CN110791204A - Single-component UV viscosity-reducing acrylate pressure-sensitive adhesive and preparation method thereof - Google Patents
Single-component UV viscosity-reducing 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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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
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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
- C09J2301/30—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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- 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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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Abstract
The invention discloses a single-component UV visbreaking acrylate pressure-sensitive adhesive composition and a preparation method thereof, wherein the composition is formed by fully mixing and reacting five components of 45-60% of solid content solvent type acrylate resin, dipentaerythritol hexaacrylate, an ultraviolet light initiator, an isocyanate latent curing agent and a polyurethane catalyst according to a certain weight part, and then diluting the mixture to 45-60% of solid content by using an organic solvent, wherein the 45-60% of solid content solvent type acrylate resin is formed by hydroxypropyl acrylate, hydroxyethyl acrylate, acrylic acid, methyl methacrylate, 2-ethylhexyl acrylate, α -cyanoacrylate, glycidyl acrylate and ethylene glycol dimethacrylate according to a certain proportion.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a single-component UV visbreaking acrylate pressure-sensitive adhesive and a preparation method thereof.
Background
Acrylate copolymers obtained by copolymerization of various acrylate monomers are an important class of resinous pressure-sensitive adhesives, and have many advantages: the appearance is colorless and transparent and has good weather resistance; the formula is simple; the pressure-sensitive adhesive meeting various performance requirements can be prepared by utilizing copolymerization and crosslinking, and can be applied to protective adhesive tapes. It is suitable for the manufacture and processing of chip, monocrystalline silicon, semiconductor and optical instrument. The initial adhesion and the holding adhesion of the pressure-sensitive adhesive are required to be good in the using process, but the final stripping force is low. The UV visbreaking pressure-sensitive adhesive is produced by the way, the initial adhesion and the sustained adhesion are the same as the common acrylic pressure-sensitive adhesive, the DPHA is promoted to be instantly polymerized by UV irradiation when the UV initiator is used, a dense cross-linked network is formed, the stripping force of the pressure-sensitive adhesive is greatly reduced, and the pressure-sensitive adhesive is easy to strip.
Patent application documents of publication numbers CN 105778806a and CN 106995665a respectively provide a heat-resistant UV pressure-sensitive adhesive and a composition of the corresponding UV pressure-sensitive adhesive, and the claims refer to solvent-based high-temperature-resistant polyacrylate pressure-sensitive adhesive, and the fact that the high-temperature-resistant polyacrylate pressure-sensitive adhesive does not exist, and the curing agent is used for curing on the basis of the common pressure-sensitive adhesive to achieve a certain temperature-resistant effect. As described in "development of pressure-sensitive adhesive tape with high temperature resistance" of Li Zhou et al, bonding 2005, 26(5), the pressure-sensitive adhesive has high temperature resistance after being thermally cured; in the Chinese adhesive Vol.15No.12, Dec.2006 of the research on the high-temperature resistant solvent type acrylate pressure-sensitive adhesive for the protective film of the sensitivity and the like, the high-temperature resistance of the acrylate pressure-sensitive adhesive can be realized only by adding a curing agent. The above two patents do not meet the objective facts of directly using solvent type high temperature resistant polyacrylate pressure sensitive adhesive.
The patent publication No. CN105086730A discloses a two-component UV tack-reducing pressure sensitive adhesive. The double-component curing UV visbreaking pressure-sensitive adhesive provided by the scheme is relatively complex in storage, transportation and use.
Therefore, the problem to be solved in the field is to provide a pressure-sensitive adhesive scheme with excellent performance and strong operability.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the single-component UV viscosity-reducing acrylate pressure-sensitive adhesive which has the advantages of initial adhesion, good permanent adhesion, low final stripping force, easiness in preparation, easiness in obtaining and diluting of raw materials, good process controllability and stable product quality.
The composition comprises the following components in parts by weight:
70-80 parts of solvent type acrylate resin with the solid content of 45% -60%;
10-20 parts of dipentaerythritol hexaacrylate;
1-2 parts of an ultraviolet initiator;
1-2 parts of a latent isocyanate curing agent;
the mass of the polyurethane catalyst is 1 percent of that of the substance D;
and fully mixing the components, and diluting the mixture to 45 to 60 percent of solid content by using an organic solvent to obtain the single-component UV viscosity-reducing acrylate pressure-sensitive adhesive.
