CN110628337A - Preparation method of thixotropic epoxy resin adhesive film - Google Patents
Preparation method of thixotropic epoxy resin adhesive film Download PDFInfo
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- CN110628337A CN110628337A CN201910942750.3A CN201910942750A CN110628337A CN 110628337 A CN110628337 A CN 110628337A CN 201910942750 A CN201910942750 A CN 201910942750A CN 110628337 A CN110628337 A CN 110628337A
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- epoxy resin
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- thixotropic
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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
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
Abstract
The invention relates to the technical field of photovoltaic cells, in particular to a preparation method of thixotropic epoxy resin, which comprises the following steps: (1) weighing the component A: 100 parts of bisphenol A epoxy resin, 10-30 parts of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexyl carboxylate, 10-20 parts of fumed silica, 10-20 parts of diluent and 0.3-0.8 part of antioxidant, and (2) weighing the components B: 10-20 parts of curing agent, 2-10 parts of toughening agent and 0.5-2.8 parts of accelerator, and (3) mixing the component A and the component B in proportion, adding 2-8 parts of filler, uniformly mixing, and extruding to obtain a thixotropic epoxy resin adhesive film; the preparation method of the thixotropic epoxy resin adhesive film is simple in process, and the problems of low heat resistance and high brittleness caused by curing of epoxy resin and amine curing agent are solved by adding the toughening agent, the accelerant and the diluent.
Description
Technical Field
The invention relates to the technical field of photovoltaic cells, in particular to a preparation method of a thixotropic epoxy resin adhesive film.
Background
The epoxy resin means that one molecular structure contains at least two or more epoxy groups. The epoxy resin composition is not cured at normal room temperature or normal heating, so that the epoxy resin composition cannot be directly used alone. After the curing agent is added, the curing agent is crosslinked to form a reticular structure, so that various excellent properties of the curing agent can be displayed. The epoxy resin has many kinds, the most important of which is bisphenol A type epoxy resin, which accounts for more than 85 percent of the epoxy resin used at present, and after the curing agent is added, the epoxy resin has good adhesive property to glass and metal.
Although the epoxy resin adhesive film has high crosslinking density and hardness, the technical defects of poor impact resistance and poor toughness exist.
Disclosure of Invention
The purpose of the invention is: the method for preparing the thixotropic epoxy resin adhesive film overcomes the defects in the prior art, and the epoxy resin prepared by the method has the characteristics of strong impact resistance and good flexibility.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 10-30 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 10-20 parts of fumed silica, 10-20 parts of diluent, 0.3-0.8 part of antioxidant,
(2) weighing the component B: 10-20 parts of curing agent, 2-10 parts of toughening agent and 0.5-2.8 parts of accelerator
(3) And (3) mixing the component A and the component B in proportion, adding 2-8 parts of a filling agent, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Further, the bisphenol A epoxy resin comprises one of E-51, E-44 and E-55.
Further, the curing agent is an amine curing agent and is selected from one or more of m-PDA, MPD, diaminodiphenylmethane DDM, HT-972 and DEH-50.
Further, the curing agent is a mixture of m-PDA and diaminodiphenylmethane DDM, and the mass ratio of m-PDA to diaminodiphenylmethane DDM is 1: 1-3.
Further, the diluent is selected from one of acetone and ethanol.
Further, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, wherein the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Further, the toughening agent is selected from one of polyamide, nitrile rubber, carboxyl-terminated liquid nitrile rubber and polysulfide rubber.
Further, the accelerator is one of salicylic acid and benzyl dimethylamine.
Furthermore, the filling agent is talcum powder or aluminum powder.
The technical scheme adopted by the invention has the beneficial effects that:
the preparation method of the thixotropic epoxy resin adhesive film is simple in process, the problems of low heat resistance and high brittleness caused by curing of epoxy resin and an amine curing agent are solved by adding the toughening agent, the accelerant can reduce the reaction activation energy of the curing agent and improve the physical properties of the curing agent, in order that the elongation of the modified epoxy resin adhesive after curing is reduced, the brittleness of a cured product is increased, cracks are generated when a certain external extrusion force is borne, and the cured product is expanded to crack, the improvement can be realized by adding the toughening agent, the toughening agent contains an active group, the toughening agent is not completely compatible with the cured adhesive, so that the toughness of the cured product is obviously increased, the viscosity of the adhesive is reduced, the fluidity of the adhesive is increased, and the service life of the adhesive is prolonged.
Detailed Description
The invention will now be further illustrated with reference to specific examples.
Example 1
A method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 10 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 10 parts of fumed silica, 10 parts of diluent and 0.3 part of antioxidant,
(2) weighing the component B: 10 parts of curing agent, 2 parts of toughening agent and 0.5 part of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 2 parts of filler, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Wherein the bisphenol A epoxy resin is E-51.
Wherein the curing agent is an amine curing agent selected from m-phenylenediamine-PDA.
Wherein the diluent is acetone.
Wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Wherein the toughening agent is polyamide.
Wherein the promoter is salicylic acid.
Wherein the filler is talc powder.
Example 2
A method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 12 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 12 parts of fumed silica, 12 parts of diluent and 0.4 part of antioxidant,
(2) weighing the component B: 12 parts of curing agent, 3 parts of toughening agent and 0.6 part of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 3 parts of filler, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Wherein the bisphenol A epoxy resin is E-51.
Wherein the curing agent is a mixture of m-phenylenediamine m-PDA and diaminodiphenylmethane DDM, and the mass ratio of the m-phenylenediamine m-PDA to the diaminodiphenylmethane DDM is 1: 1.
