CN117025151A - Epoxy resin adhesive and preparation method thereof - Google Patents
Epoxy resin adhesive and preparation method thereof Download PDFInfo
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- CN117025151A CN117025151A CN202311057523.5A CN202311057523A CN117025151A CN 117025151 A CN117025151 A CN 117025151A CN 202311057523 A CN202311057523 A CN 202311057523A CN 117025151 A CN117025151 A CN 117025151A
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- silane coupling
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 55
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 55
- 239000000853 adhesive Substances 0.000 title claims abstract description 41
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000011258 core-shell material Substances 0.000 claims abstract description 17
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 12
- 239000011256 inorganic filler Substances 0.000 claims abstract description 12
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 12
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 150000001412 amines Chemical class 0.000 claims abstract description 9
- 239000012745 toughening agent Substances 0.000 claims abstract description 8
- 239000003085 diluting agent Substances 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 75
- 239000000377 silicon dioxide Substances 0.000 claims description 35
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 23
- 230000002209 hydrophobic effect Effects 0.000 claims description 22
- 239000003963 antioxidant agent Substances 0.000 claims description 18
- 230000003078 antioxidant effect Effects 0.000 claims description 18
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000003365 glass fiber Substances 0.000 claims description 16
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 10
- 239000003063 flame retardant Substances 0.000 claims description 10
- 239000004952 Polyamide Substances 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 229920002647 polyamide Polymers 0.000 claims description 9
- 229920006332 epoxy adhesive Polymers 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- CFEKOKRYQRODRZ-UHFFFAOYSA-N 2-cyclohexylethane-1,1-diamine Chemical compound NC(N)CC1CCCCC1 CFEKOKRYQRODRZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000281 calcium bentonite Inorganic materials 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 21
- 239000005062 Polybutadiene Substances 0.000 description 13
- 229920002857 polybutadiene Polymers 0.000 description 13
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 description 7
- 235000019445 benzyl alcohol Nutrition 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 239000005060 rubber Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GOJUJUVQIVIZAV-UHFFFAOYSA-N 2-amino-4,6-dichloropyrimidine-5-carbaldehyde Chemical group NC1=NC(Cl)=C(C=O)C(Cl)=N1 GOJUJUVQIVIZAV-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007771 core particle Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an epoxy resin adhesive, which relates to the technical field of epoxy resin adhesives, and consists of a component A and a component B in a mass ratio of 2:1, wherein the component A comprises the following components in parts by weight: 44-150 parts of epoxy resin, 2-8 parts of diluent, 10-60 parts of flexibilizer, 15-60 parts of inorganic filler, 1-5 parts of thixotropic agent and 1-5 parts of auxiliary agent; and the component B comprises the following components: 22-65 parts of amine curing agent, 20-45 parts of inorganic filler, 2-6 parts of thixotropic agent, 1-6 parts of auxiliary agent and 1-5 parts of accelerator. According to the epoxy resin adhesive and the preparation method thereof, the high-performance core-shell particles are prepared through synthesis, and the high-performance core-shell particles are used as the toughening agent for toughening the epoxy resin, so that the toughness of the epoxy resin adhesive can be obviously improved under the condition that the mechanical property of the epoxy resin is not reduced.
Description
Technical Field
The invention relates to the technical field of epoxy resin adhesives, in particular to an epoxy resin adhesive and a preparation method thereof.
Background
The epoxy resin adhesive has excellent adhesion, electrical insulation performance, chemical stability, durability and wide application. With the development of light weight and precision of the electronic industry, the performance requirement on the epoxy adhesive is higher and higher.
In the preparation of the epoxy resin adhesive, the epoxy resin is a linear thermoplastic substance, and a three-dimensional net structure is obtained after a curing agent is added, so that the structure is hard and brittle. In addition, the epoxy resin is shrunk in the process of heating, solidifying and cooling to form a solidified object, internal stress is generated, cracks are easily generated in the solidified object, the epoxy resin is not impact-resistant and poor in toughness, and the existing epoxy resin adhesive is poor in toughness and low in impact strength.
In the prior art, bisphenol A type epoxy resin and a curing agent are combined, and then rubber or elastomer toughening agent is matched, so that the impact strength of the cured resin is improved, and the adhesiveness of the cured resin are improved. However, the existing toughening agents, while improving part of the toughness, have other properties that are not good.
