CN118638495B - Single-component water-soluble acrylate pressure-sensitive adhesive and preparation method thereof - Google Patents
Single-component water-soluble acrylate pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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Abstract
The invention discloses a single-component water-soluble acrylate pressure-sensitive adhesive and a preparation method thereof, belonging to the technical field of pressure-sensitive adhesives, wherein the single-component water-soluble acrylate pressure-sensitive adhesive comprises the following components in percentage by mass: 35% 39% soft monomer, 2.5% 5% hard monomer, 3.5% 25% functional monomer, 0.01% 0.5% initiator, 50% 60% solvent, 0% 1.5% curing agent inhibitor, 3% 10% neutralizer, wherein, soft monomer comprises butyl acrylate, isooctyl acrylate and methoxy polyethylene glycol acrylic ester with molecular weight of 400, and the water-soluble pressure-sensitive adhesive of the invention does not need to add external curing agent under the premise of guaranteeing good mechanical property, is simple and economic, can be water-soluble and can be repulped, and can be fine solve the problem that the traditional adhesive cannot be water-soluble after film formation and leads to non-repulpable.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a single-component water-soluble acrylate pressure-sensitive adhesive and a preparation method thereof.
Background
The acrylic acid ester pressure-sensitive adhesive is generally a copolymer obtained by copolymerization of acrylic acid ester soft monomers such as butyl acrylate, isooctyl acrylate and the like as main materials, hard monomers such as methyl acrylate, methyl methacrylate, vinyl acetate and the like as well as functional monomers such as acrylic acid, hydroxyethyl acrylate, hydroxypropyl acrylate and the like. The acrylic acid ester pressure-sensitive adhesive has the advantages of excellent adhesive property, ageing resistance, low cost, stable performance, simple synthesis process and the like, so that the acrylic acid ester pressure-sensitive adhesive is very popular in the fields of self-adhesive tapes, labels, medicines, automobile parts, electronic appliances, home care and the like.
In recent years, acrylate pressure-sensitive adhesives have been more widely used and developed. With the progress of the age, people pay attention to the environmental protection of various products, saving, environmental protection and recycling are becoming the signs of the development of the society nowadays, and the water-based performance of acrylate pressure-sensitive adhesives is becoming a great trend of the industry in this respect. In the paper, printing and packaging industry, a large number of pressure sensitive adhesive articles are used, and therefore, in the waste paper that we regularly recycle, a large amount of adhesives are contained, which adhere to the fibers and are difficult to remove, and then affect the normal operation of the production equipment, reducing the production efficiency, and therefore waste paper containing conventional adhesives is generally considered to be non-repulpable. To address this problem, redevelopment of repulpable adhesives has become a very important direction.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the application and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application.
Therefore, the invention aims to provide a single-component water-soluble acrylate pressure-sensitive adhesive and a preparation method thereof, which can well solve the problem that the traditional adhesive cannot be dissolved in water after film formation and cannot be repulpable on the premise of ensuring good mechanical properties.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
a single-component water-soluble acrylate pressure-sensitive adhesive comprises the following components in percentage by mass:
35 to 39 percent of soft monomer, 2.5 to 5 percent of hard monomer, 3.5 to 25 percent of functional monomer, 0.01 to 0.5 percent of initiator, 50 to 60 percent of solvent, 0 to 1.5 percent of curing agent inhibitor and 3 to 10 percent of neutralizer;
wherein the soft monomer consists of butyl acrylate, isooctyl acrylate and methoxy polyethylene glycol acrylate with a molecular weight of 400.
As a preferable scheme of the one-component water-soluble acrylate pressure-sensitive adhesive, the hard monomer is one or more of methyl acrylate, methyl methacrylate, vinyl acetate and styrene.
As a preferable scheme of the single-component water-soluble acrylate pressure-sensitive adhesive, the functional monomer is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate, hydroxypropyl acrylate, N-methylolacrylamide and glycidyl methacrylate.
As a preferable scheme of the one-component water-soluble acrylate pressure-sensitive adhesive, the initiator is one or two of azodiisobutyronitrile and dibenzoyl peroxide.
As a preferable scheme of the single-component water-soluble acrylate pressure-sensitive adhesive, the solvent is one or more of ethanol, ethyl acetate, isopropanol, acetone, methanol and toluene.
As a preferable scheme of the one-component water-soluble acrylate pressure-sensitive adhesive, the curing agent is aluminum acetylacetonate, and the curing agent inhibitor is acetylacetone.
