CN114507496A - Two-component epoxy resin encapsulating adhesive - Google Patents
Two-component epoxy resin encapsulating adhesive Download PDFInfo
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- CN114507496A CN114507496A CN202210228805.6A CN202210228805A CN114507496A CN 114507496 A CN114507496 A CN 114507496A CN 202210228805 A CN202210228805 A CN 202210228805A CN 114507496 A CN114507496 A CN 114507496A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
- C08G59/1455—Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/688—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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
- C09J187/00—Adhesives based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09J187/005—Block or graft polymers not provided for in groups C09J101/00 - C09J185/04
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses a two-component epoxy resin encapsulating adhesive, which innovatively adopts specific modified epoxy resin as a resin matrix and combines with a specific modified curing accelerator, the two components of the epoxy resin encapsulating adhesive have combined action, the defects of poor rheological stability, short service life and the like of a system are obviously overcome, other mechanical properties and electrical properties are not influenced, the problems of the two-component epoxy encapsulating adhesive in the prior art are solved, the two-component epoxy resin encapsulating adhesive is favorably applied to a motor, and the reliability of a connecting part (a rotor neck) of a rotor neck commutator and a winding in the motor, especially the motor is ensured.
Description
The invention relates to a split application of Chinese patent application, which has an application date of 2020, 12 and 15 months and an application number of 2020114840927 and is named as 'two-component epoxy resin encapsulating adhesive and a preparation method and application thereof'.
Technical Field
The invention belongs to the technical field of electronic sealants, and particularly relates to a two-component epoxy resin encapsulating adhesive.
Background
The service life of the motor is influenced due to severe working conditions such as high rotating speed, high vibration, high load and the like when the motor works, so that strict requirements are imposed on the motor, particularly a rotor structure which runs at a high speed; the connection part (rotor neck) of the rotor neck commutator and the winding is a weak link of the whole motor, and the part is usually fixed by adhesive in the industry, so that the shock resistance and the disconnection resistance of the motor are improved, and the reliability of the whole motor is improved.
The prior two-component epoxy encapsulating adhesive generally has the following problems that firstly, the rheological stability of the encapsulating adhesive in the prior art is insufficient, rheological additives of the prior encapsulating adhesive product comprise fumed silica, modified fumed silica, organic bentonite, polyamide and the like, the rheological additives achieve the aim of controlling the system rheology by a hydrogen bond binding mechanism, the structure has limited effect in polar resin of epoxy resin, the rheological property of the adhesive is continuously changed in the processes of storage, transportation and use of the product, the problem of insufficient hanging adhesive and the problem of flowing are often caused, and the product is often required to be reworked; secondly, the working life is too short, the working life is only 1-2 hours after the two components are mixed, the rheological stability becomes poor after the working life is too long, the phenomena of insufficient coating, flowing and the like are caused, the encapsulating glue is seriously wasted, the production efficiency is seriously influenced, and the whole motor is often scrapped because the glue flows into the groove of the commutator.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an improved two-component epoxy resin encapsulating adhesive which has excellent rheological stability, viscosity stability and longer service life.
In order to solve the technical problems, the invention adopts the following technical scheme:
a two-component epoxy resin encapsulating adhesive comprises a component A and a component B, wherein the component A comprises an epoxy resin matrix, a first thixotropic agent and a filler, the component B comprises an anhydride curing agent and a curing accelerator, the epoxy resin matrix is modified epoxy resin, the modified epoxy resin is prepared by the reaction of an oil-soluble nonionic surfactant and the epoxy resin, and the oil-soluble nonionic surfactant is sorbitan fatty acid ester and/or castor oil polyoxyethylene ether; the curing accelerator is a modified curing accelerator, and the modified curing accelerator is prepared by reacting fatty alcohol-polyoxyethylene ether phosphate with an amine curing accelerator.
According to some preferred aspects of the present invention, the feeding mass ratio of the oil-soluble nonionic surfactant to the epoxy resin in the preparation of the modified epoxy resin is 1: 6-12. Further preferably, in the process of preparing the modified epoxy resin, the feeding mass ratio of the oil-soluble nonionic surfactant to the epoxy resin is 1: 8-12.
According to some preferred aspects of the present invention, the modified epoxy resin is prepared by reacting an oil-soluble nonionic surfactant with an epoxy resin at 200-220 ℃.
