CN111533841B - High-adhesion high-temperature-resistant water-based alumite back adhesive resin and preparation method thereof - Google Patents
High-adhesion high-temperature-resistant water-based alumite back adhesive resin and preparation method thereof Download PDFInfo
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- 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
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- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- 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
- C09J133/18—Homopolymers or copolymers of nitriles
- C09J133/20—Homopolymers or copolymers of acrylonitrile
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Abstract
The invention relates to a high-adhesion high-temperature-resistant water-based alumite back adhesive resin and a preparation method thereof, wherein the water-based alumite back adhesive resin comprises the following components in percentage by mass: 20-30 parts of acrylonitrile, 25-35 parts of diethylaminoethyl methacrylate, 35-55 parts of hydroxypropyl acrylate, 4-8 parts of emulsifier, 15-24 parts of deionized water and 0.1-0.4 part of initiator, the characteristics of high vitrification temperature, cohesive force, solvent resistance, self-thickening property of hard monomers and stronger hydrophilicity, viscosity retention and peeling strength of hydroxypropyl acrylate are combined in a balanced manner, a pre-emulsification process is adopted, seed pre-emulsion is prepared firstly, then emulsion and initiator are heated and dripped to polymerize and crosslink micelle, the concentration of free radicals and branched chain products are increased, the dispersion, heat transfer and mass transfer properties of a system are ensured, the stability of the system is improved, the phenomena of implosion and gelation are reduced, the heat resistance stability and the adhesion and solidification properties of the waterborne alumite gum resin are improved, the hot stamping performance, viscosity retention and peeling strength of alumite are improved, and the range of applicable base materials is widened.
Description
Technical Field
The invention relates to a high-adhesion high-temperature-resistant water-based alumite back adhesive resin and a preparation method thereof, belonging to the technical field of water-based alumite back adhesive resins.
Background
The water-based alumite gum resin is suitable for thermoprinting plastic films such as PP, PVC, PET, acrylic, ABS, PC and the like, various products, UV printing ink gloss oil paper products with smooth surfaces, leather, synthetic leather and other base materials, has better thermoprinting effect compared with the traditional oil gum, and meets the environmental protection requirement of industries such as packaging, medicines, cosmetics and the like on organic solvent residue. The electro-aluminum hot stamping method has the advantages that the printing material and the hot stamping foil are pressed mutually in a short time by means of moving pressure and temperature during electro-aluminum hot stamping, the purpose of protecting the printing material or packaging identification by hot stamping is achieved, the water-based electro-aluminum gum and the base material of the printing material during hot stamping have a good bonding effect after being preheated, and the hot stamping effect is directly influenced. The waterborne alumite gum resin in the prior art is mainly prepared by taking acrylic resin as a main raw material and chemically modifying and blending additive resin, has poor heat-resistant stability and adhesive curing performance, and influences the hot stamping performance, the holding viscosity, the peel strength and the range of applicable base materials of alumite.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high-adhesion high-temperature-resistant water-based alumite gum resin and the preparation method thereof, so that the phenomena of implosion and gelation are reduced through full emulsification, the heat-resistant stability and the adhesion curing performance of the water-based alumite gum resin are improved, the hot stamping performance, the holding viscosity and the peeling strength of alumite are improved, and the range of applicable base materials is widened.
The invention is realized by the following technical scheme:
the high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the following components in percentage by mass: 20-30 parts of acrylonitrile, 25-35 parts of diethylaminoethyl methacrylate, 35-55 parts of hydroxypropyl acrylate, 4-8 parts of an emulsifier, 15-24 parts of deionized water and 0.1-0.4 part of an initiator;
the emulsifier is any one or mixture of more of alkylphenol polyoxyethylene, polyoxyethylene dodecyl phenyl ether, fatty alcohol polyoxyethylene polyoxypropylene ether and polyoxyethylene octyl phenol ether; the initiator is any one or mixture of sodium persulfate, potassium persulfate, nickel persulfate or ammonium bisulfite;
the mass fraction of the poster in the waterborne alumite back glue resin is 5-10 parts of curing agent, and the curing agent is the mixture of sodium silicate and any one or more of silicon dioxide, zinc oxide, metaborate and silicon nitride.