Wherein the diluent is acetone.
Wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Wherein the toughening agent is polyamide.
Wherein the promoter is salicylic acid.
Wherein the filler is talc powder.
Example 3
A method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 20 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 15 parts of fumed silica, 15 parts of diluent and 0.5 part of antioxidant,
(2) weighing the component B: 15 parts of curing agent, 6 parts of toughening agent and 1.6 parts of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 5 parts of filler, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Wherein the bisphenol A epoxy resin is E-44.
Wherein the curing agent is a mixture of m-phenylenediamine m-PDA and diaminodiphenylmethane DDM, and the mass ratio of the m-phenylenediamine m-PDA to the diaminodiphenylmethane DDM is 1:2.
Wherein the diluent is ethanol.
Wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Wherein, the toughening agent is carboxyl-terminated liquid nitrile rubber.
Wherein, the accelerant is benzyl dimethylamine.
Wherein the filler is aluminum powder.
Example 4
A method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 25 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 18 parts of fumed silica, 18 parts of diluent and 0.6 part of antioxidant,
(2) weighing the component B: 28 parts of curing agent, 8 parts of toughening agent and 2.5 parts of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 6 parts of filler, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Wherein the bisphenol A epoxy resin is E-55.
Wherein the curing agent is a mixture of m-phenylenediamine m-PDA and diaminodiphenylmethane DDM, and the mass ratio of the m-phenylenediamine m-PDA to the diaminodiphenylmethane DDM is 1: 2.5.
Wherein the diluent is acetone.
Wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Wherein, the toughening agent is polysulfide rubber.
Wherein, the accelerant is benzyl dimethylamine.
Wherein the filler is aluminum powder.
Example 5
A method of preparing a thixotropic epoxy resin, the method comprising the steps of:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 30 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 20 parts of fumed silica, 20 parts of diluent and 0.8 part of antioxidant,
(2) weighing the component B: 20 parts of curing agent, 10 parts of toughening agent and 2.8 parts of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 8 parts of filler, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
Wherein the bisphenol A epoxy resin is E-55.
Wherein the curing agent is a mixture of m-phenylenediamine m-PDA and diaminodiphenylmethane DDM, and the mass ratio of the m-phenylenediamine m-PDA to the diaminodiphenylmethane DDM is 1: 3.
Wherein the diluent is acetone.
Wherein the antioxidant comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
Wherein, the toughening agent is polysulfide rubber.
Wherein the promoter is salicylic acid.
Wherein the filler is talc powder.
The preparation method of the thixotropic epoxy resin adhesive film is simple in process, the problems of low heat resistance and high brittleness caused by curing of epoxy resin and an amine curing agent are solved by adding the toughening agent, the accelerant can reduce the reaction activation energy of the curing agent and improve the physical properties of the curing agent, in order that the elongation of the modified epoxy resin adhesive after curing is reduced, the brittleness of a cured product is increased, cracks are generated when a certain external extrusion force is borne, and the cured product is expanded to crack, the improvement can be realized by adding the toughening agent, the toughening agent contains an active group, the toughening agent is not completely compatible with the cured adhesive, so that the toughness of the cured product is obviously increased, the viscosity of the adhesive is reduced, the fluidity of the adhesive is increased, and the service life of the adhesive is prolonged.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (9)
1. A preparation method of thixotropic epoxy resin is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) weighing the component A: 100 parts of bisphenol A epoxy resin, 10-30 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl carboxylate, 10-20 parts of fumed silica, 10-20 parts of diluent, 0.3-0.8 part of antioxidant,
(2) weighing the component B: 10 to 20 portions of curing agent, 2 to 10 portions of flexibilizer, 0.5 to 2.8 portions of accelerant,
(3) and (3) mixing the component A and the component B in proportion, adding 2-8 parts of a filling agent, uniformly mixing, and extruding to obtain the thixotropic epoxy resin adhesive film.
2. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the bisphenol A epoxy resin comprises one of E-51, E-44 and E-55.
3. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the curing agent is amine curing agent, and is selected from one or more of m-PDA, MPD, diaminodiphenylmethane DDM, HT-972 and DEH-50.
4. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the curing agent is a mixture of m-phenylenediamine m-PDA and diaminodiphenylmethane DDM, and the mass ratio of the m-phenylenediamine m-PDA to the diaminodiphenylmethane DDM is 1: 1-3.
5. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the diluent is selected from one of acetone and ethanol.
6. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the antioxidant comprises a main antioxidant and an auxiliary antioxidant, wherein the main antioxidant is an antioxidant 1010, and the auxiliary antioxidant is an antioxidant 1076.
7. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the toughening agent is selected from one of polyamide, nitrile rubber, carboxyl-terminated liquid nitrile rubber and polysulfide rubber.
8. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the accelerator is one of salicylic acid and benzyl dimethylamine.
9. The method of claim 1 for preparing a thixotropic epoxy resin, wherein: the filling agent is talcum powder or aluminum powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982388A (en) * | 2020-01-02 | 2020-04-10 | 中国科学院兰州化学物理研究所 | Room-temperature curing coating with abradable sealing function and preparation method thereof |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982388A (en) * | 2020-01-02 | 2020-04-10 | 中国科学院兰州化学物理研究所 | Room-temperature curing coating with abradable sealing function and preparation method thereof |
| CN110982388B (en) * | 2020-01-02 | 2021-06-01 | 中国科学院兰州化学物理研究所 | Room-temperature curing coating with abradable sealing function and preparation method thereof |
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Application publication date: 20191231 |