According to some preferred aspects of the invention, the sorbitan fatty acid ester is a combination of one or more selected from span-20, span-60 and span-80.
According to some preferred aspects of the present invention, the castor oil polyoxyethylene ether is a combination of one or more selected from the group consisting of EL-10, EL-20, EL-30, and EL-40.
According to some preferred aspects of the invention, the epoxy resin is a bisphenol a type liquid epoxy resin, such as E54 bisphenol a epoxy resin, E51 bisphenol a epoxy resin, E44 bisphenol a epoxy resin, and the like.
According to some preferred aspects of the present invention, the amine-based curing accelerator is a combination of one or more selected from the group consisting of N, N-dimethylbenzylamine, 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30), imidazole, dimethylcyclohexylamine, and triethanolamine.
According to some preferred aspects of the invention, in the preparation process of the modified curing accelerator, the feeding mass ratio of the fatty alcohol-polyoxyethylene ether phosphate to the amine curing accelerator is 0.2-2.5: 1. Further preferably, in the process of preparing the modified curing accelerator, the feeding mass ratio of the fatty alcohol-polyoxyethylene ether phosphate to the amine curing accelerator is 0.5-2: 1. Still more preferably, in the process of preparing the modified curing accelerator, the feeding mass ratio of the fatty alcohol-polyoxyethylene ether phosphate to the amine curing accelerator is 1-2: 1.
According to some preferred aspects of the present invention, the modified curing accelerator is prepared by reacting a fatty alcohol-polyoxyethylene ether phosphate with an amine-based curing accelerator at 90 to 110 ℃.
According to some preferred and specific aspects of the present invention, the a component further comprises a first rheology aid, a first defoamer, and the b component further comprises a second thixotropic agent, a second rheology aid, and a second defoamer.
According to some preferred and specific aspects of the present invention, the a component comprises, in mass percent: 60-90% of modified epoxy resin, 0.2-4% of first thixotropic agent, 8-40% of filler, 0.2-2% of first rheological additive and 0.05-0.2% of first defoaming agent;
the component B comprises the following components in percentage by mass: 90-99% of anhydride curing agent, 0.2-4% of modified curing accelerator, 0.2-4% of second thixotropic agent, 0.2-2% of second flow transformation assistant and 0.02-0.2% of second defoaming agent;
in the two-component epoxy resin encapsulating glue, the feeding mass ratio of the component A to the component B is 1-5: 1.
According to some preferred aspects of the present invention, the first thixotropic agent and the second thixotropic agent are fumed silica, respectively, which can contribute better to the electrical properties of the system than other thixotropic agents.
According to some preferred aspects of the invention, the first rheology aid and the second rheology aid are BEZ75 and/or BYK-3560, respectively.
According to some preferred aspects of the present invention, the first and second defoamers are each a fluorocarbon defoamer, and can be, for example, Qingtian DH-2020, DH-2022.
According to some preferred aspects of the invention, the filler is a combination of one or more selected from the group consisting of white carbon, talc, calcium carbonate, barium sulfate and wollastonite. Furthermore, the white carbon black is precipitated white carbon black, the fineness of the talcum powder is 1250-.
According to some preferred aspects of the present invention, the anhydride curing agent is a combination of one or more selected from the group consisting of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, elaeostearic anhydride, cyclopentadiene and maleic anhydride, glycerol trimellitate, polyazelaic anhydride, chlorendic anhydride and pyromellitic dianhydride.
The invention provides another technical scheme that: the preparation method of the two-component epoxy resin encapsulating adhesive comprises the following steps:
preparation of the component A: reacting oil-soluble nonionic surfactant with epoxy resin at the temperature of 200-220 ℃ to prepare modified epoxy resin, adding a first thixotropic agent and a filler, stirring, adding a selective first rheological additive and a first defoaming agent, and uniformly mixing to prepare the modified epoxy resin;
preparation of the component B: fatty alcohol-polyoxyethylene ether phosphate and amine curing accelerator react at 90-110 ℃ to prepare modified curing accelerator, and then the rest of the component B is added and mixed uniformly to prepare the modified curing accelerator.
According to some preferred aspects of the present invention, the modified epoxy resin is prepared by: heating part of epoxy resin, heating to 200-220 ℃, adding an oil-soluble nonionic surfactant, mixing, reacting, then adding the rest epoxy resin, and continuing to perform heat preservation reaction to obtain the epoxy resin.
