the nonionic emulsifier is isomeric tridecanol polyoxyethylene ether, and the reactive emulsifier is one of environment-friendly reactive emulsifiers SR-10 and ER-10.
The functional monomer is at least one of acrylic acid, methacrylic acid, glycidyl methacrylate, self-crosslinking monomer diacetone acrylamide (DAAM), adipic Acid Dihydrazide (ADH), acetoacetoxyethyl methacrylate (AAEM) and silane coupling agent monomer, and the silane coupling agent monomer is one of vinyl trimethoxy silane, vinyl triethoxy silane, vinyl tri (beta-methoxyethoxy) silane and gamma- (methacryloyloxy) propyl trimethoxy silane.
Wherein the soft monomer is at least one of n-butyl acrylate, isooctyl acrylate, lauryl methacrylate, beta-hydroxyethyl acrylate, beta-hydroxypropyl acrylate and octadecyl acrylate; the hard monomer is methyl methacrylate or styrene.
A preparation method of acrylate emulsion for moisture-resistant rubbing water-based ink comprises the following steps:
s100, dissolving, namely dissolving the water-based acrylic resin in a reaction kettle at a high temperature;
s200, preparing a monomer pre-emulsion, and pre-emulsifying a part of emulsifier and all monomers;
s300, carrying out polymerization reaction, namely adding the rest of emulsifier and half of deionized water into a reaction kettle, adding the resin liquid prepared in the step one, introducing condensed water, introducing nitrogen, stirring and heating, adding 30-42.8% of initiator solution, simultaneously adding 5-20% of monomer pre-emulsion, stirring and reacting for 15min to form blue-phase seed emulsion, heating, controlling the temperature to be 80-90 ℃, simultaneously dropwise adding the rest of monomer pre-emulsion and initiator, reacting for 4h, cooling to 60-70 ℃, respectively adding redox initiator for removing residual monomer, and carrying out heat preservation reaction for 0.5 h;
s400, adjusting the pH value, cooling to 40 ℃, and adjusting the pH value to about 8.5;
s500, filtering and discharging, and filtering the feed liquid with the pH value adjusted to obtain the required emulsion.
The initiator in step S300 is one of ammonium persulfate, potassium persulfate, and sodium persulfate.
The redox initiator in step S300 is one of ammonium persulfate-sodium bisulfite, potassium persulfate-sodium bisulfite, t-butyl hydroperoxide-sodium formaldehyde sulfoxylate, t-butyl hydroperoxide-sodium bisulfite, and t-butyl hydroperoxide-iso-ascorbic acid.
The monomer pre-emulsion preparation in step S200 is to weigh 50-80% of the total amount of the emulsifier, 20-40% of the total amount of the deionized water, and pre-emulsify all monomers to prepare the monomer pre-emulsion.
The dissolving in the step S100 is to weigh 30% of aqueous solid acrylic resin, 8-12% of ammonia water and 58-62% of deionized water, add the mixture into a reaction kettle, and heat the mixture to 70-85 ℃ until the resin is completely dissolved, so as to obtain a light yellow clear solution.
| Name of raw materials | Weight/g |
| Aqueous solid acrylic resin S70+ S120 | 15+30 |
| Ammonia (25%) | 18 |
| Deionized water | 280 |
| Anionic emulsifiers | 4.14 |
| Nonionic emulsifiers | 2.5 |
| Reactive emulsifier | 1.25 |
| Soft monomer 1 | 70 |
| Soft monomer 2 | 10 |
| Soft monomer 3 | 60 |
| Methacrylic acid methyl ester | 20 |
| Styrene (meth) acrylic acid ester | 20 |
| Functional monomer 1 | 2 |
| Silane coupling agent monomer | 2 |
| Self-crosslinking monomers 1 | 6 |
| Self-crosslinking monomers 2 | 3 |
| Initiator | 1.8 |
| Redox initiators | 0.25 |
This example was prepared according to the components in the table above, as follows:
s100, dissolving, weighing aqueous solid acrylic resin S7015g, S12030 g, 18g of ammonia water and 87g of deionized water, adding into a reaction kettle, and heating to 80-85 ℃ until the resin is completely dissolved to obtain a light yellow clear solution;
s200, preparing monomer pre-emulsion, weighing 2.48g of anionic emulsifier, 1.5g of nonionic emulsifier, 0.75g of reactive emulsifier, 56g of deionized water, and all monomers for pre-emulsification to prepare monomer pre-emulsion;
s300, carrying out polymerization reaction, namely weighing the residual emulsifier and 140g of water, adding the rest emulsifier and 140g of water into a reaction kettle, adding the resin liquid obtained in the step S100, introducing condensed water, introducing nitrogen, heating to 80 ℃ while stirring, adding part of initiator solution and part of monomer pre-emulsion into the reaction kettle, and carrying out stirring reaction for 15min to obtain the blue-phase seed emulsion. And (3) heating and raising the temperature in a seed emulsion reaction system, controlling the temperature to be 80-90 ℃, and then simultaneously dropwise adding the residual monomer pre-emulsion and the initiator component for reacting for 4 hours in total. Cooling to 65 ℃, adding 0.25g of redox initiator for removing residual monomers, and reacting for 0.5h under heat preservation;
s400, adjusting the pH value, cooling to 40 ℃, and adjusting the pH value to 8.5;
s500, filtering and discharging, and filtering the feed liquid with the pH value adjusted to obtain the emulsion A.