Further, the solid part in the solvent type acrylate resin with the solid content of 45% -60% consists of the following components in parts by weight:
20-25 parts of hydroxypropyl acrylate;
5-7 parts of hydroxyethyl acrylate;
4-6 parts of acrylic acid;
12-18 parts of methyl methacrylate;
40-45 parts of 2-ethylhexyl acrylate;
α -6-9 parts of cyanoacrylate;
0.3-0.5 part of glycidyl acrylate;
0.5-0.8 part of ethylene glycol dimethacrylate;
further, the ultraviolet light initiator consists of two solid photoinitiators, wherein the mass ratio of bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide to 2-benzyl-2-methylamino-1- (4-morpholinylphenyl) butanone is 4/6.
Further, the isocyanate latent curing agent is HDI biuret blocked by polyisocyanate derivative ketoxime with the deblocking temperature of 85-130 ℃.
Furthermore, the polyurethane catalyst is organic bismuth catalyst bismuth acetate, and the deblocking temperature of the substance E can be effectively reduced.
The invention also provides a corresponding preparation method for the single-component UV visbreaking acrylate pressure-sensitive adhesive composition which is prepared from the components according to the corresponding proportion. The preparation method comprises the following steps:
dissolving hydroxypropyl acrylate, hydroxyethyl acrylate, acrylic acid, methyl methacrylate, 2-ethylhexyl acrylate, α -cyanoacrylate, glycidyl acrylate and ethylene glycol dimethacrylate in an organic solvent according to a certain proportion, wherein the water content of the organic solvent is less than 300 ppm.
The first step is as follows: and (3) putting 1/4-1/2 with the mass of the dissolved solution into a reaction kettle, continuously stirring, heating to 65-75 ℃ by using hot water, dropwise adding a certain amount of initiator solution, continuously heating to 50-70 ℃, and reacting for 0.8-2 h.
Wherein the amount of the added initiator is 50 percent of the total mass of the initiator, and the initiator is the initiator for free radical polymerization of acrylate monomers.
The second step is that: dropwise adding the rest solution, simultaneously dropwise adding a certain amount of initiator solution, continuously stirring in the dropwise adding process, keeping the reaction temperature of 50-70 ℃ as constant as possible, and completing dropwise adding within 2.5-3.5 h; and after the dropwise addition is finished, adding the rest initiator at one time, continuously reacting for 0.8-1.2 h at the temperature, slowly heating to 80-90 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Wherein, the initiator added for the first time in the second step accounts for 40 percent of the total mass of the initiator, and the initiator added for the second time accounts for 10 percent of the total mass of the initiator.
The third step: adding dipentaerythritol hexaacrylate, an ultraviolet light initiator, an isocyanate latent curing agent, a polyurethane catalyst and the rest solvent, fully stirring, continuously stirring for 30min after all the components are completely dissolved, and keeping the material temperature below 50 ℃ in the whole process.
The fourth step: discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
Wherein the discharging and filtering are carried out in a dark place or under yellow light, and the materials are packed by a metal barrel and stored in a sealed way.
The single-component UV visbreaking acrylic pressure-sensitive adhesive provided by the invention has the advantages of good initial adhesion and permanent adhesion, low final stripping force and the like.
The single-component UV visbreaking acrylic pressure-sensitive composition provided by the invention is easy to prepare, easily available in raw materials, easy to dilute, good in process controllability and stable in product quality.
The PET protective film prepared from the single-component UV visbreaking acrylic pressure-sensitive composition has lower peeling force, and can be widely applied to preparation of protective films for process protection and delivery protection of chips, monocrystalline silicon, semiconductors, optical instruments and equipment and the like.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the scheme of the embodiment, a certain amount of dipentaerythritol hexaacrylate, an ultraviolet light initiator, an isocyanate latent curing agent and a polyurethane catalyst are added to the synthesized solvent type acrylate pressure-sensitive adhesive for the first time to prepare the single-component UV visbreaking acrylic acid pressure-sensitive adhesive. The whole scheme is simple and easy to implement, raw materials are easy to obtain, the process controllability is good, and the product quality is stable.