The invention provides another technical scheme that: the application of the two-component epoxy resin encapsulating adhesive in a motor.
When the two-component epoxy resin encapsulating adhesive is used, the A component and the B component are mixed according to a set proportion and then can be used; one of the problems in the prior art is that after two components are mixed, the working life is only 1-2 hours, and then the rheological stability becomes poor, so that the phenomena of insufficient coating, flowing and the like are caused, the coating glue waste is serious, the production efficiency is seriously influenced, and the whole motor is often scrapped because the glue flows into a commutator groove; after the two components are mixed, the pot life of the two-component epoxy resin encapsulating adhesive can be greatly prolonged to more than 10 hours, and the problems of unstable rheological property, easy generation of insufficient adhesive hanging, flowing and the like in the prior art can be solved.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
the two-component epoxy resin encapsulating adhesive disclosed by the invention innovatively adopts specific modified epoxy resin as a resin matrix and is combined with a specific modified curing accelerator, so that the service life is greatly prolonged, the rheological stability and the viscosity stability of the encapsulating adhesive are excellent, and other mechanical properties and electrical properties are not influenced; specifically, according to the invention, the modified epoxy resin is subjected to graft modification by adopting a specific oil-soluble nonionic surfactant, so that a nonpolar long carbon chain is introduced, the epoxy resin has better rheological stability under the action of the nonpolar long carbon chain and the thixotropic agent, and the overall viscosity stability and rheological stability of the epoxy resin are further improved by slight crosslinking during graft modification; the amine curing accelerator is modified by the fatty alcohol-polyoxyethylene ether phosphate, so that the reaction speed of the system at low temperature is reduced, the modified epoxy resin is combined, the combined action of the fatty alcohol-polyoxyethylene ether phosphate and the modified epoxy resin obviously overcomes the defects of poor rheological stability, short service life and the like of the system, the problem of the two-component epoxy encapsulating adhesive in the prior art is solved, the two-component epoxy encapsulating adhesive is favorably applied to a motor, and the reliability of the motor, particularly the reliability of a connecting part (the rotor neck) of a rotor neck commutator and a winding in the motor is ensured.
Drawings
FIG. 1 is a schematic diagram of a testing apparatus used in a pot life test according to an embodiment of the present invention;
wherein, 1, a water bath; 2. a peristaltic pump; 3. an oven; 4. a latex tube; 5. a rotor; 6. and a speed reducer.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these examples are for the purpose of illustrating the general principles, essential features and advantages of the present invention, and the present invention is not limited by the following examples. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments. The raw materials used in the examples are all commercially available commercial products. In the following examples, all starting materials are essentially obtained commercially or prepared by conventional methods in the art, unless otherwise specified.
In the examples described below, E54 bisphenol A epoxy resin was purchased from Nantong star; e51 bisphenol A epoxy resin was purchased from Nantong star; e44 bisphenol A epoxy resin was purchased from Nantong star; span-20, span-60 and span-80 are all purchased from Zhejiang amanta chemical industry, castor oil polyoxyethylene ether EL-10, EL-20, EL-30 and EL-40 are all purchased from Jiangsu Haian national force chemical industry, fatty alcohol polyoxyethylene ether (3) phosphate is purchased from Jiangsu Haian petrochemical industry, methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride are purchased from Jiaxing south Wanxing chemical engineering Limited company, tung oil anhydride is purchased from Shandong Jiaying chemical engineering Limited company, maleic anhydride is purchased from Jinhao chemical industry, N, N-dimethylbenzylamine is purchased from Hezhou Huayang technology, gas-phase silicon dioxide is purchased from Hubei Hufu nanometer material, wollastonite is purchased from Jiangxi Huajie Tai mineral fiber technology Limited company, talcum powder is purchased from Hezhou Roo chemical engineering Limited company, rheological additive is BEZ75 (purchased from Dede new material), the defoaming agent is a green field DH-2020 fluorocarbon defoaming agent.
Example 1
The embodiment provides a two-component epoxy resin encapsulating glue which comprises a component A and a component B.
Wherein, the raw materials of the component A comprise 40 kg of E54 bisphenol A epoxy resin, 40 kg of E51 bisphenol A epoxy resin, 4 kg of span-80, 4 kg of EL-10, 1 kg of fumed silica, 18.5 kg of wollastonite, 0.5 kg of rheological additive and 0.1 kg of defoaming agent;
the raw materials of the component B comprise 48 kg of methyl tetrahydrophthalic anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator, 0.2 kg of rheological additive and 25g of defoaming agent.