A preparation method of high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the following steps:
(1) adding 20-30 parts of acrylonitrile, 25-35 parts of diethylaminoethyl methacrylate, 35-55 parts of hydroxypropyl acrylate, 4-8 parts of an emulsifier and 9-16 parts of deionized water into a stirring kettle by mass percent, stirring and mixing for 30-60min at the speed of 200-250r/min, and emulsifying to form seed pre-emulsion;
(2) adding seed pre-emulsion accounting for 10% of the total weight of the seed pre-emulsion, deionized water with the mass fraction of 6-8 parts and an initiator with the mass fraction of 0.03-0.2 part into a polymerization kettle in a nitrogen atmosphere, heating to 60-75 ℃, keeping the temperature, carrying out reflux reaction for 30-40min, heating to 80-85 ℃, dropwise adding the rest of the seed pre-emulsion and the initiator with the mass fraction of 0.07-0.2 part, wherein the rest of the seed pre-emulsion and the initiator are slow and fast in time and are dropwise added for 1-2h, continuing the reaction for 2-2.5h, cooling to 40-45 ℃, carrying out heat preservation for 20-30min, and cooling to obtain the water-based alumite back adhesive resin.
The preparation method of the high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the step (2) of adding 5-10 parts by mass of a curing agent in the continuous reaction process, wherein the curing agent is a mixture of sodium silicate and any one or more of silicon dioxide, zinc oxide, metaborate and silicon nitride, and the stirring rate is 310-.
The invention has the beneficial effects that:
(1) hard monomer acrylonitrile, diethylaminoethyl methacrylate and functional group monomer hydroxypropyl acrylate are adopted as an emulsion polymerization crosslinking resin monomer, the characteristics of high glass transition temperature, cohesive force, solvent resistance, self-thickening property of the hard monomer and stronger hydrophilicity, viscosity and peel strength of the hydroxypropyl acrylate are combined in a balanced manner, and the nonionic emulsifier reduces the surface tension of the resin monomer in the seed pre-emulsion and improves the dispersing performance;
(2) the water-soluble persulfate or bisulfite is taken as an initiator to diffuse into the polymeric micelle or emulsified particles to initiate the growth of polymeric molecular chains, and the adhesive property of the curing system to the surfaces of metal, leather and ceramic substrates is improved through ionic bonds, so that the heat-resistant stability and the adhesive curing property of the cross-linked water-based alumite back adhesive resin are improved, the hot stamping property, the holding property and the peeling strength of the alumite are improved, and the range of applicable substrates is widened;
(3) the method adopts a pre-emulsification process, firstly prepares a seed pre-emulsion, then increases the temperature to dropwise add the emulsion and an initiator to polymerize and crosslink micelles, avoids emulsion layering, increases the concentration of free radicals and branched chain products, is easier to crosslink and improves the conversion rate under the conditions of proper temperature, stirring speed and reaction time, ensures the dispersion, heat transfer and mass transfer performance of a system, improves the stability of the system, fully emulsifies, reduces the phenomena of implosion and gelation, and improves the bonding stability.
Detailed Description
The following examples further illustrate embodiments of the present invention.
Example 1:
a preparation method of high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the following steps:
(1) adding 25 parts of acrylonitrile, 34 parts of diethylaminoethyl methacrylate, 43 parts of hydroxypropyl acrylate, 5 parts of an emulsifier and 11 parts of deionized water into a stirring kettle according to mass fraction, wherein the emulsifier is composed of alkylphenol polyoxyethylene and polyoxyethylene dodecyl phenyl ether according to a mass ratio of 1:1, stirring and mixing for 40min at 230r/min, and emulsifying to obtain a seed pre-emulsion;
(2) under the nitrogen atmosphere, adding seed pre-emulsion accounting for 10% of the total weight of the seed pre-emulsion, deionized water with the mass fraction of 7 parts and an initiator with the mass fraction of 0.08 part into a polymerization kettle, heating to 65 ℃, keeping the temperature constant, and carrying out reflux reaction for 35 min;
heating to 82 ℃, and dropwise adding the rest seed pre-emulsion and 0.1 part of initiator by mass, wherein the initiator is sodium persulfate and nickel persulfate according to the mass ratio of 1:1, the speed of the rest seed pre-emulsion and the initiator is slow firstly and then fast, the dripping time is 2 hours, the stirring speed is 350r/min, the reaction is continued for 2.2 hours, the temperature is reduced to 42 ℃, the temperature is kept for 25 minutes, and the water-based alumite back adhesive resin is obtained after cooling.
