CN114573747A - Acrylate polymer for antistatic pressure-sensitive adhesive and preparation method thereof - Google Patents

Acrylate polymer for antistatic pressure-sensitive adhesive and preparation method thereof Download PDF

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CN114573747A
CN114573747A CN202210253912.4A CN202210253912A CN114573747A CN 114573747 A CN114573747 A CN 114573747A CN 202210253912 A CN202210253912 A CN 202210253912A CN 114573747 A CN114573747 A CN 114573747A
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polymer
acrylate
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sensitive adhesive
weight
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谢宠
阮晓亮
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Dongsheng Chemistry Shanghai Co ltd
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Dongsheng Chemistry Shanghai Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives 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
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/062Copolymers with monomers not covered by C09J133/06
    • C09J133/064Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38Pressure-sensitive adhesives [PSA]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses an acrylate polymer for an antistatic pressure-sensitive adhesive, which comprises a polymer, a solvent and an initiator; the polymer comprises a first unit containing an acrylate monomer, a second unit containing an alkenyloxy group and an ionic group and containing a double-bond polymerizable functional monomer, and a third unit containing a hydroxyl or carboxyl vinyl functional monomer, wherein the first unit accounts for 70-95% of the total weight of the polymer, the second unit accounts for 3-25% of the total weight of the polymer, and the third unit accounts for 1-7% of the total weight of the polymer; the weight percentage of the initiator, the polymer and the solvent is 0.0019-1.0021: 1: 1.00 to 1.60. The acrylate polymer for the antistatic pressure-sensitive adhesive can effectively solve the contradiction between static removal and the influence of low molecular weight substance separation on optical equipment, and has the advantages of simple method and easy popularization and use.

Description

Acrylate polymer for antistatic pressure-sensitive adhesive and preparation method thereof
Technical Field
The invention relates to the field of polymer synthesis, in particular to an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof.
Background
Static electricity is a unipolar charge carried by an object, which is relatively stationary, and is retained on the surface of the object, and is formed by electron or ion transfer as a result of a local imbalance between positive and negative charges. The reason for the unbalanced distribution of electrons is that the electrons are separated from the orbit by external force, which includes various energies (such as kinetic energy, potential energy, thermal energy, chemical energy, etc.), so that static electricity is generated in daily life, such as contact, friction, washing, electrolysis, piezoelectricity, deviation, induction, etc.
Electrostatic discharge can cause the following damage to semiconductor devices: 1. the thin oxide layer is broken down; 2. the leakage current density is high, causing the conductor to be fused; 3. increased leakage current, which causes premature failure, and functional damage to the device from breakdown voltage variations. With the application of large-scale MOS circuits and Surface Mount Devices (SMDs) and the development of device process technologies, the energy sensitivity to electrostatic discharge (ESD) is increased, and thin insulating layers are easily damaged and fail.
The harm of static electricity to the production of electronic products mainly comprises the following aspects: 1. dust in air is adsorbed by static electricity, so that short circuit between device leads is easily caused; 2. electrostatic discharge damage to damage the device and prevent it from working; 3. the heat generated by the electrostatic discharge field or current damages the device; 4. the electrostatic discharge amplitude is very large, and the electronic product is damaged by electromagnetic interference due to an electromagnetic field with extremely wide frequency spectrum (from dozens of mega to thousands of mega, and hundreds of volts per meter); 5. the products damaged by electrostatic discharge are reworked and repaired, the production cost is increased, and the economic benefit of enterprises is influenced. In summary, electrostatic hazards exist throughout the production of electronic products.
Heretofore, in order to suppress the above-mentioned damage of static electricity, in the production process of a pressure-sensitive adhesive for protective films, improvement has been mainly made by:
1. mainly by adding low molecular weight surfactants (for example, refer to Japanese patent laid-open No. 9-165460) or ionic antistatic agents (for example, refer to Chinese patent CN1727426B, CN 100351294C). However, in this method, the added low-molecular surfactant or ionic antistatic agent is likely to precipitate from the polymer and aggregate on the surface of the adhesive, and when applied to a protective film for optical parts, there is a risk of damaging the optical characteristics of the optical member.
