CN114854350A - Low-viscosity high-thixotropy epoxy resin sealant and preparation method and application thereof - Google Patents
Low-viscosity high-thixotropy epoxy resin sealant and preparation method and application thereof Download PDFInfo
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- CN114854350A CN114854350A CN202210572115.2A CN202210572115A CN114854350A CN 114854350 A CN114854350 A CN 114854350A CN 202210572115 A CN202210572115 A CN 202210572115A CN 114854350 A CN114854350 A CN 114854350A
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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
- 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
- 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
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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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a low-viscosity high-thixotropy epoxy resin sealant and a preparation method thereof, belonging to the technical field of electronic packaging adhesives. The single-component epoxy resin adhesive prepared by the invention has the advantages that the viscosity of a mixture is 1900mPa & s, the viscosity is low, the thixotropic index is 1.25, the thixotropic index is high, the mixture is surface-dried at 120-140 ℃ in 30-40 minutes, a cured product does not crack or foam at high temperature of 240-260 ℃, the effect is obvious, and the adhesive is suitable for high-temperature sealing electronic materials.
Description
The application is a divisional application with application date of 2019, 07, 17 and application number of 201910645563.9, and the invention name of low-viscosity high-thixotropy epoxy resin sealant and a preparation method thereof.
Technical Field
The invention belongs to the technical field of electronic packaging adhesives, and particularly relates to a low-viscosity high-thixotropy epoxy resin sealant as well as a preparation method and application thereof.
Background
The epoxy resin generally refers to a high molecular prepolymer having 2 or more epoxy groups and having a skeleton made of an organic compound such as an aliphatic or aromatic compound. At present, the types of epoxy resin are complete and the functions are different. Bisphenol a epoxy resin contains a highly polar molecular structure such as a hydroxyl group, an epoxy group, and an ether bond in its structure, and can preferably generate intermolecular forces with an adjacent interface. The bisphenol A epoxy resin has excellent performance after being cured due to the special performance of the bisphenol A epoxy resin: the material has the advantages of small shrinkage, excellent electrical property, good high temperature resistance and the like. Therefore, the method can be widely applied to electronic components, military communication products and the like. Especially in the application of electronic packaging materials, the material is very popular. The stability of the molecular structure of the epoxy resin enables the epoxy resin to maintain the self-performance at 200 ℃. However, epoxy resin can exhibit its properties only by opening epoxy groups with a curing agent and by crosslinking the epoxy groups to form an insoluble, infusible thermosetting resin having a three-dimensional network structure. Epoxy resin is used as a sealing material of electronic products, and is required to have good flowing property, the viscosity is required to be controlled below 4000mPa & s at normal temperature, but in the process of gluing, the sealing effect is poor due to flowing and permeation of glue solution. Therefore, on the premise of ensuring the fluidity at normal temperature, the high thixotropy is very important.
Disclosure of Invention
The invention provides a low-viscosity high-thixotropy epoxy resin sealant, a preparation method and application thereof.
In order to achieve the purpose, the invention provides the following technical scheme: a low-viscosity high-thixotropy epoxy resin sealant is prepared from the following components in parts by weight of 1: 1, mixing the component A and the component B;
the component A is prepared from the following components in percentage by weight: bisphenol A epoxy resin E5180%, phenyl glycidyl ether 15%, defoaming agent 62010.5%, fumed silica 0.5%, polyamide wax 1%, polysulfide rubber 1%, and carboxyl-terminated liquid nitrile rubber 2%;
the component B is prepared from the following components in percentage by weight: 95% of polytetrahydrofthalic anhydride, 1.5% of triethanolamine and 3.5% of benzoyl peroxide;
the preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin E51, phenyl glycidyl ether and a defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at a rotation speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at a rotation speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component A;
(2) sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B;
(3) and (3) uniformly mixing the component A in the step (1) and the component B in the step (2) to prepare the low-viscosity high-thixotropy epoxy resin sealant.
The preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin E51, phenyl glycidyl ether and a defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at a rotation speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at a rotation speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component A;
(2) sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B;
(3) and (3) uniformly mixing the component A in the step (1) and the component B in the step (2) to prepare the low-viscosity high-thixotropy epoxy resin sealant.
The invention also provides application of the low-viscosity high-thixotropy epoxy resin sealant prepared by the scheme or the low-viscosity high-thixotropy epoxy resin sealant prepared by the preparation method in high-temperature sealing of electronic materials.
