CN112940201B - Water-based resin for elastic wave glue and preparation method thereof - Google Patents
Water-based resin for elastic wave glue and preparation method thereof Download PDFInfo
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- CN112940201B CN112940201B CN202110164647.8A CN202110164647A CN112940201B CN 112940201 B CN112940201 B CN 112940201B CN 202110164647 A CN202110164647 A CN 202110164647A CN 112940201 B CN112940201 B CN 112940201B
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention relates to the field of high polymer materials, and in particular relates to an aqueous resin for an elastic wave adhesive and a preparation method thereof. The preparation raw materials of the waterborne resin for the elastic wave glue comprise, by weight, 100 parts of epoxy resin, 50-70 parts of organic solvent, 12-20 parts of coupling agent, 0.5-1 part of initiator, 10-18 parts of acrylic comonomer, 6-10 parts of fumed silica and 0.2-0.5 part of hydroquinone. The aqueous resin for the elastic wave adhesive can be used alone or mixed with other resins to prepare the elastic wave adhesive, so that the prepared elastic wave adhesive has good high temperature resistance, excellent toughness and stability.
Description
Technical Field
The invention relates to the field of high polymer materials, and in particular relates to a water-based resin for an elastic wave adhesive and a preparation method thereof.
Background
The elastic wave glue is prepared from some resins, the elastic wave glue is prepared by coating on cloth and is one of important elements of a loudspeaker, and the loudspeaker generates heat when being used for a long time, so that the elastic wave glue resin needs to be prepared and has good high-temperature resistance.
Epoxy resins have excellent adhesion, mechanical strength, and corrosion resistance, but their heat resistance is not particularly desirable. The inorganic nano particles have the characteristics of surface effect, volume effect and the like, and when the inorganic nano particles are applied to epoxy resin, the bonding performance of the epoxy resin can be improved, and the high-temperature resistance of the epoxy resin can also be improved to a certain extent. However, although some coupling agents, inorganic nanoparticles and epoxy resins are generally used to react to obtain modified epoxy resins, the coupling agents can improve the compatibility of the inorganic nanoparticles and the epoxy resins, but the effect of improving the compatibility is not ideal, and thus the modification effect is affected.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides an aqueous resin for an elastomer, and the aqueous resin for the elastomer is prepared from the following raw materials, by weight, 100 parts of an epoxy resin, 50-70 parts of an organic solvent, 12-20 parts of a coupling agent, 0.5-1 part of an initiator, 10-18 parts of an acrylic comonomer, 6-10 parts of fumed silica and 0.2-0.5 part of hydroquinone.
In a preferred embodiment of the present invention, the epoxy resin includes a bisphenol a epoxy resin.
As a preferred embodiment of the present invention, the epoxy resin further includes butyl glycidyl ether.
As a preferable technical scheme of the invention, the organic solvent is an alcohol ether solvent or/and an alcohol solvent.
As a preferred technical scheme of the invention, the coupling agent is an aminosilane coupling agent.
In a preferred embodiment of the present invention, the aminosilane coupling agent is at least one selected from the group consisting of γ -aminopropyltriethoxysilane, γ -aminopropyltrimethoxysilane, N- β (aminoethyl) - γ -aminopropyltriethoxysilane, N- β (aminoethyl) - γ -aminopropylmethyldiethoxysilane, phenylaminomethyltriethoxysilane, phenylaminomethyltrimethoxysilane and aminoethylmethyltrimethoxysilane.
In a preferred embodiment of the present invention, the acrylic comonomer is at least one selected from the group consisting of methyl acrylate, N-butyl acrylate, 2-hydroxyethyl acrylate, glycidyl methacrylate, methyl methacrylate, butyl methacrylate, N-methylol acrylamide, and lauryl methacrylate.
In a preferred embodiment of the present invention, the fumed silica has an average particle size of 8 to 20 nm.
The second aspect of the invention provides a preparation method of an aqueous resin for an elastic wave glue, which comprises the following preparation steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; and then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 5-6h after the mixed solution B is dropwise added, and finally adding hydroquinone to react for 30-40min to obtain the water-based resin for the elastic wave glue.
In a preferred embodiment of the present invention, the reaction temperature in step S4 is 80 to 110 ℃.