As a preferable scheme of the single-component water-soluble acrylate pressure-sensitive adhesive, the neutralizing agent is one or more of AMP-95, triethanolamine and sodium hydroxide aqueous solution.
A method for a single-component water-soluble acrylate pressure-sensitive adhesive comprises the following specific steps:
s1, weighing all the required solvents according to a proportion, uniformly mixing, putting into a reaction bottle, stirring, heating to 74-85 ℃ through water bath to generate stable reflux;
S2, weighing the required monomers and the initiator according to a proportion, uniformly mixing, and after the initiator is completely dissolved and the reflux in the reaction bottle is stable, starting to drop the mixture into the reaction bottle through a constant-pressure separating funnel, wherein the dropping is completed after 2 hours of use;
S3, after the mixed monomers are dripped, a first section of heat preservation is started at a reflux temperature, the first section of heat preservation time is 2 hours, a first group of initiators which are dissolved by the solvent are added after the heat preservation is finished, then a second section of heat preservation is carried out at the reflux temperature, the second section of heat preservation time is 1 hour, a second group of initiators which are dissolved by the solvent are added after the heat preservation is finished, then a third section of heat preservation is carried out at the reflux temperature, and the third section of heat preservation time is 2 hours;
and S4, after the third section of heat preservation is finished, cooling to 40 ℃, adding a diluting solvent, a curing agent and a neutralizing agent, and stirring to obtain the required single-component water-soluble acrylate pressure-sensitive adhesive.
Compared with the prior art, the invention has the following beneficial effects: the water-soluble pressure-sensitive adhesive prepared by the invention has good mechanical property, does not need to add external curing agent, is simple and economical, and can be dissolved in water for repulping.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following detailed description will be given with reference to the accompanying drawings and detailed embodiments, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained from these drawings without inventive faculty for a person skilled in the art. Wherein:
FIG. 1 is a flow chart of a method of the present invention for a one-component water-soluble acrylate pressure sensitive adhesive.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings.
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
The invention provides a single-component water-soluble acrylate pressure-sensitive adhesive and a preparation method thereof, which can well solve the problem that the traditional adhesive cannot be dissolved in water after film formation and cannot be repulpable under the premise of ensuring good mechanical properties.
To illustrate the above scheme, the following examples 1-4 and comparative examples 1-2 were provided for verification.
Example 1
Accurately weighing 33g of acetone, 100g of isopropanol and 40g of ethanol, uniformly mixing, adding the mixture into a reaction bottle, starting heating to about 75 ℃, allowing a solvent to start to flow back stably, accurately weighing 145g of butyl acrylate, 20g of acrylic acid, 15g of vinyl acetate, 20g of hydroxyethyl acrylate, 0.125g of azobisisobutyronitrile, uniformly mixing, adding the mixture into a constant pressure separating funnel, dripping for 2 hours, after dripping, starting to perform first-stage heat preservation at a reflux temperature for 2 hours, adding 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone after the first-stage heat preservation, starting to perform second-stage heat preservation for 1 hour, adding 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone after the second-stage heat preservation, and starting to perform third-stage heat preservation for 2 hours. After the third period of heat preservation is finished and the temperature is reduced to 40 ℃,20g of isopropanol is added for dilution, and then 12.4g of AMP-95 is added for neutralization, so that a hydrosol sample is obtained.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Example 2
117G of ethyl acetate and 16g of isopropanol are accurately weighed, are uniformly mixed and added into a reaction bottle, and are heated to about 78 ℃ to ensure that the solvent starts to flow back stably. 57g of butyl acrylate, 58g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 40g of ethoxyethoxyethoxyethyl acrylate, 0.1g of dibenzoyl peroxide are accurately weighed, added into a constant pressure separating funnel after being uniformly mixed, dripped for 2 hours, subjected to first-stage heat preservation at reflux temperature for 2 hours after dripping, added with 0.2g of dibenzoyl peroxide dissolved by 2.5g of ethyl acetate after the first-stage heat preservation, subjected to second-stage heat preservation for 1 hour, added with 0.2g of dibenzoyl peroxide dissolved by 2.5g of ethyl acetate after the second-stage heat preservation, subjected to third-stage heat preservation for 2 hours, subjected to third-stage heat preservation, added with 55g of isopropanol for dilution after the third-stage heat preservation is finished, and neutralized by 16.6g of triethanolamine after the dripping is finished, and a hydrosol sample is obtained.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Example 3