Example 2:
a preparation method of high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the following steps:
(1) adding 21 parts of acrylonitrile, 24 parts of diethylaminoethyl methacrylate, 52 parts of hydroxypropyl acrylate, 6 parts of an emulsifier and 10 parts of deionized water into a stirring kettle according to mass fraction, stirring and mixing the emulsifier which is fatty alcohol polyoxyethylene polyoxypropylene ether at 240r/min for 50min, and emulsifying to obtain a seed pre-emulsion;
(2) under the nitrogen atmosphere, adding seed pre-emulsion accounting for 10% of the total weight of the seed pre-emulsion, deionized water with the mass fraction of 6 parts and an initiator with the mass fraction of 0.04 part into a polymerization kettle, heating to 70 ℃, keeping the temperature, and carrying out reflux reaction for 40min, wherein the initiator consists of potassium persulfate and ammonium bisulfite with the mass ratio of 1: 1;
heating to 83 ℃, dropwise adding the rest of seed pre-emulsion and 0.15 part of initiator by mass, wherein the rest of seed pre-emulsion and initiator are slow and fast, the dropwise adding time is 1.5h, and 8 parts of curing agent by mass is added, and the curing agent is sodium silicate, silicon dioxide and metaborate according to the mass ratio of 2:1:1, the stirring speed is 330r/min during the continuous reaction, the reaction is continued for 2h, the temperature is reduced to 45 ℃, the temperature is kept for 30min, and the water-based alumite back adhesive resin is obtained after cooling.
Example 3:
a preparation method of high-adhesion high-temperature-resistant water-based alumite back adhesive resin comprises the following steps:
(1) adding 29 parts of acrylonitrile, 27 parts of diethylaminoethyl methacrylate, 38 parts of hydroxypropyl acrylate, 4 parts of an emulsifier and 13 parts of deionized water into a stirring kettle according to mass fraction, wherein the emulsifier is composed of polyoxyethylene dodecyl phenyl ether and polyoxyethylene octyl phenol ether according to a mass ratio of 1:1, stirring and mixing for 30min at 210r/min, and emulsifying to form a seed pre-emulsion;
(2) under the nitrogen atmosphere, adding seed pre-emulsion accounting for 10% of the total weight of the seed pre-emulsion, deionized water with the mass fraction of 6 parts and an initiator with the mass fraction of 0.06 part into a polymerization kettle, heating to 65 ℃, keeping the temperature, and carrying out reflux reaction for 35min, wherein the initiator is composed of sodium persulfate, potassium persulfate and ammonium bisulfite with the mass ratio of 1:1: 2;
heating to 85 ℃, dropwise adding the rest of seed pre-emulsion and 0.12 part of initiator by mass, wherein the rest of seed pre-emulsion and initiator are slow first and then fast, the dropwise adding time is 2h, adding 8 parts of curing agent by mass, the curing agent is composed of sodium silicate, zinc oxide and silicon nitride according to the mass ratio of 2:1:1, stirring at the speed of 360r/min during continuous reaction, continuing the reaction for 2h, cooling to 40 ℃, preserving the heat for 20min, and cooling to obtain the waterborne alumite back adhesive resin.