The preparation method of the two-component epoxy resin encapsulating adhesive comprises the following steps:
preparation of the component A:
preparation of modified epoxy resin: heating 20 kg of E54 bisphenol A epoxy resin and 20 kg of E51 bisphenol A epoxy resin, heating to 210 +/-5 ℃, adding 4 kg of span-80 and 4 kg of EL-10, and uniformly stirring; keeping the temperature of the system at 210 +/-5 ℃ for reaction for 60min, and then adding the rest epoxy resin; keeping the temperature of the system at 210 +/-5 ℃, and continuing to react for 60min to obtain modified epoxy resin;
cooling the prepared modified epoxy resin to below 50 ℃ by introducing cooling water, and adding metered fumed silica and wollastonite into the modified epoxy resin for five times under the condition of high-speed dispersion; continuing dispersing at high speed for 60min after adding; adding rheological additive and defoaming agent, and dispersing at low speed for 30min to obtain encapsulating gel A component.
Preparation of the component B:
preparation of modified curing accelerator: uniformly mixing N, N-dimethylbenzylamine and fatty alcohol-polyoxyethylene ether (3) phosphate according to the mass ratio of 1:1, heating to 100 ℃, and reacting for 60min under the condition of stirring to obtain a modified curing accelerator;
and (3) uniformly mixing 48 kg of methyl tetrahydrophthalic anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator prepared by the method, 0.2 kg of rheological additive and 25g of defoaming agent, and stirring at a high speed for 30min to obtain the component B of the encapsulating adhesive.
Example 2
The embodiment provides a two-component epoxy resin encapsulating glue which comprises a component A and a component B.
Wherein, the raw materials of the component A comprise 80 kg of E54 bisphenol A epoxy resin, 4 kg of EL-10, 4 kg of EL-20, 1 kg of fumed silica, 18.5 kg of wollastonite, 0.5 kg of rheological additive and 0.1 kg of defoaming agent;
the raw materials of the component B comprise 48 kg of methyl hexahydrophthalic anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator, 0.2 kg of rheological additive and 25g of defoaming agent.
The preparation method of the two-component epoxy resin encapsulating adhesive comprises the following steps:
preparation of the component A:
preparation of modified epoxy resin: heating 40 kg of E54 bisphenol A epoxy resin, heating to 210 +/-5 ℃, adding 4 kg of EL-10 and 4 kg of EL-20, and uniformly stirring; keeping the temperature of the system at 210 +/-5 ℃ for reaction for 60min, and then adding the rest epoxy resin; keeping the temperature of the system at 210 +/-5 ℃, and continuing to react for 60min to obtain modified epoxy resin;
cooling the prepared modified epoxy resin to below 50 ℃ by introducing cooling water, and adding metered fumed silica and wollastonite into the modified epoxy resin for five times under the condition of high-speed dispersion; continuing dispersing at high speed for 60min after adding; adding rheological additive and defoaming agent, and dispersing at low speed for 30min to obtain encapsulating gel A component.
Preparation of the component B:
preparation of modified curing accelerator: uniformly mixing N, N-dimethylbenzylamine and fatty alcohol-polyoxyethylene ether (3) phosphate according to the mass ratio of 1:1, heating to 100 ℃, and reacting for 60min under the condition of stirring to obtain a modified curing accelerator;
and (3) uniformly mixing 48 kg of methyl hexahydrophthalic anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator prepared by the method, 0.2 kg of rheological additive and 25g of defoaming agent, and stirring at a high speed for 30min to obtain the component B of the encapsulating adhesive.
Example 3
The embodiment provides a two-component epoxy resin encapsulating glue which comprises a component A and a component B.
Wherein, the raw materials of the component A comprise 80 kg of E51 bisphenol A epoxy resin, 4 kg of span-80, 4 kg of span-20, 1 kg of fumed silica, 18.5 kg of wollastonite, 0.5 kg of rheological additive and 0.1 kg of defoaming agent;
the raw materials of the component B comprise 24 kg of methyl tetrahydrophthalic anhydride, 24 kg of tung oil anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator, 0.2 kg of rheological additive and 25g of defoamer.