Disclosure of Invention
The invention aims to provide an epoxy resin adhesive and a preparation method thereof, wherein high-performance core-shell particles are prepared through synthesis, and the high-performance core-shell particles are used as a toughening agent for toughening epoxy resin, so that the toughness of the epoxy resin adhesive can be obviously improved under the condition that the mechanical property of the epoxy resin is not reduced.
In order to achieve the purpose, the invention provides an epoxy resin adhesive which comprises the following components in parts by weight:
and (3) a component A: 44-150 parts of epoxy resin, 2-8 parts of diluent, 10-60 parts of flexibilizer, 15-60 parts of inorganic filler, 1-5 parts of thixotropic agent and 1-5 parts of auxiliary agent;
and the component B comprises the following components: 22-65 parts of amine curing agent, 20-45 parts of inorganic filler, 2-6 parts of thixotropic agent, 1-6 parts of auxiliary agent and 1-5 parts of accelerator.
Preferably, the epoxy resin is one or more of epoxy resin E51, epoxy resin E44, epoxy resin E31 and epoxy resin E20.
Preferably, the toughening agent is SiO 2 PB@PMMA core-shell particles.
Preferably, the inorganic filler is one or more of alumina, glass fiber, silica micropowder, calcium carbonate, bentonite and kaolin.
Preferably, the thixotropic agent is one or more of hydrophobic silica H18, hydrophobic silica H15, hydrophobic silica H30, hydrophobic silica H2000, hydrophilic silica N20.
Preferably, the amine curing agent is one or more of isophorone diamine, polyamide 650, polyetheramine 230, trimethylhexamethylene diamine, piperidine, and diaminomethyl cyclohexyl methane.
Preferably, the auxiliary agent comprises one or more of a silane coupling agent, an antioxidant and a flame retardant;
the silane coupling agent is one or more of silane coupling agent KH-550, silane coupling agent KH-560 and silane coupling agent KH-792;
the antioxidant is one or more of Pasteur 1010 and Pasteur 1076;
the flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, antimony trioxide, phosphorus-containing flame retardant, nitrogen-containing flame retardant and silicon-based flame retardant.
A preparation method of an epoxy resin adhesive comprises the following steps:
s1, placing epoxy resin, a diluent, a toughening agent, an inorganic filler, a thixotropic agent and an auxiliary agent in parts by weight into a strong stirrer, and stirring for 120min at 60 ℃ in vacuum to obtain a component A;
s2, adding an amine curing agent, an inorganic filler, a thixotropic agent, an auxiliary agent and an accelerator into a strong stirrer according to parts by weight, and stirring for 120min at 60 ℃ in vacuum to obtain a component B;
and S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Therefore, the epoxy resin adhesive and the preparation method thereof adopting the formula can toughen the epoxy resin through the core-shell particles, and can compound the soft rubber phase and the rigid phase in a unique core-shell mode under the condition of not reducing the mechanical property of the epoxy resin, namely, the high-efficiency toughening effect is obtained through the double-layer design of polymer molecules and particles, and the toughness of the epoxy resin adhesive is improved. And the core-shell particles and the filler are uniformly dispersed in the epoxy resin, namely, the particles are independently dispersed in the resin, so that the heat resistance, strength and rigidity loss caused by incomplete phase separation are avoided, the whole adhesive system is stable, and the toughness of the epoxy resin adhesive is improved.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
The technical scheme of the invention is further described below by examples.
The present invention will be explained in more detail by the following examples, and the purpose of the present invention is to protect all changes and modifications within the scope of the present invention, and the present invention is not limited to the following examples.
Example 1
S1, 118 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether and SiO 2 12 parts of PB@PMMA core-shell particles, 39 parts of silica micropowder, 10 parts of alumina, 10 parts of glass fiber, 4 parts of hydrophobic silica (H18), 2 parts of silane coupling agent (KH-560) and 1 part of antioxidant are placed into a strong stirrer, and are stirred in vacuum for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 16 parts of polyetheramine (D-230), 10 parts of isophorone diamine (IPDA), 28 parts of silica powder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Example 2
S1, 124 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether and SiO 2 16 parts of PB@PMMA core-shell particles, 29 parts of silica micropowder, 10 parts of alumina, 10 parts of glass fiber, 4 parts of hydrophobic silica (H18) and silane coupling2 parts of agent (KH-560) and 1 part of antioxidant are put into a strong mixer, and are stirred for 120min under the condition of 60 ℃ in vacuum to obtain the component A.