The water-based ink A is prepared by the synthesized emulsion A according to the following proportion:
and mixing the emulsion A with the color paste which is ground in advance and other auxiliary agents, and mechanically blending to obtain the water-based ink A.
Example 2
| Name of raw materials | Weight/g |
| Aqueous solid acrylic resin J678 | 45 |
| Ammonia (25%) | 18 |
| Deionized water | 280 |
| Anionic emulsifiers | 8.28 |
| Reactive emulsifier | 4.21 |
| Soft monomer 1 | 80 |
| Soft monomer 2 | 10 |
| Soft monomer 3 | 50 |
| Methacrylic acid methyl ester | 20 |
| Styrene (meth) acrylic acid ester | 20 |
| Silane coupling agent monomer | 2 |
| Self-crosslinking monomers 1 | 6 |
| Self-crosslinking monomers 2 | 3 |
| Initiator | 1.8 |
| Redox initiators | 0.25 |
This example was prepared according to the components in the table above, as follows:
s100, dissolving, namely weighing aqueous solid acrylic resin J67845g, 18g of ammonia water and 87g of deionized water, adding into a reaction kettle, and heating to 85 ℃ until the resin is completely dissolved to obtain a light yellow clear solution;
s200, preparing monomer pre-emulsion, weighing 5.09g of anionic emulsifier, 2.53g of reactive emulsifier, 56g of deionized water and all monomers for pre-emulsification to prepare monomer pre-emulsion;
s300, carrying out polymerization reaction, weighing the rest emulsifier and 140g of water, adding the rest emulsifier and 140g of water into a reaction kettle, adding the resin liquid obtained in the step S100, introducing condensed water, introducing nitrogen, heating to 80 ℃ while stirring, adding part of initiator into the reaction kettle to be dissolved by deionized water, adding part of monomer pre-emulsion at the same time, and carrying out stirring reaction for 15min to form the blue-phase seed emulsion. And (3) heating and raising the temperature in a seed emulsion reaction system, controlling the temperature to be 80-90 ℃, and then simultaneously dropwise adding the residual monomer pre-emulsion and the initiator component for reacting for 4 hours in total. Cooling to 70 ℃, adding 0.25g of redox initiator for removing residual monomers, and reacting for 0.5h under heat preservation;
s400, adjusting the pH value, cooling to 40 ℃, and adjusting the pH value to 8.5;
s500, filtering and discharging, and filtering the feed liquid with the pH value adjusted to obtain emulsion B.
The synthesized emulsion B is used for preparing water-based ink B according to the following proportion:
and mixing the emulsion B with the color paste which is ground in advance and other auxiliary agents, and mechanically blending to obtain the water-based ink B.
The performance test results of the water-based inks A and B are as follows:
| sample (I) | Initial fastness | Fastness at 50 ℃ for 1h | Wet and rubbing resistance |
| A Water-based ink | 4-5 | 5 | >20 times (twice) |
| B Water-based ink | 4-5 | 5 | >15 times of |
The detection method of the water-based ink is tested according to GB/T13217.7-2009 liquid ink adhesion fastness detection method, QB/T4103-2010 water-based gravure plastic film surface printing ink.
The prepared water-based ink has good stability, moderate viscosity, high adhesion fastness, water resistance and wet rubbing resistance, can be normally used on a PE film blowing conjoined printing machine, and has the potential of large-scale production and application.
The above-mentioned embodiments only express a certain implementation mode of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention; it should be noted that, for those skilled in the art, without departing from the concept of the present invention, several variations and modifications can be made, which are within the protection scope of the present invention; therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The acrylic ester emulsion for the wet-rubbing-resistant water-based ink is characterized by comprising the following components: 8-12% of water-based acrylic resin, 0.9-1.7% of emulsifier, 52-58% of deionized water, 1-5% of functional monomer, 20-27% of soft monomer and 7-14% of hard monomer.