The preparation method of the two-component epoxy resin encapsulating adhesive comprises the following steps:
preparation of the component A:
preparation of modified epoxy resin: heating 40 kg of E51 bisphenol A epoxy resin, heating to 210 +/-5 ℃, adding 4 kg of span-80 and 4 kg of span-20, and uniformly stirring; keeping the temperature of the system at 210 +/-5 ℃ for reaction for 60min, and then adding the rest epoxy resin; keeping the temperature of the system at 210 +/-5 ℃, and continuing to react for 60min to obtain modified epoxy resin;
cooling the prepared modified epoxy resin to below 50 ℃ by introducing cooling water, and adding metered fumed silica and wollastonite into the modified epoxy resin for five times under the condition of high-speed dispersion; continuing dispersing at high speed for 60min after adding; adding rheological additive and defoaming agent, and dispersing at low speed for 30min to obtain encapsulating gel A component.
Preparation of the component B:
preparation of modified curing accelerator: uniformly mixing 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) and fatty alcohol polyoxyethylene ether (3) phosphate according to a mass ratio of 4:5, heating to 100 ℃, and reacting for 60min under the condition of stirring to obtain a modified curing accelerator;
24 kg of methyl tetrahydrophthalic anhydride, 24 kg of tung oil anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator prepared by the method, 0.2 kg of rheological additive and 25g of defoamer are uniformly mixed and stirred at high speed for 30min to obtain the encapsulating adhesive component B.
Example 4
The embodiment provides a two-component epoxy resin encapsulating glue which comprises a component A and a component B.
Wherein, the raw materials of the component A comprise 20 kg of E51 bisphenol A epoxy resin, 60 kg of E44 bisphenol A epoxy resin, 4 kg of span-20, 4 kg of EL-40, 1 kg of fumed silica, 18.5 kg of wollastonite, 0.5 kg of rheological additive and 0.1 kg of defoaming agent;
the raw materials of the component B comprise 24 kg of methyl tetrahydrophthalic anhydride, 24 kg of tung oil anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator, 0.2 kg of rheological additive and 25g of defoamer.
The preparation method of the two-component epoxy resin encapsulating adhesive comprises the following steps:
preparation of the component A:
preparation of modified epoxy resin: heating 10 kg of E51 bisphenol A epoxy resin and 30 kg of E44 bisphenol A epoxy resin, heating to 210 +/-5 ℃, adding 4 kg of span-20 and 4 kg of EL-40, and uniformly stirring; keeping the temperature of the system at 210 +/-5 ℃ for reaction for 60min, and then adding the rest epoxy resin; keeping the temperature of the system at 210 +/-5 ℃, and continuing to react for 60min to obtain modified epoxy resin;
cooling the prepared modified epoxy resin to below 50 ℃ by introducing cooling water, and adding metered fumed silica and wollastonite into the modified epoxy resin for five times under the condition of high-speed dispersion; continuing dispersing at high speed for 60min after adding; adding rheological additive and defoaming agent, and dispersing at low speed for 30min to obtain encapsulating gel A component.
Preparation of the component B:
preparation of modified curing accelerator: uniformly mixing 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30) and fatty alcohol polyoxyethylene ether (3) phosphate according to a mass ratio of 4:5, heating to 100 ℃, and reacting for 60min under the condition of stirring to obtain a modified curing accelerator;
24 kg of methyl tetrahydrophthalic anhydride, 24 kg of tung oil anhydride, 0.2 kg of fumed silica, 0.2 kg of modified curing accelerator prepared by the method, 0.2 kg of rheological additive and 25g of defoamer are uniformly mixed and stirred at high speed for 30min to obtain the encapsulating adhesive component B.
Comparative example 1
Basically, the method is the same as the method of the embodiment 1, and the method only differs from the method in that: the component A does not modify the epoxy resin, and directly disperses the epoxy resin with other components at high speed; the component B is not used for modifying the curing accelerator, and is directly mixed with other components.
Comparative example 2
Basically, the method is the same as the method of the embodiment 1, and the method only differs from the method in that: the component A does not modify the epoxy resin, and directly disperses the epoxy resin with other components at high speed and uniformly.
Comparative example 3
Basically, the method is the same as the method of the embodiment 1, and the method only differs from the method in that: the component B does not modify the curing accelerator, and is directly mixed with other auxiliary agents.
Performance test
The two-component epoxy encapsulating adhesive prepared in the above examples 1 to 4 and comparative examples 1 to 3 were subjected to the following performance tests, and the specific results are shown in table 1.