The invention has the following beneficial effects:
1. the invention mainly modifies the epoxy resin, and keeps the good adhesive property of the epoxy resin;
2. according to the invention, the fumed silica is used for modifying the epoxy resin, and the fumed silica can be well dispersed in the system, so that the aqueous resin for the elastic wave glue has good high temperature resistance;
3. the aqueous resin for the elastic wave adhesive can be used independently or mixed with other resins to prepare the elastic wave adhesive, so that the prepared elastic wave adhesive has good high temperature resistance;
4. according to the invention, hydroquinone is used, so that raw materials which are not completely reacted in a system can be removed, and the performance of the aqueous resin for the elastic wave glue cannot be influenced due to the existence of other residual raw materials;
5. according to the invention, the modification of the epoxy resin by the fumed silica can be well realized by using the synergistic effect of the aminosilane coupling agent and the fumed silica;
6. the silicon-based group is grafted through the coupling agent, and the prepared aqueous resin for the elastic wave glue has excellent toughness and stability.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definition provided in the present disclosure, the definition of the term provided in the present disclosure controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present invention, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The first aspect of the invention provides an aqueous resin for an elastic wave adhesive, which is prepared from the following raw materials, by weight, 100 parts of an epoxy resin, 50-70 parts of an organic solvent, 12-20 parts of a coupling agent, 0.5-1 part of an initiator, 10-18 parts of an acrylic comonomer, 6-10 parts of fumed silica and 0.2-0.5 part of hydroquinone.
In a preferred embodiment, the raw materials for preparing the waterborne resin for the elastomer comprise, by weight, 100 parts of epoxy resin, 60 parts of organic solvent, 16 parts of coupling agent, 0.7 part of initiator, 15 parts of acrylic comonomer, 8 parts of fumed silica and 0.3 part of hydroquinone.
Epoxy resin
In one embodiment, the epoxy resin comprises a bisphenol a type epoxy resin.
In one embodiment, the bisphenol A type epoxy resin is composed of bisphenol A type epoxy resin-1 having an epoxy equivalent of 176-184g/eq and bisphenol A type epoxy resin-2 having an epoxy equivalent of 184-190 g/eq.
In one embodiment, the weight ratio of bisphenol a epoxy resin-1 to bisphenol a epoxy resin-2 is 1: (2-3); more preferably, the weight ratio of the bisphenol A epoxy resin-1 to the bisphenol A epoxy resin-2 is 1: 2.5.
in one embodiment, the bisphenol A type epoxy resin-1 is NPEL-127 of south Asia; the bisphenol A type epoxy resin-2 is NPEL-128 of south Asia.
In one embodiment, the epoxy resin further comprises butyl glycidyl ether.
In one embodiment, the butyl glycidyl ether has an epoxy equivalent weight of 145-155 g/eq.
In one embodiment, the weight of the butyl glycidyl ether is 10 to 15% of the weight of the epoxy resin; more preferably, the weight of the butyl glycidyl ether is 12% of the weight of the epoxy resin.
In one embodiment, the butyl glycidyl ether is HELOXY 61.
In the present invention, the applicant modified 176-184g/eq of bisphenol A epoxy resin-1, 184-190g/eq of bisphenol A epoxy resin-2, and butyl glycidyl ether by the modification method of the present invention.
Organic solvent
In one embodiment, the organic solvent is an alcohol ether solvent or/and an alcohol solvent.
In a preferred embodiment, the organic solvent is an alcohol ether solvent and an alcohol solvent; wherein the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: (1.5-2.2); further preferably, the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: 1.8.
in one embodiment, the alcohol ether solvent is at least one selected from the group consisting of ethylene glycol butyl ether, ethylene glycol ethyl ether, ethylene glycol methyl ether; further preferably, the alcohol ether solvent is ethylene glycol butyl ether.
In one embodiment, the alcoholic solvent is a vicinal diol; examples of the vicinal diols include ethylene glycol, 1, 2-propylene glycol, 1, 2-butylene glycol, 2, 3-butylene glycol, etc.; further preferably, the vicinal diol is 1, 2-propanediol.