117G of ethyl acetate and 16g of isopropanol are accurately weighed, uniformly mixed and added into a reaction bottle, the temperature is started to rise to about 78 ℃, the solvent starts to flow back stably, 57.5g of butyl acrylate, 57.5g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 40g of methoxy polyethylene glycol acrylate (400), 0.05g of azobisisobutyronitrile are accurately weighed, uniformly mixed and added into a constant pressure separating funnel, the time is 2 hours, after the end of the dropwise addition, the first section of heat preservation is started at the reflux temperature for 2 hours, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the first section of heat preservation, the second section of heat preservation is started for 1 hour, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the second section of heat preservation, the third section of heat preservation is started for 2 hours, the third section of heat preservation time is ended, the third section of time is cooled to be started, the temperature is reduced to 40 ℃, 55g of isopropanol is added, 1.5 g of water-diluted acetone and 1g of water-diluted acetone solution are added, and 1g of water-diluted acetone solution is neutralized, and 1g of acetone solution is obtained.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Example 4
101G of ethyl acetate, 19.3g of isopropanol and 43.3g of toluene are accurately weighed and uniformly mixed and added into a reaction bottle, the temperature is started to rise to about 81 ℃, the solvent starts to flow back stably, 68g of butyl acrylate, 67g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 20g of ethoxyethoxyethyl acrylate (600), 0.05g of azobisisobutyronitrile, the mixture is uniformly mixed and added into a constant pressure separating funnel, the time is 2 hours, after the dripping is finished, the first section of heat preservation is started at the reflux temperature, the heat preservation time is 2 hours, the first section of heat preservation is finished, the 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added, the second section of heat preservation time is 1 hour, the second section of heat preservation is finished, the 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added, the third section of heat preservation time is started to be 2 hours, the third section of heat preservation time is finished, the temperature is reduced to 40 ℃, the water solution is added into 3.7g of isopropanol, and 2.0 g of water solution of acetylacetone is added into 2.0% of water, and the water solution is obtained.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Comparative example 1
Accurately weighing 33g of acetone, 100g of isopropanol and 40g of ethanol, uniformly mixing, adding the mixture into a reaction bottle, starting heating to about 75 ℃, allowing a solvent to start to flow back stably, accurately weighing 153g of butyl acrylate, 12g of acrylic acid, 15g of vinyl acetate, 20g of hydroxyethyl acrylate, 0.125g of azobisisobutyronitrile, uniformly mixing, adding into a constant pressure separating funnel, dripping for 2 hours, performing first-stage heat preservation at a reflux temperature after dripping is finished, keeping the temperature for 2 hours, adding 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone after the first-stage heat preservation is finished, starting second-stage heat preservation, keeping the temperature for 1 hour, adding 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone after the second-stage heat preservation is finished, starting third-stage heat preservation, keeping the temperature for 2 hours, cooling to 40 ℃ after the third-stage heat preservation, adding 20g of isopropanol, and neutralizing to obtain a water-in sol sample.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Comparative example 2:
Accurately weighing 33g of acetone, 100g of isopropanol and 40g of ethanol, uniformly mixing, adding the mixture into a reaction bottle, heating to about 75 ℃ and allowing the solvent to start to flow back stably. 153g of butyl acrylate, 12g of acrylic acid, 15g of vinyl acetate, 20g of hydroxyethyl acrylate and 0.125g of azodiisobutyronitrile are accurately weighed, are added into a constant pressure separating funnel after being uniformly mixed, are dripped for 2 hours, are subjected to first-stage heat preservation at reflux temperature, the heat preservation time is 2 hours, 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone is added after the first-stage heat preservation is finished, the second-stage heat preservation is started, the second-stage heat preservation time is 1 hour, 0.25g of dibenzoyl peroxide dissolved by 2.5g of acetone is added after the second-stage heat preservation is finished, the third-stage heat preservation time is 2 hours, and are added with 20g of isopropanol for dilution after the third-stage heat preservation time is finished and is cooled to 40 ℃, and are added with 12.4g of AMP-95 for neutralization, and 1g of acetylacetone aluminum are added, so that a hydrosol sample is obtained.
The prepared hydrosol sample is coated on the corona surface of a transparent PET film with the thickness of 25 mu m, the thickness of the coated dry glue is about 25 mu m, and the coated dry glue is baked for 2 minutes at the temperature of 120 ℃ and then is attached to the release PET, so that the hydrosol adhesive tape is obtained.