TABLE 1
Description of the drawings: when performance tests are carried out, the mass ratio of the A component to the B component is 5: 4.
A. And (3) testing the pot life: the mixed encapsulating glue is put into a water bath 1 at the temperature of 45 ℃, then the rotor 5 (the rotor 5 is connected with a speed reducer 6) which is preheated (in an oven 3) is rubberized (the encapsulating glue is guided in through a latex tube 4) through a peristaltic pump 2, the preheating temperature of the rotor 3 is 130 ℃, the glue is rubberized once every half hour, the phenomena of thinning, flowing and the like of the glue are observed, and particularly, the phenomena of flowing into a commutator are noticed. If the phenomena of severe thinning and flowing occur and the liquid begins to flow into the groove of the commutator, the liquid can not be reused; the test apparatus used for the test is shown in FIG. 1.
B. Viscosity: and respectively putting the component A and the component B into a water bath at the temperature of 25 ℃, keeping the temperature for 2 hours, then mixing and stirring for 10 minutes, and testing by using a rotational viscometer at the uniform rotating speed of 8 r/min.
C. Color/softening point after curing: mixing the component A and the component B according to the mass ratio of 5:4, stirring uniformly, placing the mixture into an oven at 130 ℃, curing for 2 hours, observing the color after curing, and measuring the softening point by a DSC method.
D. Volume resistance/breakdown strength: mixing the component A and the component B according to the mass ratio of 5:4, stirring uniformly, placing the mixture into a mould, placing the mould into an oven at 130 ℃, curing for 2 hours to prepare a circular sheet with the thickness of 0.8-1.0mm and the diameter of 150mm, and then testing (the testing national standard is GB/T10064-2006).
E. Rheological properties: the rheological properties are expressed in terms of the thixotropic index, which is the ratio of the viscosities measured at 6r/min and 60r/min by a rotational viscometer.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The two-component epoxy resin encapsulating adhesive is characterized by comprising a component A and a component B, wherein:
the component A comprises modified epoxy resin, a first thixotropic agent and a filler, wherein the modified epoxy resin is prepared by the reaction of an oil-soluble nonionic surfactant and epoxy resin, and the oil-soluble nonionic surfactant is sorbitan fatty acid ester and/or castor oil polyoxyethylene ether;
the component B comprises an anhydride curing agent and a modified curing accelerator, wherein the modified curing accelerator is prepared by reacting fatty alcohol-polyoxyethylene ether phosphate with an amine curing accelerator;
the pot life of the double-component epoxy resin encapsulating adhesive is more than 10 hours.
2. The two-part epoxy encapsulating adhesive according to claim 1, wherein the pot life of the two-part epoxy encapsulating adhesive is 14-16 hours.
3. The two-component epoxy resin encapsulating adhesive according to claim 1, wherein the feeding mass ratio of the oil-soluble nonionic surfactant to the epoxy resin is 1: 6-12, and the feeding mass ratio of the fatty alcohol-polyoxyethylene ether phosphate to the amine curing accelerator is 0.2-2.5: 1.
4. The two-component epoxy resin encapsulating adhesive according to claim 3, wherein the feeding mass ratio of the oil-soluble nonionic surfactant to the epoxy resin is 1: 8-12, and the feeding mass ratio of the fatty alcohol-polyoxyethylene ether phosphate to the amine curing accelerator is 0.5-2: 1.
5. The two-component epoxy encapsulating adhesive according to claim 1, wherein the component A further comprises a first rheological additive and a first defoaming agent, the component B further comprises a second thixotropic agent, a second rheological additive and a second defoaming agent, the first thixotropic agent and the second thixotropic agent are fumed silica respectively, the first rheological additive and the second rheological additive are BEZ75 and/or BYK-3560 respectively, and the first defoaming agent and the second defoaming agent are fluorocarbon defoaming agents respectively.
6. The two-component epoxy resin encapsulating adhesive according to claim 5, wherein in the two-component epoxy resin encapsulating adhesive, the feeding mass ratio of the component A to the component B is controlled to be 1-5: 1;
in the component A, by mass percentage, 60-90% of modified epoxy resin, 0.2-4% of first thixotropic agent, 8-40% of filler, 0.2-2% of first rheological additive and 0.05-0.2% of first defoaming agent, wherein the sum of the contents of the components is 100%;
in the component B, by mass percentage, 90-99% of an anhydride curing agent, 0.2-4% of a modified curing accelerator, 0.2-4% of a second thixotropic agent, 0.2-2% of a second flow-change assistant and 0.02-0.2% of a second defoaming agent, and the sum of the contents of the components is 100%.