The applicant invents that the weather resistance of the aqueous resin for the elasto-rubber can be well improved by using the o-glycol and the alcohol ether solvent in the system, and the surface of the aqueous resin for the elasto-rubber has good smoothness after being cured. Possibly, the gas-phase silicon dioxide is mutually synergistic in the o-glycol, the glycidyl methacrylate and the lauryl methacrylate, so that the gas-phase silicon dioxide can be well dispersed in a system, and the weather resistance of the ebonite is improved.
Coupling agent
In one embodiment, the coupling agent is an aminosilane coupling agent.
In one embodiment, the aminosilane coupling agent is selected from at least one of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, N-beta (aminoethyl) -gamma-aminopropyltriethoxysilane, N-beta (aminoethyl) -gamma-aminopropylmethyldiethoxysilane, phenylaminomethyltriethoxysilane, phenylaminomethyltrimethoxysilane, and aminoethylmethyltrimethoxysilane.
In a preferred embodiment, the coupling agent is N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane.
In one embodiment, the weight ratio of N- β (aminoethyl) - γ -aminopropyltrimethoxysilane to phenylaminomethyltrimethoxysilane is (2.4-3): 1; further preferably, the weight ratio of the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane to the phenylaminomethyltrimethoxysilane is 2.7: 1.
in one embodiment, the N- β (aminoethyl) - γ -aminopropyltrimethoxysilane is KBM-603.
In one embodiment, the phenylaminomethyltrimethoxysilane is nan Da-73.
The applicant finds that when N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane are used as coupling agents, the weather resistance of the waterborne resin for the elastic wave glue can be well improved. On the one hand, the possibility is that NHZ and Si- (O-CH3)3 in the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and the phenylaminomethyltrimethoxysilane can be grafted together by an epoxy group in the epoxy resin and a silicon hydroxyl group in the fumed silica to form a molecule with a relatively longer molecular chain, so that the compatibility of the fumed silica in the epoxy resin is increased.
Initiator
The initiator is not limited, and the initiators typically used for acrylic resins are all used in the present system. Examples of the initiator include azobisbutyronitrile, benzoyl peroxide, dibenzoyl peroxide, and ammonium persulfate.
In one embodiment, the initiator is benzoyl peroxide.
Acrylic comonomers
In one embodiment, the acrylic comonomer is selected from at least one of methyl acrylate, N-butyl acrylate, 2-hydroxyethyl acrylate, glycidyl methacrylate, methyl methacrylate, butyl methacrylate, N-methylol acrylamide, lauryl methacrylate.
In one embodiment, the acrylic comonomer is a mixture of glycidyl methacrylate (CAS number: 106-91-2) and lauryl methacrylate (CAS number: 142-90-5); wherein the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is (1.8-2.5): 1; further preferably, the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is 2.3: 1.
applicants have found that the use of glycidyl methacrylate in the system of the present invention to interact with lauryl methacrylate can increase the weatherability of waterborne resins for elastomerics. Probably because the glycidyl methacrylate has double functional groups, the glycidyl methacrylate has the double functional groups to be copolymerized with lauryl methacrylate, epoxy groups are contained in the glycidyl methacrylate and can react with amino groups, hydroxyl groups and other groups in the system, and the lauryl methacrylate has longer carbon chains and interacts with the glycidyl methacrylate to ensure that the system has higher crosslinking density.
Fumed silica
In one embodiment, the fumed silica has an average particle size of from 8 to 20 nm; further preferably, the fumed silica has an average particle size of 12 nm.
In one embodiment, the fumed silica is AEROSIL A200.
The second aspect of the invention provides a preparation method of an aqueous resin for an elastic wave glue, which comprises the following preparation steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; and then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 5-6h after the mixed solution B is dropwise added, and finally adding hydroquinone to react for 30-40min to obtain the water-based resin for the elastic wave glue.
In one embodiment, the reaction temperature in step S4 is 80-110 ℃.
Several specific examples of the present invention are given below, but the present invention is not limited by the examples.
In addition, the starting materials in the present invention are all commercially available unless otherwise specified.