S2, adding 30 parts of polyamide (650), 18 parts of polyether amine (D-230), 10 parts of isophorone diamine (IPDA), 26 parts of silica powder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Example 3
S1, 130 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether and SiO 2 20 parts of PB@PMMA core-shell particles, 19 parts of silica micropowder, 10 parts of alumina, 10 parts of glass fiber, 4 parts of hydrophobic silica (H18), 2 parts of silane coupling agent (KH-560) and 1 part of antioxidant are placed into a strong stirrer, and are stirred in vacuum for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 20 parts of polyetheramine (D-230), 10 parts of isophorone diamine (IPDA), 24 parts of silica powder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Example 4
S1, 136 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether and SiO 2 24 parts of PB@PMMA core-shell particles, 9 parts of silica micropowder, 10 parts of alumina, 10 parts of glass fiber, 4 parts of hydrophobic silica (H18), 2 parts of silane coupling agent (KH-560) and 1 part of antioxidant are placed into a strong stirrer, and are stirred in vacuum for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 22 parts of polyether amine (D-230), 10 parts of isophorone diamine (IPDA), 22 parts of silica micropowder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Example 5
S1, 142 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether and SiO 2 28 parts of PB@PMMA core-shell particles, 9 parts of alumina, 10 parts of glass fibers, 4 parts of hydrophobic silica (H18), 2 parts of a silane coupling agent (KH-560) and 1 part of an antioxidant are placed into a strong stirrer, and are stirred in vacuum for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 24 parts of polyetheramine (D-230), 10 parts of isophorone diamine (IPDA), 20 parts of silica powder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Example 6
1, 3-butadiene is adopted as a raw material, polybutadiene (PB) soft rubber particles are prepared through emulsion polymerization, the Polybutadiene (PB) soft rubber particles are used as an inner core, methyl Methacrylate (MMA) is used as a monomer to form a hard polymethyl methacrylate (PMMA) shell on the surface of the soft rubber inner core particles, PB@PMMA particles are prepared, and meanwhile gamma-aminopropyl triethoxysilane (KH 550) is adopted for nano SiO 2 Surface treatment is carried out by hydroxyl and SiO after siloxane hydrolysis on gamma-aminopropyl triethoxysilane 2 Surface hydroxyl condensation on SiO 2 Amino groups are introduced on the surface to make the surface positively charged. Finally, adsorbing modified SiO with positive charges on the surface of the core-shell particles with negative charges through electrostatic self-assembly 2 Nano particles, and SiO is prepared 2 PB@PMMA core-shell particles.
Comparative example 1
S1, 100 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether, 69 parts of silica micropowder, 10 parts of alumina, 10 parts of glass fiber, 4 parts of hydrophobic silica (H18), 2 parts of silane coupling agent (KH-560) and 1 part of antioxidant are placed into a strong stirrer, and are stirred in vacuum for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 10 parts of polyetheramine (D-230), 10 parts of isophorone diamine (IPDA), 34 parts of silica micropowder, 5 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
TABLE 1 Table of Properties of epoxy resin adhesives in example 3 and comparative example 1
| Comparative example 1 | Example 3 | |
| Tensile Strength (MPa) | 64.7 | 60.1 |
| Shear strength (Mpa) | 23.1 | 29.4 |
| Elongation at break (%) | 1.7 | 3.1 |
Comparative example 2
S1, 100 parts of epoxy resin (E51), 4 parts of benzyl glycidyl ether, 39 parts of silica micropowder, 20 parts of alumina, 30 parts of glass fiber, 4 parts of hydrophobic silica (H18), 2 parts of silane coupling agent (KH-560) and 1 part of antioxidant are placed into a strong mixer, and vacuum mixing is carried out for 120min at 60 ℃ to obtain a component A.
S2, adding 30 parts of polyamide (650), 10 parts of polyetheramine (D-230), 10 parts of isophorone diamine (IPDA), 24 parts of silica powder, 15 parts of alumina, 5 parts of glass fiber, 2 parts of hydrophobic silica (H18), 1 part of silane coupling agent (KH-550), 1 part of antioxidant and 2 parts of benzyl alcohol into a strong stirrer, and stirring for 120min at 60 ℃ under vacuum to obtain a component B.