The mechanism of the invention is as follows:
hard monomer acrylonitrile, diethylaminoethyl methacrylate and functional group monomer hydroxypropyl acrylate are adopted as an emulsion polymerization crosslinking resin monomer, the molecular chain polarity is increased through polymerization, the characteristics of higher vitrification temperature of acrylonitrile and diethylaminoethyl methacrylate, improvement of mutual attraction cohesive force, solvent resistance and self-thickening property of the water-based gum between adjacent parts in the same substance are combined in a balanced manner, the characteristics of stronger hydrophilicity, viscosity retention and peeling strength are endowed to the water-based gum through the acrylonitrile and the diethylaminoethyl methacrylate, the wettability and the adhesive force to a hot stamping base material are improved, a good bonding effect is realized after preheating, an emulsion is synthesized, the phenomenon of polymerization explosion caused by overlarge viscosity of a polymer emulsion is avoided, the heat-resistant stability and the adhesive curing performance of the crosslinking resin are improved, the hot stamping performance, the viscosity retention, the peeling strength and the range of applicable base materials are improved;
the low cloud point nonionic emulsifiers such as alkylphenol ethoxylates, polyoxyethylene dodecyl phenyl ether, polyoxyethylene polyoxypropylene ether polyoxyethylene octyl phenol ether and the like are adopted, are easily soluble in polar solvents, have good emulsifying, wetting, dispersing and solubilizing properties on the seed pre-emulsion, can reduce the surface tension of resin monomers in the seed pre-emulsion, reduce coacervate during polymerization to improve the dispersing performance, increase the dispersing performance of the resin monomers in a water phase and the solubilization of formed micelles, and improve the chemical stability;
the water-soluble persulfate or hydrosulfite which is any one or a mixture of more of sodium persulfate, potassium persulfate, ammonium persulfate and ammonium bisulfite is adopted as an initiator to be heated and decomposed into a free radical compound which is used for diffusing into polymeric micelles or emulsified particles to initiate the growth of polymeric molecular chains, so that the uniformity of emulsion, the nucleation speed of monomers and the chain expansion rate are improved;
the inorganic adhesive curing system is formed by mixing sodium silicate and any one or more of silicon dioxide, zinc oxide, metaborate and silicon nitride, is compatible with acrylic waterborne adhesive resin for modification, improves the adhesive property on the surfaces of metal, leather and ceramic substrates through ionic bonds, reduces the thermal expansion coefficient and stress, avoids curing cracking, and improves the high-temperature resistant adhesive property and the substrate range;
the performance of the aqueous electrochemical aluminum back adhesive resin prepared in the embodiments 1-3 of the invention and the aqueous electrochemical aluminum back adhesive resin in the prior art are used as a control example for performance detection, and the detection results are as follows:
according to the invention, a novel formula and a pre-emulsification process are adopted, the seed pre-emulsion is prepared, then the emulsion and the initiator are heated and dripped to polymerize and crosslink the micelle, the emulsion dispersibility and the uniformity are improved, the emulsion is prevented from layering, the free radical concentration and the branched chain product are increased under the conditions of proper temperature, stirring speed and reaction time, the crosslinking is easier to occur, the conversion rate is improved, the dispersion, heat transfer and mass transfer performance of the system are ensured, the system stability is improved, the phenomena of implosion and gelation are reduced by full emulsification, and the adhesion stability is improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. The high-adhesion high-temperature-resistant water-based alumite back adhesive resin is characterized by comprising the following components in percentage by mass: 20-30 parts of acrylonitrile, 25-35 parts of diethylaminoethyl methacrylate, 35-55 parts of hydroxypropyl acrylate, 4-8 parts of an emulsifier, 15-24 parts of deionized water and 0.1-0.4 part of an initiator;
the preparation method comprises the following steps:
(1) adding 20-30 parts of acrylonitrile, 25-35 parts of diethylaminoethyl methacrylate, 35-55 parts of hydroxypropyl acrylate, 4-8 parts of an emulsifier and 9-16 parts of deionized water into a stirring kettle by mass percent, stirring and mixing for 30-60min at the speed of 200-250r/min, and emulsifying to form seed pre-emulsion;
(2) adding seed pre-emulsion accounting for 10% of the total weight of the seed pre-emulsion, deionized water with the mass fraction of 6-8 parts and an initiator with the mass fraction of 0.03-0.2 part into a polymerization kettle in a nitrogen atmosphere, heating to 60-75 ℃, keeping the temperature, carrying out reflux reaction for 30-40min, heating to 80-85 ℃, dropwise adding the rest of seed pre-emulsion and the initiator with the mass fraction of 0.07-0.2 part, continuing to react for 2-2.5h, cooling to 40-45 ℃, carrying out heat preservation for 20-30min, and cooling to obtain the waterborne alumite back adhesive resin.