Therefore, the scheme provides a single-component UV visbreaking acrylate pressure-sensitive adhesive composition scheme which specifically comprises the following components in parts by weight:
70-80 parts of solvent type acrylate resin with the solid content of 45% -60%;
10-20 parts of dipentaerythritol hexaacrylate;
1-2 parts of an ultraviolet initiator;
1-2 parts of a latent isocyanate curing agent;
the mass of the polyurethane catalyst is 1 percent of that of the substance D;
and fully mixing the components, and diluting the mixture to 45 to 60 percent of solid content by using an organic solvent to obtain the single-component UV viscosity-reducing acrylate pressure-sensitive adhesive.
Further, the solid part in the solvent type acrylate resin with the solid content of 45% -60% consists of the following components in parts by weight:
20-25 parts of hydroxypropyl acrylate;
5-7 parts of hydroxyethyl acrylate;
4-6 parts of acrylic acid;
12-18 parts of methyl methacrylate;
40-45 parts of 2-ethylhexyl acrylate;
α -6-9 parts of cyanoacrylate;
0.3-0.5 part of glycidyl acrylate;
0.5-0.8 part of ethylene glycol dimethacrylate;
further, the ultraviolet light initiator consists of two solid photoinitiators, wherein the mass ratio of bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide to 2-benzyl-2-methylamino-1- (4-morpholinylphenyl) butanone is 4/6.
Further, the isocyanate latent curing agent is HDI biuret blocked by polyisocyanate derivative ketoxime with the deblocking temperature of 85-130 ℃.
Furthermore, the polyurethane catalyst is organic bismuth catalyst bismuth acetate, and the deblocking temperature of the substance E can be effectively reduced.
Aiming at the scheme of the single-component UV visbreaking acrylate pressure-sensitive adhesive, the preparation method is further provided, and the preparation method specifically comprises the following steps:
dissolving hydroxypropyl acrylate, hydroxyethyl acrylate, acrylic acid, methyl methacrylate, 2-ethylhexyl acrylate, α -cyanoacrylate, glycidyl acrylate and ethylene glycol dimethacrylate in an organic solvent according to a certain proportion, wherein the water content of the organic solvent is less than 300 ppm.
The first step is as follows: and (3) putting 1/4-1/2 with the mass of the dissolved solution into a reaction kettle, continuously stirring, heating to 65-75 ℃ by using hot water, dropwise adding a certain amount of initiator solution, continuously heating to 50-70 ℃, and reacting for 0.8-2 h.
Wherein the amount of the added initiator is 50 percent of the total mass of the initiator, and the initiator is the initiator for free radical polymerization of acrylate monomers.
The second step is that: dropwise adding the rest solution, simultaneously dropwise adding a certain amount of initiator solution, continuously stirring in the dropwise adding process, keeping the reaction temperature of 50-70 ℃ as constant as possible, and completing dropwise adding within 2.5-3.5 h; and after the dropwise addition is finished, adding the rest initiator at one time, continuously reacting for 0.8-1.2 h at the temperature, slowly heating to 80-90 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Wherein, the initiator added for the first time in the second step accounts for 40 percent of the total mass of the initiator, and the initiator added for the second time accounts for 10 percent of the total mass of the initiator.
The third step: adding dipentaerythritol hexaacrylate, an ultraviolet light initiator, an isocyanate latent curing agent, a polyurethane catalyst and the rest solvent, fully stirring, continuously stirring for 30min after all the components are completely dissolved, and keeping the material temperature below 50 ℃ in the whole process.
The fourth step: discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
Wherein the discharging and filtering are carried out in a dark place or under yellow light, and the materials are packed by a metal barrel and stored in a sealed way.
According to the single-component UV viscosity-reducing acrylic pressure-sensitive adhesive formed based on the scheme, when the single-component UV viscosity-reducing acrylic pressure-sensitive adhesive is specifically applied, the single-component UV viscosity-reducing acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET (polyethylene terephthalate) film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through high-temperature baking, hydroxyl groups in acrylic resin react with a latent curing agent to be cured, a coated release film is wound, the coated release film is cured for 48 hours at 50 ℃, a UV viscosity-reducing protective adhesive tape can be manufactured, the peeling force of the adhesive tape can reach about 20N/25mm (measured by adhering to the surface of stainless steel), the peeling force of the adhesive surface is reduced to.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards. If there is no corresponding national standard, it is carried out according to the usual international standards, to the conventional conditions or to the conditions recommended by the manufacturer. Unless otherwise indicated, all parts are parts by weight, all percentages are percentages by weight, and the polymer molecular weight is the number average molecular weight.
Unless defined or stated 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. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention.