Four tape samples prepared in the above 4 examples and 2 comparative examples were tested for peel force according to the pressure-sensitive adhesive tape 180 ° peel strength test method GB/T2792-1998 and the ball primary adhesion test according to the pressure-sensitive adhesive tape primary adhesion test method-inclined plane ball method GB/T4852-2002. The water solubility test method comprises the following steps: cutting the adhesive tape with the width of 2.5cm and the length of 15cm, tearing off the release film, completely soaking in water, and observing the dissolution condition of the adhesive surface after 24 hours. The test results are shown in tables 1 and 2:
Table 1 shows the data of the one-component water-soluble pressure-sensitive adhesive instant property test prepared in examples 1 to 4 and comparative examples 1 to 2
| Sample of | 180 Degree peel force (N/25 mm) | Initial binding of rolling ball | Constant-temperature adhesive | Water-solubility |
| Example 1 | 14.4 | <3# | 2H drop off | 10% Dissolution |
| Example 2 | 14.8 | 13# | Drop for 15h | Completely dissolve |
| Example 3 | 11.5 | 16# | Drop for 70h | Completely dissolve |
| Example 4 | 15.2 | <3# | Drop for 20h | Completely dissolve |
| Comparative example 1 | 10.1 | 3# | 5H drop off | Can not be dissolved |
| Comparative example 2 | 8.2 | 3# | Drop for 80h | Can not be dissolved |
Table 2 shows the performance test data of the one-component water-soluble pressure-sensitive adhesives prepared in examples 1 to 4 and comparative examples 1 to 2 after curing
| Sample of | 180 Degree peel force (N/25 mm) | Initial binding of rolling ball | Constant-temperature adhesive | Water-solubility |
| Example 1 | 13.8 | <3# | Fall for 2h50min | 10% Dissolution |
| Example 2 | 14.5 | 13# | Drop for 15h | Completely dissolve |
| Example 3 | 10 | 14# | 126H drop off | Completely dissolve |
| Example 4 | 14.3 | <3# | Drop for 50h | Completely dissolve |
| Comparative example 1 | 9.8 | 3# | 5.5H drop off | Can not be dissolved |
| Comparative example 2 | 6.5 | 3# | 115H drop off | Can not be dissolved |
From the above test data of 4 examples and 2 comparative examples, it can be seen that the neutralized adhesive film was not water-soluble when the amount of acrylic acid was small, probably because the amount of acid was too small, the overall hydrophilicity after neutralization was still not strong enough to be water-soluble, and that the adhesive film was water-soluble in a small amount after increasing the amount of acrylic acid to 5%, but still was not fully soluble, and the initial tack was low overall after neutralization, as can be seen from example 1. After different soft monomers with stronger hydrophilicity are introduced in the examples 2-4, the water solubility of the adhesive film is obviously improved, the final water solubility is not affected even if a built-in curing agent is added, and when methoxy polyethylene glycol acrylate with the molecular weight of 400 is selected, the stripping force, the initial adhesion of the rolling ball, the normal-temperature adhesion and the water solubility can be better balanced, and the comprehensive performance is optimal.
Although the invention has been described hereinabove with reference to embodiments, various modifications thereof may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the features of the disclosed embodiments may be combined with each other in any manner as long as there is no structural conflict, and the exhaustive description of these combinations is not given in this specification merely for the sake of omitting the descriptions and saving resources. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (2)
1. A one-component water-soluble acrylate pressure-sensitive adhesive, characterized by comprising, by mass:
122g of ethyl acetate, 71g of isopropanol, 57.5g of butyl acrylate, 57.5g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 40g of methoxypolyethylene glycol acrylate with a molecular weight of 400, 0.25g of azobisisobutyronitrile, 1.85g of 30% aqueous sodium hydroxide solution, 10.4g of triethanolamine, 1g of acetylacetone and 1g of aluminum acetylacetonate;
Wherein, the single-component water-soluble acrylate pressure-sensitive adhesive is prepared as follows:
117g of ethyl acetate, 16g of isopropanol are accurately weighed, uniformly mixed and added into a reaction bottle, the temperature is started to rise to about 78 ℃, the solvent starts to flow back stably, 57.5g of butyl acrylate, 57.5g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 40g of methoxypolyethylene glycol acrylate with molecular weight of 400, 0.05g of azobisisobutyronitrile, uniformly mixed and added into a constant pressure separating funnel, the time is 2 hours, after the end of the dropwise addition, the first-stage heat preservation is started at the reflux temperature for 2 hours, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the first-stage heat preservation, the second-stage heat preservation is started for 1 hour, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the second-stage heat preservation, the third-stage heat preservation is started for 2 hours, the third-stage heat preservation time is started to be finished, the third-stage heat preservation time is cooled to be 40 ℃, 1g of isopropanol and 1.55 g of water-diluted acetone solution are added, and 1.3 g of water-phase acetone is added, and 1% of water-diluted acetone solution is obtained.