Examples
Example 1
Embodiment 1 of the invention specifically provides an aqueous resin for an elasto-wave glue, and the aqueous resin for the elasto-wave glue is prepared from 100 parts by weight of epoxy resin, 50 parts by weight of organic solvent, 12 parts by weight of coupling agent, 0.5 part by weight of initiator, 10 parts by weight of acrylic acid comonomer, 6 parts by weight of fumed silica and 0.2 part by weight of hydroquinone;
the epoxy resin comprises bisphenol A type epoxy resin; the bisphenol A type epoxy resin consists of bisphenol A type epoxy resin-1 with the epoxy equivalent of 176-184g/eq and bisphenol A type epoxy resin-2 with the epoxy equivalent of 184-190 g/eq; the weight ratio of the bisphenol A epoxy resin-1 to the bisphenol A epoxy resin-2 is 1: 2; the epoxy resin further comprises butyl glycidyl ether; the epoxy equivalent of the butyl glycidyl ether is 145-155 g/eq; the weight of the butyl glycidyl ether is 10 percent of the weight of the epoxy resin;
the organic solvent is an alcohol ether solvent and an alcohol solvent; wherein the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: 1.5; the alcohol ether solvent is ethylene glycol butyl ether; the alcohol solvent is o-glycol; the vicinal diol is 1, 2-propanediol;
the coupling agent is an aminosilane coupling agent; the coupling agent is N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane; the weight ratio of the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane to the phenylaminomethyltrimethoxysilane is 2.4: 1;
the initiator is benzoyl peroxide;
the acrylic comonomer is a mixture of glycidyl methacrylate (CAS number: 106-91-2) and lauryl methacrylate (CAS number: 142-90-5); wherein the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is 1.8: 1;
the average particle size of the fumed silica is 12 nm;
the preparation method of the water-based resin for the elastic wave glue comprises the following preparation steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 6 hours after the mixed solution B is dropwise added, and finally adding hydroquinone to react for 40min to obtain the water-based resin for the elastic wave glue;
the reaction temperature in said step S4 was 80 ℃.
The bisphenol A type epoxy resin-1 is NPEL-127 of south Asia; the bisphenol A type epoxy resin-2 is NPEL-128 of south Asia; the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane is KBM-603; the phenylaminomethyl trimethoxy silane is nanda-73. The butyl glycidyl ether is HELOXY 61; the fumed silica is AEROSIL A200.
Example 2
Embodiment 2 of the invention specifically provides an aqueous resin for an elasto-wave glue, which is prepared from 100 parts by weight of epoxy resin, 70 parts by weight of organic solvent, 20 parts by weight of coupling agent, 1 part by weight of initiator, 18 parts by weight of acrylic comonomer, 10 parts by weight of fumed silica and 0.5 part by weight of hydroquinone;
the epoxy resin comprises bisphenol A type epoxy resin; the bisphenol A type epoxy resin consists of bisphenol A type epoxy resin-1 with the epoxy equivalent of 176-184g/eq and bisphenol A type epoxy resin-2 with the epoxy equivalent of 184-190 g/eq; the weight ratio of the bisphenol A epoxy resin-1 to the bisphenol A epoxy resin-2 is 1: 3; the epoxy resin further comprises butyl glycidyl ether; the epoxy equivalent of the butyl glycidyl ether is 145-155 g/eq; the weight of the butyl glycidyl ether is 15 percent of the weight of the epoxy resin;
the organic solvent is an alcohol ether solvent and an alcohol solvent; wherein the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: 2.2; the alcohol ether solvent is ethylene glycol butyl ether; the alcohol solvent is o-glycol; the vicinal diol is 1, 2-propanediol;
the coupling agent is an aminosilane coupling agent; the coupling agent is N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane; the weight ratio of the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane to the phenylaminomethyltrimethoxysilane is 3: 1;
the initiator is benzoyl peroxide;
the acrylic comonomer is a mixture of glycidyl methacrylate (CAS number: 106-91-2) and lauryl methacrylate (CAS number: 142-90-5); wherein the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is 2.5: 1;
the average particle size of the fumed silica is 12 nm;
the preparation method of the water-based resin for the elastic wave glue comprises the following preparation steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 5 hours after the mixed solution B is dropwise added, and finally adding hydroquinone to react for 30 minutes to obtain the water-based resin for the elastic wave glue;
the reaction temperature in said step S4 was 110 ℃.