Example 1:
a) 200Kg of hydroxypropyl acrylate, 50Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 450Kg of 2-ethylhexyl acrylate, 90Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, and then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for standby.
b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of an organic solvent for later use.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 285.7Kg of dipentaerythritol hexaacrylate, 81911.44 Kg of UV initiator, 31917.16Kg of UV initiator, 1Kg of latent curing agent, 10g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 19N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.55N/25mm after the adhesive surface is irradiated by UV light.
Example 2:
a) 230Kg of hydroxypropyl acrylate, 70Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 430Kg of 2-ethylhexyl acrylate, 60Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, and then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for later use.
b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of an organic solvent for later use.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 400Kg of dipentaerythritol hexaacrylate, 81916 Kg of UV initiator, 31924 Kg of UV initiator, 1.5Kg of latent curing agent, 15g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 20N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.5N/25mm after the adhesive surface is irradiated by UV light.
Example 3:
a) 200Kg of hydroxypropyl acrylate, 50Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 450Kg of 2-ethylhexyl acrylate, 90Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, and then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for standby.
b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of an organic solvent for later use.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 500Kg of dipentaerythritol hexaacrylate, 81920 Kg of UV initiator, 31930 Kg of UV initiator, 2Kg of latent curing agent, 20g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 22N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.4N/25mm after the adhesive surface is irradiated by UV light.
Example 4:
a) 200Kg of hydroxypropyl acrylate, 50Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 450Kg of 2-ethylhexyl acrylate, 90Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, and then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for standby.
b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of an organic solvent for later use.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 400Kg of dipentaerythritol hexaacrylate, 81916 Kg of UV initiator, 31924 Kg of UV initiator, 1.5Kg of latent curing agent, 15g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 18N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.51N/25mm after the adhesive surface is irradiated by UV light.
Example 5:
a) 230Kg of hydroxypropyl acrylate, 70Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 430Kg of 2-ethylhexyl acrylate, 60Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for standby, b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of organic solvent for standby.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 500Kg of dipentaerythritol hexaacrylate, 81920 Kg of UV initiator, 31930 Kg of UV initiator, 2Kg of latent curing agent, 20g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 21N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.48N/25mm after the adhesive surface is irradiated by UV light.
Example 6:
a) 200Kg of hydroxypropyl acrylate, 50Kg of hydroxyethyl acrylate, 50Kg of acrylic acid, 150Kg of methyl methacrylate, 450Kg of 2-ethylhexyl acrylate, 90Kg of α -cyanoacrylate, 4Kg of glycidyl acrylate and 6Kg of ethylene glycol dimethacrylate are added into an overhead tank, and then 800Kg of organic solvent (the water content is less than 300ppm) is added and fully stirred for standby.
b) 10Kg of azodiisobutyronitrile as an initiator is dissolved in 50Kg of an organic solvent for later use.
Adding 600Kg of the solution a) into a reaction kettle, continuously stirring, heating to 60 ℃ by using hot water, beginning to add 30Kg of the solution b), continuously heating to 72 ℃, and reacting at the temperature for 1 h.
Dropwise adding the rest 1200Kg of solution a, and simultaneously dropwise adding 20Kg of solution b), continuously stirring in the dropwise adding process, keeping the reaction temperature at 72 ℃ as constant as possible, and finishing the dropwise adding within 3 hours; and after the dropwise addition is finished, adding the remaining 10Kg of solution b) at one time, continuously reacting for one hour at the temperature, slowly heating to 85 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃.
Adding 285.7Kg of dipentaerythritol hexaacrylate, 81911.44 Kg of UV initiator, 31917.16Kg of UV initiator, 1Kg of latent curing agent, 10g of catalyst and 150Kg of organic solvent, stirring thoroughly, continuing to stir for 30min after all the components are completely dissolved, and keeping the temperature of the materials below 50 ℃ in the whole process.
Discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
The single-component UV visbreaking acrylic pressure-sensitive adhesive is coated on the surface of a corona-treated transparent PET film through a coating machine, the thickness of a dry film is about 30 micrometers, a solvent is volatilized through a high-temperature drying tunnel, hydroxyl in acrylic resin reacts with a latent curing agent to be cured, a coated release film is wound, the film is cured for 48 hours at 50 ℃, the UV visbreaking protective adhesive tape can be prepared, the stripping force is 23N/25mm (measured by adhering to the surface of stainless steel), and the stripping force is reduced to 0.54N/25mm after the adhesive surface is irradiated by UV light.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The single-component UV visbreaking acrylate pressure-sensitive adhesive is characterized by comprising the following components in parts by weight:
70-80 parts of solvent type acrylate resin with the solid content of 45% -60%;
10-20 parts of dipentaerythritol hexaacrylate;
1-2 parts of an ultraviolet initiator;
1-2 parts of a latent isocyanate curing agent;
the mass of the polyurethane catalyst is 1 percent of that of the substance D;
the components are fully mixed and diluted to 45 to 60 percent of solid content by an organic solvent.
2. The one-component UV vis-broken acrylate pressure sensitive adhesive of claim 1, wherein: the solvent type acrylate resin with the solid content of 45% -60% comprises the following components in parts by weight:
20-25 parts of hydroxypropyl acrylate;
5-7 parts of hydroxyethyl acrylate;
4-6 parts of acrylic acid;
12-18 parts of methyl methacrylate;
40-45 parts of 2-ethylhexyl acrylate;
α -6-9 parts of cyanoacrylate;
0.3-0.5 part of glycidyl acrylate;
0.5-0.8 part of ethylene glycol dimethacrylate.
3. The one-component UV vis-breaking acrylate pressure sensitive adhesive of claim 1, wherein the UV initiator consists of two solid photoinitiators.
4. The one-component UV visbreaking acrylate pressure sensitive adhesive according to claim 3, wherein the ultraviolet photoinitiator consists of bis (2,4, 6-trimethylbenzoyl) phenylphosphonium oxide and 2-benzyl-2-methylamino-1- (4-morpholinylphenyl) butanone A in a mass ratio of 4/6.
5. The one-component UV visbreaking acrylate pressure sensitive adhesive of claim 1, wherein the isocyanate latent curing agent is a polyisocyanate derivative having a deblocking temperature of 85 ℃ to 130 ℃.
6. The one-component UV visbreaking acrylate pressure sensitive adhesive of claim 1, wherein the polyurethane catalyst is an organic bismuth-based catalyst.
7. The preparation method of the single-component UV visbreaking acrylate pressure-sensitive adhesive is characterized by comprising the following steps:
the first step is as follows: putting part of 45-60% of solvent type acrylate resin with solid content into a reaction kettle, continuously stirring, heating to 50-70 ℃ by using hot water, dropwise adding a certain amount of initiator solution, continuously heating to 65-75 ℃, and reacting for 0.8-2 h;
the second step is that: dropwise adding the residual solvent type acrylate resin with the solid content of 45-60 percent, simultaneously dropwise adding a certain amount of initiator solution, continuously stirring in the dropwise adding process, keeping the reaction temperature of 50-70 ℃ as constant as possible, and completing dropwise adding within 2.5-3.5 h; after the dropwise addition is finished, adding the rest initiator at one time, continuously reacting for 0.8-1.2 h at the temperature, slowly heating to 80-90 ℃, reacting for 30min at the temperature, adding a terminator, and cooling to below 50 ℃;
the third step: adding dipentaerythritol hexaacrylate, an ultraviolet light initiator, an isocyanate latent curing agent, a polyurethane catalyst and the rest solvent, fully stirring, continuously stirring for 30min after all the components are completely dissolved, and keeping the material temperature below 50 ℃ in the whole process;
the fourth step: discharging, filtering and packaging to obtain the single-component UV visbreaking acrylic pressure-sensitive adhesive.
8. The method of claim 7, wherein in step one, 1/4-1/2 solvent-based acrylate resin is added at 45% -60% solids.
9. The preparation method according to claim 7, wherein the amount of the initiator added in the first step is 50% of the total mass of the initiator, the amount of the initiator added in the second step is 40% of the total mass of the initiator, the amount of the initiator added in the second step is 10% of the total mass of the initiator, and the initiator is an initiator for radical polymerization of acrylate monomers.
10. The method of claim 7, comprising the step of preparing a 45% to 60% solids solvent-borne acrylate resin comprising:
dissolving hydroxypropyl acrylate, hydroxyethyl acrylate, acrylic acid, methyl methacrylate, 2-ethylhexyl acrylate, α -cyanoacrylate, glycidyl acrylate and ethylene glycol dimethacrylate in an organic solvent according to a certain proportion, wherein the water content of the organic solvent is less than 300 ppm.
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