2. Adhesives prepared by using monomers having an alkenyloxy group of (meth) acrylic acid (for example, see chinese patent CN 1749344B). However, in this method, the (meth) acrylic acid alkenyloxy monomer used has no ionic group, and the antistatic property is generally improved by adding an ion-containing antistatic agent, but the same problem as described in 1 is present after adding an ionic antistatic agent.
The acrylic ester polymer for the antistatic pressure-sensitive adhesive and the preparation method thereof, which can effectively solve the contradiction between the reverse static elimination and the influence of the precipitation of low molecular weight substances on optical equipment, are needed to solve the technical problems.
Disclosure of Invention
In order to solve the technical problems, the invention provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof. The acrylate polymer for the antistatic pressure-sensitive adhesive can effectively solve the contradiction between static removal and the influence of low molecular weight substance separation on optical equipment, and has the advantages of simple method and easy popularization and use.
The invention solves the technical problems by the following technical scheme:
the invention provides an acrylate polymer for an antistatic pressure-sensitive adhesive, which comprises a polymer, a solvent and an initiator; the polymer comprises a first unit containing an acrylate monomer, a second unit containing an alkenyloxy group and an ionic group and containing a double-bond polymerizable functional monomer, and a third unit containing a hydroxyl or carboxyl vinyl functional monomer, wherein the first unit accounts for 70-95% of the total weight of the polymer, the second unit accounts for 3-25% of the total weight of the polymer, and the third unit accounts for 1-7% of the total weight of the polymer; the weight percentage of the initiator, the polymer and the solvent is 0.0019-1.0021: 1: 1.00 to 1.60.
In the present invention, the first unit is a polymer containing an acrylate monomer, which is conventional in the art;
preferably, the first unit is selected from alkyl acrylates having an alkyl group containing 4 to 12 carbon atoms;
more preferably, the first unit is one or more of butyl acrylate, hexyl acrylate, isooctyl acrylate, n-octyl acrylate, 2-ethylhexyl acrylate, isononyl acrylate, and decyl acrylate.
In the invention, the glass transition temperature of the subsequent pressure-sensitive adhesive can be changed by adjusting the type and the content of the first unit;
preferably, the glass transition temperature of the first unit is lower than 0 ℃;
preferably, the weight percentage of the first unit in the polymer is 70-90%;
more preferably, the weight percentage of the first unit in the polymer is 80-90%;
even more preferably, the weight percentage of the first unit to the polymer is 85%.
In the invention, the second unit is a polymerizable functional monomer containing an alkenyloxy group and an ionic group and double bonds, and has high hydrophilic characteristics;
preferably, the second unit contains an ethoxy group with 5-20 repeating units, wherein the ionic group comprises an ammonia ion or a sodium ion;
preferably, the second unit is one or more of REASAOP SR-10, REASAOP SR-10(S), REASAOP SR-20(S) and KH-10 of DSK company of ADEKA company of Japan, and the raw materials are selected to ensure that the end product has excellent static conductive performance.
In the invention, the content of the second unit mainly determines the antistatic performance and compatibility of the product;
preferably, the second unit accounts for 5 to 15 percent of the weight of the polymer;
more preferably, the second unit accounts for 5 to 12 percent of the weight of the polymer;
even more preferably, the second unit is 10% by weight of the polymer; the applicant found that increasing the content of the second unit can increase the antistatic property of the pressure sensitive adhesive, but as the content of the second unit increases, the compatibility of the product becomes poor and polymerization becomes difficult, finally determining the weight percentage of the second unit of the present application.