The bisphenol A type epoxy resin-1 is NPEL-127 of south Asia; the bisphenol A type epoxy resin-2 is NPEL-128 of south Asia; the butyl glycidyl ether is HELOXY 61; the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane is KBM-603; the phenylaminomethyl trimethoxy silane is nanda-73; the fumed silica is AEROSIL A200.
Example 3
Embodiment 3 of the invention specifically provides an aqueous resin for an elastomer, which comprises the following raw materials, by weight, 100 parts of epoxy resin, 60 parts of an organic solvent, 16 parts of a coupling agent, 0.7 part of an initiator, 15 parts of an acrylic comonomer, 8 parts of fumed silica and 0.3 part of hydroquinone;
the epoxy resin comprises bisphenol A type epoxy resin; the bisphenol A type epoxy resin consists of bisphenol A type epoxy resin-1 with the epoxy equivalent of 176-184g/eq and bisphenol A type epoxy resin-2 with the epoxy equivalent of 184-190 g/eq; the weight ratio of the bisphenol A epoxy resin-1 to the bisphenol A epoxy resin-2 is 1: 2.5; the epoxy resin further comprises butyl glycidyl ether; the epoxy equivalent of the butyl glycidyl ether is 145-155 g/eq; the weight of the butyl glycidyl ether is 12 percent of the weight of the epoxy resin;
the organic solvent is an alcohol ether solvent and an alcohol solvent; the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: 1.8; the alcohol ether solvent is ethylene glycol butyl ether; the alcohol solvent is o-glycol; the vicinal diol is 1, 2-propanediol;
the coupling agent is an aminosilane coupling agent; the coupling agent is N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane; the weight ratio of the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane to the phenylaminomethyltrimethoxysilane is 2.7: 1;
the initiator is benzoyl peroxide;
the acrylic comonomer is a mixture of glycidyl methacrylate (CAS number: 106-91-2) and lauryl methacrylate (CAS number: 142-90-5); the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is 2.3: 1;
the average particle size of the fumed silica is 12 nm;
the preparation method of the water-based resin for the elastic wave glue comprises the following preparation steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 5.5 hours after the mixed solution B is dropwise added, and finally adding hydroquinone to react for 35 minutes to obtain the water-based resin for the elastic wave glue;
the reaction temperature in said step S4 was 100 ℃.
The bisphenol A type epoxy resin-1 is NPEL-127 of south Asia; the bisphenol A type epoxy resin-2 is NPEL-128 of south Asia; the butyl glycidyl ether is HELOXY 61; the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane is KBM-603; the phenylaminomethyl trimethoxy silane is nanda-73; the fumed silica is AEROSIL A200.
Example 4
Example 4 of the present invention specifically provides an aqueous resin for an elastomer, which is similar to example 3, except that no alcohol solvent is used.
Example 5
Example 5 of the present invention specifically provides an aqueous resin for an elasto-glue, which is similar to example 3, except that ethanol is used instead of vicinal diol.
Example 6
Example 6 of the present invention specifically provides an aqueous resin for an elastomer composition, which is prepared in the same manner as in example 3, except that gamma-aminopropyltriethoxysilane is used in place of N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane.
Example 7
Example 7 of the present invention specifically provides an aqueous resin for an elastomer composition, which is similar to example 3, except that phenylaminomethyltrimethoxysilane is not present.
Example 8
Example 8 of the present invention specifically provides an aqueous resin for an elasto-adhesive, which is similar to example 3, except that lauryl methacrylate is not present.
Performance testing
The aqueous resin for the catapult glue in the example and curing agent polyetheramine 230 (weight ratio 2: 1) are uniformly mixed, coated on 20T double 36 cotton cloth, the coating thickness is 50 μm, the mixture is cured for 10 hours at 50 ℃ to prepare a test sample, the test sample is placed in an environment at 50 ℃, the test sample is placed for 30 days, and the surface phenomenon is observed, wherein the number of the test samples is 100.