Compared with the prior art, the invention has the beneficial effects that:
the single-component epoxy resin sealant prepared by the invention has the advantages of viscosity of 1900mPa & s, low viscosity, thixotropic index of 1.25, high thixotropic index, surface drying of the mixture at 120-140 ℃ within 30-40 minutes, no cracking and no foaming of a cured product at high temperature of 240-260 ℃, obvious effect and suitability for high-temperature sealing of electronic materials.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The low-viscosity high-thixotropy epoxy resin sealant is prepared by mixing a component A and a component B;
wherein the component A comprises the following components in percentage by weight: 80% of bisphenol A epoxy resin E12, 10% of dodecyl glycidyl ether, 1% of defoaming agent 6201, 0.5% of fumed silica, 0.5% of polyamide wax, 4% of carboxyl-terminated liquid nitrile rubber and 4% of polysulfide rubber;
the component B comprises the following components in percentage by weight: 95% of polytetrahydrofthalic anhydride, 1% of triethanolamine and 4% of benzoyl peroxide;
the preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin, dodecyl glycidyl ether and defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at the rotating speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed and dry environment at the temperature of 10-25 ℃ to obtain the component A.
(2) Sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, discharging after vacuumizing, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B.
(3) 100g of the A component of step (1) and 100g of the B component of step (2) were mixed uniformly, defoamed in vacuum, and tested for viscosity and thixotropic index at 25 ℃ and the results are shown in Table 1.
Example 2
The low-viscosity high-thixotropy epoxy resin sealant is prepared by mixing a component A and a component B;
wherein the component A comprises the following components in percentage by weight: 80% of bisphenol A type epoxy resin E44, 12% of ethylene glycol glycidyl ether, 1% of defoaming agent 6201, 0.5% of fumed silica, 1% of polyamide wax, 2% of carboxyl-terminated liquid nitrile rubber and 3.5% of polysulfide rubber;
the component B comprises the following components in percentage by weight: 95% phthalic anhydride, 5% benzoyl peroxide;
the preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin E44, ethylene glycol glycidyl ether and a defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at a rotation speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at a rotation speed of 400rpm, vacuumizing, discharging, and standing at a closed, dry and temperature of 10-25 ℃ to obtain a component A.
(2) Sequentially adding phthalic anhydride and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B.
(3) 100g of the component A obtained in the step (1) and 100g of the component B obtained in the step (2) were uniformly mixed, and after vacuum defoaming, the viscosity and thixotropic index were measured at 25 ℃. The results are shown in Table 1.
Example 3
The low-viscosity high-thixotropy epoxy resin sealant is prepared by mixing a component A and a component B;
wherein the component A comprises the following components in percentage by weight: 80% of bisphenol A type epoxy resin E51, 15% of phenyl glycidyl ether, 0.5% of defoaming agent 6201, 0.5% of fumed silica, 1% of polyamide wax, 1% of polysulfide rubber and 2% of carboxyl-terminated liquid nitrile rubber;
the component B comprises the following components in percentage by weight: 95% polytetrahydrofthalic anhydride, 1.5% triethanolamine, 3.5% benzoyl peroxide;
the preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin E51, phenyl glycidyl ether and a defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at a rotation speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at a rotation speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component A.
(2) Sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, discharging after vacuumizing, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B.
(3) 100g of the component A obtained in the step (1) and 100g of the component B obtained in the step (2) were uniformly mixed, and after vacuum defoaming, the viscosity and thixotropic index were measured at 25 ℃. The results are shown in Table 1.
TABLE 1
| Test items | Unit of | Example 1 | Example 2 | Example 3 |
| Viscosity of the oil | mPa·s | 2500 | 2000 | 1900 |
| Thixotropic index | 1.20 | 1.22 | 1.25 |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. The low-viscosity high-thixotropy epoxy resin sealant is characterized in that: the weight ratio of 1: 1, mixing the component A and the component B;
the component A is prepared from the following components in percentage by weight: bisphenol A epoxy resin E5180%, phenyl glycidyl ether 15%, defoaming agent 62010.5%, fumed silica 0.5%, polyamide wax 1%, polysulfide rubber 1%, and carboxyl-terminated liquid nitrile rubber 2%;
the component B is prepared from the following components in percentage by weight: 95% of polytetrahydrofthalic anhydride, 1.5% of triethanolamine and 3.5% of benzoyl peroxide;
the preparation method of the low-viscosity high-thixotropy epoxy resin sealant comprises the following steps:
(1) adding bisphenol A type epoxy resin E51, phenyl glycidyl ether and a defoaming agent 6201 into a three-neck flask at one time, heating to 60 ℃, mixing and stirring for 30min at a rotation speed of 400rpm, adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at a rotation speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component A;
(2) sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B;
(3) and (3) uniformly mixing the component A in the step (1) and the component B in the step (2) to prepare the low-viscosity high-thixotropy epoxy resin sealant.