And S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
Table 2 table of properties of epoxy resin adhesives in examples 1, 2, 4, 5 and comparative example 2
| Example 1 | Example 2 | Example 4 | Example 5 | Comparative example 2 | |
| Tensile Strength (MPa) | 57.22 | 58.99 | 60.14 | 56.47 | 54.17 |
| Shear strength (Mpa) | 23.01 | 25.47 | 29.44 | 28.11 | 18.75 |
| Elongation at break (%) | 1.97 | 2.61 | 3.1 | 2.91 | 1.41 |
As can be seen from tables 1 and 2, siO 2 After the PB@PMMA core-shell particles are added, the tensile strength and the shear strength are not obviously affected, and the elongation at break is obviously improved.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (9)
1. An epoxy resin adhesive is characterized in that: comprises the following components in parts by weight,
and (3) a component A: 44-150 parts of epoxy resin, 2-8 parts of diluent, 10-60 parts of flexibilizer, 15-60 parts of inorganic filler, 1-5 parts of thixotropic agent and 1-5 parts of auxiliary agent;
and the component B comprises the following components: 22-65 parts of amine curing agent, 20-45 parts of inorganic filler, 2-6 parts of thixotropic agent, 1-6 parts of auxiliary agent and 1-5 parts of accelerator.
2. An epoxy adhesive according to claim 1, wherein: the mass ratio of the component A to the component B is 2:1.
3. An epoxy adhesive according to claim 1, wherein: the epoxy resin is one or more of epoxy resin E51, epoxy resin E44, epoxy resin E31 and epoxy resin E20.
4. An epoxy adhesive according to claim 1, wherein: the toughening agent is SiO 2 PB@PMMA core-shell particles.
5. An epoxy adhesive according to claim 1, wherein: the inorganic filler is one or more of alumina, glass fiber, silica micropowder, calcium carbonate, bentonite and kaolin.
6. An epoxy adhesive according to claim 1, wherein: the thixotropic agent is one or more of hydrophobic fumed silica H18, hydrophobic fumed silica H15, hydrophobic fumed silica H30, hydrophobic fumed silica H2000 and hydrophilic silica N20.
7. An epoxy adhesive according to claim 1, wherein: the amine curing agent is one or more of isophorone diamine, polyamide 650, polyetheramine 230, trimethylhexamethylene diamine, piperidine and diaminomethyl cyclohexyl methane.
8. An epoxy adhesive according to claim 1, wherein: the auxiliary agent comprises one or more of a silane coupling agent, an antioxidant and a flame retardant;
the silane coupling agent is one or more of silane coupling agent KH-550, silane coupling agent KH-560 and silane coupling agent KH-792;
the antioxidant is one or more of Pasteur 1010 and Pasteur 1076;
the flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, antimony trioxide, phosphorus-containing flame retardant, nitrogen-containing flame retardant and silicon-based flame retardant.
9. The method for preparing the epoxy resin adhesive according to any one of claims 1 to 8, wherein:
s1, placing epoxy resin, a diluent, a toughening agent, an inorganic filler, a thixotropic agent and an auxiliary agent in parts by weight into a strong stirrer, and stirring for 120min at 60 ℃ in vacuum to obtain a component A;
s2, adding an amine curing agent, an inorganic filler, a thixotropic agent, an auxiliary agent and an accelerator into a strong stirrer according to parts by weight, and stirring for 120min at 60 ℃ in vacuum to obtain a component B;
and S3, when the adhesive is used, the component A and the component B are mixed according to the mass ratio of 2:1 and then uniformly stirred, and the adhesive is cured for 6 hours at 70 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311057523.5A CN117025151A (en) | 2023-08-22 | 2023-08-22 | Epoxy resin adhesive and preparation method thereof |
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| CN202311057523.5A CN117025151A (en) | 2023-08-22 | 2023-08-22 | Epoxy resin adhesive and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118685142A (en) * | 2024-08-23 | 2024-09-24 | 合肥中聚和成电子材料有限公司 | Liquid crystal frame sealing adhesive and preparation method thereof |
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2023
- 2023-08-22 CN CN202311057523.5A patent/CN117025151A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118685142A (en) * | 2024-08-23 | 2024-09-24 | 合肥中聚和成电子材料有限公司 | Liquid crystal frame sealing adhesive and preparation method thereof |
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