Evaluation criteria: the laboratory is evaluated by experienced researchers, and more than or equal to 95 test samples have no foaming, cracking, falling off and yellowing phenomena and are A grade; less than 95 and more than or equal to 85 test samples have no foaming, cracking, falling off and yellowing phenomena, and are B-grade; less than 85 and more than or equal to 70 test samples have no foaming, cracking, falling off and yellowing phenomena and are grade C; and less than 70 test samples have no foaming, cracking, falling off and yellowing phenomena and are D-grade.
The test results are shown in table 1:
TABLE 1
| High temperature resistance | |
| Example 1 | Class A |
| Example 2 | Class A |
| Example 3 | Class A |
| Example 4 | Class D |
| Example 5 | Class C |
| Example 6 | Class B |
| Example 7 | Class C |
| Example 8 | Class C |
From the test results in table 1, it can be seen that the ebonite resin of the present invention has good heat resistance.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (5)
1. The aqueous resin for the elastic wave glue is characterized by comprising the following raw materials, by weight, 100 parts of epoxy resin, 50-70 parts of organic solvent, 12-20 parts of coupling agent, 0.5-1 part of initiator, 10-18 parts of acrylic comonomer, 6-10 parts of fumed silica and 0.2-0.5 part of hydroquinone;
the epoxy resin comprises bisphenol A type epoxy resin;
the organic solvent is an alcohol ether solvent and an alcohol solvent;
the weight ratio of the alcohol ether solvent to the alcohol solvent is 1: (1.5-2.2);
the alcohol ether solvent is ethylene glycol butyl ether;
the alcohol solvent is o-glycol, and the o-glycol is 1, 2-propylene glycol;
the coupling agent is N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane and phenylaminomethyltrimethoxysilane, and the weight ratio of the N-beta (aminoethyl) -gamma-aminopropyltrimethoxysilane to the phenylaminomethyltrimethoxysilane is (2.4-3): 1;
the acrylic acid comonomer is a mixture of glycidyl methacrylate and lauryl methacrylate; wherein the weight ratio of the glycidyl methacrylate to the lauryl methacrylate is (1.8-2.5): 1.
2. the waterborne resin for the elastomer gel of claim 1, wherein the epoxy resin further comprises butyl glycidyl ether.
3. The aqueous resin for an elastomer according to claim 1, wherein the fumed silica has an average particle diameter of 8 to 20 nm.
4. A method for preparing the aqueous resin for an elastomer according to any one of claims 1 to 3, which comprises the following steps:
s1: weighing corresponding parts by weight of preparation raw materials of the waterborne resin for the elastic wave glue for later use;
s2: 1/3 parts by weight of organic solvent, 1/3 parts by weight of coupling agent and fumed silica are stirred and mixed uniformly to obtain a mixed solution A;
s3: uniformly mixing an acrylic acid comonomer, an initiator and the rest of a coupling agent to obtain a mixed solution B;
s4: uniformly mixing the mixed solution A with epoxy resin to obtain a mixed solution C; and then, under the protection of nitrogen, dropwise adding the mixed solution B into the mixed solution C, continuing to react for 5-6h after the dropwise adding of the mixed solution B is finished, and finally adding hydroquinone to react for 30-40min to obtain the water-based resin for the elastic wave glue.
5. The method for preparing an aqueous resin for an elastomer composition according to claim 4, wherein the reaction temperature in step S4 is 80-110 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440723A (en) * | 2018-03-12 | 2018-08-24 | 广州市精合致新材料科技有限公司 | Aqueous bullet wave impregnation shaping glue of one kind and preparation method thereof |
| CN109280523A (en) * | 2018-10-17 | 2019-01-29 | 东莞市沅邦电子材料有限公司 | Epoxy sealing glue |
| WO2019229695A1 (en) * | 2018-06-01 | 2019-12-05 | 3M Innovative Properties Company | Acrylic-epoxy adhesive composition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440723A (en) * | 2018-03-12 | 2018-08-24 | 广州市精合致新材料科技有限公司 | Aqueous bullet wave impregnation shaping glue of one kind and preparation method thereof |
| WO2019229695A1 (en) * | 2018-06-01 | 2019-12-05 | 3M Innovative Properties Company | Acrylic-epoxy adhesive composition |
| CN109280523A (en) * | 2018-10-17 | 2019-01-29 | 东莞市沅邦电子材料有限公司 | Epoxy sealing glue |
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