2. A method for preparing a one-component water-soluble acrylate pressure-sensitive adhesive as claimed in claim 1, characterized by the following specific steps:
117g of ethyl acetate, 16g of isopropanol are accurately weighed, uniformly mixed and added into a reaction bottle, the temperature is started to rise to about 78 ℃, the solvent starts to flow back stably, 57.5g of butyl acrylate, 57.5g of isooctyl acrylate, 20g of acrylic acid, 15g of methyl acrylate, 10g of hydroxyethyl acrylate, 40g of methoxypolyethylene glycol acrylate with molecular weight of 400, 0.05g of azobisisobutyronitrile, uniformly mixed and added into a constant pressure separating funnel, the time is 2 hours, after the end of the dropwise addition, the first-stage heat preservation is started at the reflux temperature for 2 hours, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the first-stage heat preservation, the second-stage heat preservation is started for 1 hour, 0.1g of azobisisobutyronitrile dissolved by 2.5g of ethyl acetate is added after the end of the second-stage heat preservation, the third-stage heat preservation is started for 2 hours, the third-stage heat preservation time is started to be finished, the third-stage heat preservation time is cooled to be 40 ℃, 1g of isopropanol and 1.55 g of water-diluted acetone solution are added, and 1.3 g of water-phase acetone is added, and 1% of water-diluted acetone solution is obtained.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202411118878.5A CN118638495B (en) | 2024-08-15 | 2024-08-15 | Single-component water-soluble acrylate pressure-sensitive adhesive and preparation method thereof |
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| CN202411118878.5A CN118638495B (en) | 2024-08-15 | 2024-08-15 | Single-component water-soluble acrylate pressure-sensitive adhesive and preparation method thereof |
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| CN108659752A (en) * | 2018-04-11 | 2018-10-16 | 无锡海特新材料研究院有限公司 | A kind of label water-soluble polyacrylate pressure sensitive adhesive, preparation method and application |
| CN113549413A (en) * | 2021-08-16 | 2021-10-26 | 江苏耐斯数码科技股份有限公司 | Benzene-free solvent-type peelable pressure-sensitive adhesive and preparation method thereof |
| CN116536006A (en) * | 2023-06-15 | 2023-08-04 | 太仓斯迪克新材料科技有限公司 | Antistatic acrylic ester emulsion pressure-sensitive adhesive, preparation method thereof and pressure-sensitive adhesive protective film |
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| AU665567B2 (en) * | 1991-09-23 | 1996-01-11 | Minnesota Mining And Manufacturing Company | Pressure sensitive adhesive composition which is repulpable under acidic pH conditions |
| JP5422091B2 (en) * | 2003-12-26 | 2014-02-19 | 東洋インキＳｃホールディングス株式会社 | Antistatic acrylic adhesive |
| EP3345942B1 (en) * | 2017-01-05 | 2020-04-01 | IGM Resins Italia S.r.l. | Composition useful as a pressure sensitive adhesive, its use and adhesive articles comprising it |
| CN110467890B (en) * | 2019-07-16 | 2021-09-17 | 广州慧谷工程材料有限公司 | Pressure-sensitive adhesive tape, method for producing same, and resin composition for producing pressure-sensitive adhesive tape |
| CN115612428A (en) * | 2022-09-05 | 2023-01-17 | 江苏斯迪克新材料科技股份有限公司 | Acrylic pressure-sensitive adhesive and preparation method thereof, polarizer protective film and preparation method thereof |
| CN116023603A (en) * | 2023-01-06 | 2023-04-28 | 中国乐凯集团有限公司 | Acrylate polymer, pressure-sensitive adhesive composition, protective film and display device |
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| CN108659752A (en) * | 2018-04-11 | 2018-10-16 | 无锡海特新材料研究院有限公司 | A kind of label water-soluble polyacrylate pressure sensitive adhesive, preparation method and application |
| CN113549413A (en) * | 2021-08-16 | 2021-10-26 | 江苏耐斯数码科技股份有限公司 | Benzene-free solvent-type peelable pressure-sensitive adhesive and preparation method thereof |
| CN116536006A (en) * | 2023-06-15 | 2023-08-04 | 太仓斯迪克新材料科技有限公司 | Antistatic acrylic ester emulsion pressure-sensitive adhesive, preparation method thereof and pressure-sensitive adhesive protective film |
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