2. The acrylic ester emulsion for wet-rub resistant water-based ink according to claim 1, characterized in that: the water-based acrylic resin is at least one of acrylic resins Solury 70, Solury 90, Solury 120, Joncryl67 and Joncryl 678.
3. The acrylic ester emulsion for wet-rub resistant water-based ink according to claim 1, characterized in that: the emulsifier comprises an anionic emulsifier, a nonionic emulsifier and a reactive emulsifier, wherein the anionic emulsifier is fatty alcohol ether sodium sulfate or alkylaryl polyoxyethylene ether ammonium sulfate, the nonionic emulsifier is isomeric tridecanol polyoxyethylene ether, and the reactive emulsifier is one of environment-friendly reactive emulsifiers SR-10 and ER-10.
4. The acrylic ester emulsion for wet-rub resistant water-based ink according to claim 1, characterized in that: the functional monomer is at least one of acrylic acid, methacrylic acid, glycidyl methacrylate, self-crosslinking monomer diacetone acrylamide (DAAM), adipic Acid Dihydrazide (ADH), acetoacetoxyethyl methacrylate (AAEM) and silane coupling agent monomer, and the silane coupling agent monomer is one of vinyl trimethoxy silane, vinyl triethoxy silane, vinyl tri (beta-methoxyethoxy) silane and gamma- (methacryloyloxy) propyl trimethoxy silane.
5. The acrylic ester emulsion for wet-rub resistant water-based ink according to claim 1, characterized in that: the soft monomer is at least one of n-butyl acrylate, isooctyl acrylate, lauryl methacrylate, beta-hydroxyethyl acrylate, beta-hydroxypropyl acrylate and octadecyl acrylate; the hard monomer is methyl methacrylate or styrene.
6. The method for preparing the acrylate emulsion for the wet rubbing-resistant water-based ink according to any one of claims 1 to 5, characterized by comprising the following steps:
s100, dissolving, namely dissolving the water-based acrylic resin in a reaction kettle at a high temperature;
s200, preparing a monomer pre-emulsion, and pre-emulsifying a part of emulsifier and all monomers;
s300, carrying out polymerization reaction, namely adding the rest of emulsifier and half of deionized water into a reaction kettle, adding the resin liquid prepared in the step one, introducing condensed water, introducing nitrogen, stirring and heating, adding 30-42.8% of initiator solution, simultaneously adding 5-20% of monomer pre-emulsion, stirring and reacting for 15min to form blue-phase seed emulsion, heating, controlling the temperature to be 80-90 ℃, simultaneously dropwise adding the rest of monomer pre-emulsion and initiator, reacting for 4h, cooling to 60-70 ℃, respectively adding redox initiator for removing residual monomer, and carrying out heat preservation reaction for 0.5 h;
s400, adjusting the pH value, cooling to 40 ℃, and adjusting the pH value to about 8.5;
s500, filtering and discharging, and filtering the feed liquid with the pH value adjusted to obtain the required emulsion.
7. The method for preparing the acrylate emulsion for wet-rubbing resistant water-based ink according to claim 6, wherein the method comprises the following steps: the initiator in the step S300 is one of ammonium persulfate, potassium persulfate and sodium persulfate.
8. The method for preparing the acrylate emulsion for wet-rubbing resistant water-based ink according to claim 6, wherein the method comprises the following steps: the redox initiator in step S300 is one of ammonium persulfate-sodium bisulfite, potassium persulfate-sodium bisulfite, t-butyl hydroperoxide-sodium formaldehyde sulfoxylate, t-butyl hydroperoxide-sodium bisulfite, and t-butyl hydroperoxide-iso-ascorbic acid.
9. The method for preparing the acrylate emulsion for wet-rubbing resistant water-based ink according to claim 6, wherein the method comprises the following steps: the monomer pre-emulsion preparation in the step S200 is to weigh 50-80% of the total amount of the emulsifier, 20-40% of the total amount of the deionized water, and pre-emulsify all monomers to prepare the monomer pre-emulsion.
10. The method for preparing the acrylate emulsion for wet-rubbing resistant water-based ink according to claim 6, wherein the method comprises the following steps: the dissolving in the step S100 is to weigh 30% of aqueous solid acrylic resin, 8-12% of ammonia water and 58-62% of deionized water, add the weighed materials into a reaction kettle, and heat the materials to 70-85 ℃ until the resin is completely dissolved, so as to obtain a light yellow clear solution.
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