2. The high-adhesion high-temperature-resistant water-based alumite back adhesive resin as claimed in claim 1, wherein the emulsifier is any one or more of alkylphenol ethoxylates, polyoxyethylene dodecylphenyl ether, fatty alcohol polyoxyethylene polyoxypropylene ether and polyoxyethylene octylphenol ether.
3. The high-adhesion high-temperature-resistant water-based alumite back adhesive resin as claimed in claim 1, wherein the initiator is one or more of sodium persulfate, potassium persulfate, nickel persulfate and ammonium bisulfite.
4. The high-adhesion high-temperature-resistant water-based alumite adhesive-backed resin as claimed in any one of claims 1 to 3, wherein the water-based alumite adhesive-backed resin comprises 5-10 parts by mass of a curing agent.
5. The high-adhesion high-temperature-resistant water-based alumite adhesive-backed resin as claimed in claim 4, wherein the curing agent is a mixture of sodium silicate and any one or more of silicon dioxide, zinc oxide, metaborate and silicon nitride.
6. The high-adhesion high-temperature-resistant water-based alumite back adhesive resin as claimed in claim 1, wherein the emulsifier is one or more selected from alkylphenol ethoxylates, polyoxyethylene dodecylphenyl ether, fatty alcohol polyoxyethylene polyoxypropylene ether and polyoxyethylene octylphenol ether, and the initiator is one or more selected from sodium persulfate, potassium persulfate, nickel persulfate and ammonium bisulfite.
7. The high-adhesion high-temperature-resistant water-based alumite back adhesive resin as claimed in claim 1, wherein the rate of the residual seed pre-emulsion and the initiator added in step (2) is slow and fast, and the adding time is 1-2 h.
8. The high-adhesion high-temperature-resistant water-based alumite adhesive-backed resin as claimed in any one of claims 1, 6 or 7, wherein 5-10 parts by mass of a curing agent is further added during the continuous reaction in step (2), the curing agent is a mixture of sodium silicate and any one or more of silicon dioxide, zinc oxide, metaborate and silicon nitride, and the stirring rate is 310-.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070082431A (en) * | 2006-02-16 | 2007-08-21 | 대진대학교 산학협력단 | Urethane acrylic water dispersed emulsion for leather recoating |
| CN102559104A (en) * | 2011-12-26 | 2012-07-11 | 北京高盟新材料股份有限公司 | Waterborne gravure printing aluminum-coated compound glue and preparation method thereof |
| CN106832104A (en) * | 2017-01-11 | 2017-06-13 | 无锡海特新材料研究院有限公司 | High temperature resistant aluminium foil polyacrylate pressure-sensitive emulsion and application thereof and preparation method |
| CN111087962A (en) * | 2019-12-26 | 2020-05-01 | 扬州市祥华新材料科技有限公司 | Preparation and method of aqueous back adhesive for alumite gold stamping foil |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070155927A1 (en) * | 2005-12-30 | 2007-07-05 | Cytec Surface Specialties Austria Gmbh | Paste resins for aqueous paints |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070082431A (en) * | 2006-02-16 | 2007-08-21 | 대진대학교 산학협력단 | Urethane acrylic water dispersed emulsion for leather recoating |
| CN102559104A (en) * | 2011-12-26 | 2012-07-11 | 北京高盟新材料股份有限公司 | Waterborne gravure printing aluminum-coated compound glue and preparation method thereof |
| CN106832104A (en) * | 2017-01-11 | 2017-06-13 | 无锡海特新材料研究院有限公司 | High temperature resistant aluminium foil polyacrylate pressure-sensitive emulsion and application thereof and preparation method |
| CN111087962A (en) * | 2019-12-26 | 2020-05-01 | 扬州市祥华新材料科技有限公司 | Preparation and method of aqueous back adhesive for alumite gold stamping foil |
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