In the invention, the third unit mainly has the function of increasing the glass transition temperature of the pressure-sensitive adhesive, and simultaneously, the viscosity of the pressure-sensitive adhesive is also reduced along with the excessive addition of the substances;
preferably, in the third unit, the hydroxyl-containing vinyl functional monomer is one or more of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate; in the third unit, the vinyl functional monomer containing carboxyl is acrylic acid or methacrylic acid.
In the invention, the contradiction between the glass transition temperature and the viscosity of the product is solved by adjusting the type and the content of the third unit;
preferably, the third unit accounts for 2 to 6 percent of the weight of the polymer;
more preferably, the third unit accounts for 3 to 5 weight percent of the polymer;
even more preferably, the third unit is 5% by weight of the polymer.
In the present invention, the glass transition temperature of the polymer is less than 0 ℃;
preferably, the glass transition temperature of the polymer is-10 ℃;
more preferably, the glass transition temperature of the polymer is-20 ℃.
In the present invention, the initiator is conventional in the art;
preferably, the initiator is azobisisobutyronitrile;
in the present invention, the solvent is conventional in the art;
preferably, the solvent is one or more of ethyl acetate, toluene and methanol.
In the invention, the weight ratio of the polymer, the solvent and the initiator is finally determined by a great deal of experimental research of the applicant, and the contradiction between the static charge removal and the influence of the precipitation of low molecular weight substances on optical equipment is finally and effectively solved through the adjustment of the proportion;
preferably, the weight percentages of the initiator, the polymer and the solvent are 0.002: 1: 1.5.
the invention also provides a preparation method of the acrylate polymer for the antistatic pressure-sensitive adhesive, which comprises the following steps: mixing the components according to the weight percentage, adding nitrogen to deactivate, and heating in water bath for 24 hours at 65 ℃.
The invention also provides a method for preparing the polymer solution from the acrylate polymer for the antistatic pressure-sensitive adhesive, which comprises the following steps: in glue, according to the cross-linking agent: polymer 0.002: 1, adding the cross-linking agent and the polymer, and stirring.
Wherein the cross-linking agent is conventional in the field;
preferably, the cross-linking agent is aluminum acetylacetonate.
The invention has the advantages and beneficial effects that: the acrylate polymer for the antistatic pressure-sensitive adhesive can effectively eliminate the problems of the conventional pressure-sensitive adhesive for the antistatic protective film, and prevent the irreversible damage to the attached optical equipment and electronic components when the protective film which is not subjected to antistatic treatment or cannot reach the limited electrostatic discharge performance is peeled off; the preparation method of the product is simple and easy to popularize and use.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The following examples and comparative examples used the following sources of raw materials:
butyl acrylate is purchased from shanghai friendship acrylate limited, abbreviated BA;
isooctyl acrylate is available from Shanghai friendship acrylate, Inc., abbreviated as 2-EHA;
acrylic acid is available from Shanghai friendship acrylate, Inc., abbreviated as GAA;
ethoxyethoxyethyl acrylate (trade name vicsat 190#) available from osaka organic chemistry, abbreviated EEEA;
ADEKA SR-10 is available from Adeka chemistry, abbreviated SR-10;
azobisisobutyronitrile is available from four-dimensional chemistry, abbreviated as AIBN;
ethyl acetate was purchased from Jiangsu Sopp, Inc. and abbreviated as EtOAc;
toluene purchased from china petrochemical, abbreviated as TOL;
methanol was purchased from chinese national reagent, abbreviated MeOH;
aluminum acetylacetonate is available from Nippon Chemicals and is abbreviated AlAA.
Example 1
The embodiment provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof, and the method comprises the following steps: in a glass bottle, 60g of BA, 25g of 2EHA, 5g of GAA, 10g of SR-10, 90g of ethyl acetate, 50g of toluene, 10g of methanol, and 0.2g of AIBN were mixed. Wherein the specific gravity of the reaction monomer BA/2EHA/GAA/SR-10 is 60/25/5/10. The bottle was inertized with nitrogen, sealed and stirred in a water bath at 65 ℃ for 24 hours.