7. The two-component epoxy resin encapsulating adhesive according to claim 1, wherein the sorbitan fatty acid ester is one or more selected from span-20, span-60 and span-80, the castor oil polyoxyethylene ether is one or the combination of more of EL-10, EL-20, EL-30 and EL-40, and the oil-soluble nonionic surfactant is controlled to be at least two selected from span-20, span-60, span-80 EL-10, EL-20, EL-30 and EL-40, the epoxy resin is bisphenol A liquid epoxy resin, and the bisphenol A liquid epoxy resin is one or more of E54 bisphenol A epoxy resin, E51 bisphenol A epoxy resin and E44 bisphenol A epoxy resin;
the filler is one or a combination of more of white carbon black, talcum powder, calcium carbonate, barium sulfate and wollastonite; the white carbon black is precipitated white carbon black; the fineness of the talcum powder is 1250-2500 meshes; the calcium carbonate is light calcium carbonate with the fineness of 800-1500 meshes; the fineness of the barium sulfate is 3000-5000 meshes; the wollastonite is needle-shaped, and the mesh number is between 800 and 1500.
8. The two-component epoxy encapsulating adhesive according to claim 1, wherein the component A is prepared by the following method: heating part of epoxy resin, heating to 200-220 ℃, adding an oil-soluble nonionic surfactant, mixing, reacting at 200-220 ℃, adding the rest of epoxy resin, continuing to perform heat preservation reaction to prepare modified epoxy resin, then adding a first thixotropic agent and a filler, stirring, selectively adding a first rheological additive and a first defoaming agent, and uniformly mixing to prepare the modified epoxy resin.
9. The two-component epoxy resin encapsulating adhesive according to claim 1, wherein the acid anhydride curing agent is one or more selected from the group consisting of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and tung oil anhydride, and the amine curing accelerator is N, N-dimethylbenzylamine or 2,4, 6-tris (dimethylaminomethyl) phenol.
10. The two-component epoxy encapsulating adhesive according to claim 1, wherein the component B is prepared by the following method: fatty alcohol-polyoxyethylene ether phosphate and an amine curing accelerator react at 90-110 ℃ under the stirring condition to prepare a modified curing accelerator, and then the rest of the component B is added and mixed uniformly to prepare the modified curing accelerator.
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| CN102229701A (en) * | 2011-05-13 | 2011-11-02 | 湖南大学 | Non-ionic aqueous epoxy resin emulsion and its preparation method |
| CN102675890A (en) * | 2012-05-23 | 2012-09-19 | 长安大学 | Demulsifying slow breaking and quick setting modified emulsified asphalt by microwave heating and preparation method thereof |
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| JP2000169671A (en) * | 1998-12-07 | 2000-06-20 | Sumitomo Bakelite Co Ltd | Epoxy resin composition and semiconductor device |
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| CN105908511B (en) * | 2016-04-26 | 2018-03-30 | 北京化工大学 | A kind of preparation method of self-emulsification aqueous epoxy resin carbon fiber sizing agent |
| CN106749863B (en) * | 2016-11-23 | 2019-05-03 | 苏州联胜化学有限公司 | A kind of imitative reactive coating printing adhesive and preparation method thereof, application method |
| CN110105542B (en) * | 2019-05-20 | 2022-01-18 | 南京太化化工有限公司 | Amphiphilic oil-based modified bisphenol A epoxy resin surfactant and preparation method and application thereof |
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| CN102229701A (en) * | 2011-05-13 | 2011-11-02 | 湖南大学 | Non-ionic aqueous epoxy resin emulsion and its preparation method |
| CN102675890A (en) * | 2012-05-23 | 2012-09-19 | 长安大学 | Demulsifying slow breaking and quick setting modified emulsified asphalt by microwave heating and preparation method thereof |
| CN104262589A (en) * | 2014-09-05 | 2015-01-07 | 广州秀珀化工股份有限公司 | Nonionic self-emulsifying water-based epoxy curing agent with Gemini surfactant structure and preparation method thereof |
| JP2017014406A (en) * | 2015-07-01 | 2017-01-19 | 味の素株式会社 | Resin composition |
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