2. The method of preparing a low viscosity highly thixotropic epoxy resin sealant according to claim 1, comprising the steps of:
(1) sequentially adding bisphenol A type epoxy resin E51, phenyl glycidyl ether and an antifoaming agent 6201 into a three-neck flask, heating to 60 ℃, mixing and stirring for 30min at the rotating speed of 400rpm, then adding fumed silica, polyamide wax, polysulfide rubber and carboxyl-terminated liquid nitrile rubber, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component A;
(2) sequentially adding polytetrahydrofthalic anhydride, triethanolamine and benzoyl peroxide into a three-neck flask, mixing and stirring for 30min at the rotating speed of 400rpm, vacuumizing, discharging, and standing in a closed, dry and 10-25 ℃ environment to obtain a component B;
(3) and (3) uniformly mixing the component A in the step (1) and the component B in the step (2) to prepare the low-viscosity high-thixotropy epoxy resin sealant.
3. Use of the low viscosity high thixotropic epoxy resin sealant according to claim 1 or the low viscosity high thixotropic epoxy resin sealant prepared by the preparation method according to claim 2 for sealing electronic materials at high temperature.
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| CN201910645563.9A CN110467895A (en) | 2019-07-17 | 2019-07-17 | A kind of low viscosity high thixotropic epoxy resin sealant and preparation method thereof |
| CN202210572115.2A CN114854350A (en) | 2019-07-17 | 2019-07-17 | Low-viscosity high-thixotropy epoxy resin sealant and preparation method and application thereof |
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| CN110845979B (en) * | 2019-11-20 | 2021-12-03 | 北京市建筑工程研究院有限责任公司 | Modified delayed coagulation binder and preparation method thereof |
| CN111100588A (en) * | 2020-01-03 | 2020-05-05 | 鹤山市欧克特电子科技有限公司 | Insulating flame-retardant potting mixture and preparation method thereof |
| CN113604180B (en) * | 2021-08-11 | 2023-03-21 | 北京华腾新材料股份有限公司 | Low-temperature-resistant high-thixotropy epoxy daub and preparation method thereof |
| CN113501936A (en) * | 2021-08-13 | 2021-10-15 | 中国科学院兰州化学物理研究所 | Modified curing agent for epoxy resin and preparation method thereof |
| CN117304855B (en) * | 2023-10-31 | 2024-04-12 | 上海巨传电子有限公司 | Epoxy adhesive for reinforcing BGA welding column and preparation method thereof |
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| CN109628039A (en) * | 2018-12-28 | 2019-04-16 | 深圳德邦界面材料有限公司 | A kind of epoxy resin flexibility heat conduction adhesive and preparation method thereof |
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| US20090255438A1 (en) * | 2008-04-15 | 2009-10-15 | David Christopher Graham | Thermally curable encapsulant composition for inkjet print cartridge |
| US8657413B2 (en) * | 2011-01-18 | 2014-02-25 | Funai Electric Co., Ltd. | Die attach composition for silicon chip placement on a flat substrate having improved thixotropic properties |
| CN103555245B (en) * | 2013-11-18 | 2015-01-14 | 湖南固特邦土木技术发展有限公司 | Epoxy adhesive for repairing and reinforcing hinge joint and application of epoxy adhesive |
| CN105936815B (en) * | 2016-06-08 | 2018-11-30 | 天津德高化成光电科技有限责任公司 | Thixotropic epoxy, preparation method and in LED chip package application |
| CN106833470A (en) * | 2017-02-24 | 2017-06-13 | 厦门安耐伟业新材料有限公司 | Fluid sealant and preparation method thereof, application method |
| CN107722897A (en) * | 2017-10-25 | 2018-02-23 | 杭州之江新材料有限公司 | A kind of epoxy joint trimming agent and preparation method thereof |
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| CN109628039A (en) * | 2018-12-28 | 2019-04-16 | 深圳德邦界面材料有限公司 | A kind of epoxy resin flexibility heat conduction adhesive and preparation method thereof |
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