Example 2
The embodiment provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof, and the method comprises the following steps: in a glass bottle, 60g of BA, 30g of 2EHA, 5g of GAA, 5g of SR-10, 90g of ethyl acetate, 50g of toluene, 10g of methanol and 0.2g of AIBN were mixed. Wherein the specific gravity of the reaction monomer BA/2EHA/GAA/SR-10 is 60/30/5/5. The bottle was inertized with nitrogen, sealed and stirred in a water bath at 65 ℃ for 24 hours.
Example 3
The embodiment provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof, and the method comprises the following steps: in a glass bottle, 60g of BA, 20g of 2EHA, 5g of GAA, 15g of SR-10, 90g of ethyl acetate, 50g of toluene, 10g of methanol and 0.2g of AIBN were mixed. Wherein the specific gravity of the reaction monomer BA/2EHA/GAA/SR-10 is 60/20/5/15. The bottle was inertized with nitrogen, sealed and stirred in a water bath at 65 ℃ for 24 hours.
Example 4
The embodiment provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof, and the method comprises the following steps: in a glass bottle, 60g of BA, 15g of 2EHA, 5g of GAA, 20g of SR-10, 90g of ethyl acetate, 50g of toluene, 10g of methanol and 0.2g of AIBN were mixed. Wherein the specific gravity of the reaction monomer BA/2EHA/GAA/SR-10 is 60/15/5/20. The bottle was inertized with nitrogen, sealed and stirred in a water bath at 65 ℃ for 24 hours.
Comparative example 1
The comparative example provides an acrylate polymer for an antistatic pressure-sensitive adhesive and a preparation method thereof, and the method comprises the following steps: in a glass bottle, 60g of BA, 35g of 2EHA, 5g of GAA, 0g of SR-10, 90g of ethyl acetate, 50g of toluene, 10g of methanol and 0.2g of AIBN were mixed. Wherein the specific gravity of the reaction monomer BA/2EHA/GAA/SR-10 is 60/35/5/0. The bottle was inertized with nitrogen, sealed and stirred in a water bath at 65 ℃ for 24 hours.
After cooling, the products of examples 1 to 4 and comparative example 1 were respectively taken out to test the unit conversion rate and the relative viscosity, wherein the monomer conversion rate was calculated according to the actual solid content/theoretical solid content, and the results are shown in table 1 below:
TABLE 1 specific conversion and relative viscosity for examples 1-4 and comparative example 1
Specific conversion (%) Relative viscosity (I.V)
Example 1 98.7 0.79
Example 2 99.0 0.82
Example 3 98.5 0.74
Example 4 98.2 0.70
Comparative example 1 99.1 0.84
Adding acetylacetone aluminum to the products of examples 1 to 4 and comparative example 1 according to an effective component ratio of a cross-linking agent/polymer of 0.2%, fully stirring, respectively coating polymer solutions on a PET substrate, and measuring surface resistance; the simple surface resistance tester is provided with a special grounding wire, a banana plug of the grounding wire is inserted into a grounding hole on the surface of the tester, an alligator clip at the other end is clamped on the grounding bus, the surface resistance tester is flatly pressed on the anti-static table pad, and the grounding resistance of the table pad can be tested. The surface resistance tester is provided with two connecting wires and two testing electrodes with the weight of 2Kg, is suitable for testing plane materials, can distinguish the tested materials into conductors, static dissipation and insulation through testing results, can test the surface resistance and the volume resistance (or system resistance) of the materials, connects the tester and the two testing electrodes by the two connecting wires, can test the surface resistance by placing the two electrodes on the same surface of the materials, and can test the volume resistance by placing the two electrodes at the opposite positions of the two surfaces of the materials. The tester with the model BM80/2 can directly use a megohmmeter and two connecting wires to test the grounding resistance and the low resistance; the test results are shown in table 2 below:
TABLE 2 surface resistance and appearance of Polymer solutions of the products of examples 1-4 and comparative example 1
Appearance of Polymer Surface resistance (omega)
Example 1 Is transparent 8.3*108
Example 2 Is transparent 2.6*109
Example 3 Slight turbidity 1.5*108
Example 4 Turbidity 7.2*107
Comparative example 1 Is transparent 5.1*1014
From these data, it can be concluded that the above acrylate pressure-sensitive adhesives containing an alkyleneoxy group and an ionic group and a double bond polymerizable functional monomer have good antistatic properties. The polymerizable functional monomer having an alkenyloxy group and an ionic group and containing a double bond is not preferably more than 20%, or tends to cause phase separation and migration to the surface of an adherend to cause a phenomenon of "ghost image".
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The acrylate polymer for the antistatic pressure-sensitive adhesive is characterized by comprising a polymer, a solvent and an initiator; the polymer comprises a first unit containing an acrylate monomer, a second unit containing an alkenyloxy group and an ionic group and containing a double-bond polymerizable functional monomer, and a third unit containing a hydroxyl or carboxyl vinyl functional monomer, wherein the first unit accounts for 70-95% of the total weight of the polymer, the second unit accounts for 3-25% of the total weight of the polymer, and the third unit accounts for 1-7% of the total weight of the polymer; the weight percentage of the initiator, the polymer and the solvent is 0.0019-1.0021: 1: 1.00 to 1.60.
2. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 1, wherein the first unit is selected from the group consisting of alkyl acrylates having an alkyl group containing 4 to 12 carbon atoms;
and/or the second unit contains an ethoxy group with 5-20 repeating units, wherein the ionic group comprises an ammonia ion or a sodium ion;
and/or in the third unit, the hydroxyl-containing vinyl functional monomer is one or more of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate; in the third unit, the vinyl functional monomer containing carboxyl is acrylic acid or methacrylic acid.
3. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 2, wherein the first unit is one or more of butyl acrylate, hexyl acrylate, isooctyl acrylate, n-octyl acrylate, 2-ethylhexyl acrylate, isononyl acrylate and decyl acrylate;
and/or the second unit is one or more of REASAOP SR-10, REASAOP SR-10(S), REASAOP SR-20(S) of ADEKA company of Japan and KH-10 of DSK company.
4. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 1, wherein the first unit accounts for 70 to 90% by weight of the polymer;
and/or the second unit accounts for 5-15% of the weight of the polymer;
and/or the third unit accounts for 2-6% of the weight of the polymer.
5. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 4, wherein the first unit accounts for 80 to 90% by weight of the polymer;
and/or the second unit accounts for 5-12% of the weight of the polymer;
and/or the third unit accounts for 3-5% of the weight of the polymer.
6. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 5, wherein the first unit is 85% by weight of the polymer;
and/or the second unit accounts for 10% of the weight of the polymer;
and/or the third unit accounts for 5% of the weight of the polymer.
7. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 1, wherein the initiator is azobisisobutyronitrile;
and/or the solvent is one or more of ethyl acetate, toluene and methanol.
8. The acrylate polymer for antistatic pressure-sensitive adhesive according to claim 1, wherein the weight percentage of the initiator, the polymer and the solvent is 0.002: 1: 1.5.
9. the method for preparing the acrylate polymer for the antistatic pressure-sensitive adhesive according to any one of claims 1 to 8, wherein the method comprises the steps of: mixing the components according to the weight percentage, adding nitrogen to deactivate, and heating in water bath for 24 hours at 65 ℃.
10. A polymer solution prepared from the acrylate polymer for the antistatic pressure-sensitive adhesive according to any one of claims 1 to 8, comprising the following steps:
in glue, according to the cross-linking agent: polymer 0.002: 1, adding a cross-linking agent and a polymer, and stirring; wherein the cross-linking agent is aluminum acetylacetonate.
CN202210253912.4A 2022-03-15 2022-03-15 Acrylate polymer for antistatic pressure-sensitive adhesive and preparation method thereof Pending CN114573747A (en)

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Application publication date: 20220603