CN111303815A - High-thermal-conductivity epoxy pouring sealant and preparation method thereof - Google Patents
High-thermal-conductivity epoxy pouring sealant and preparation method thereof Download PDFInfo
- Publication number
- CN111303815A CN111303815A CN202010249546.6A CN202010249546A CN111303815A CN 111303815 A CN111303815 A CN 111303815A CN 202010249546 A CN202010249546 A CN 202010249546A CN 111303815 A CN111303815 A CN 111303815A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- epoxy
- terminated
- thermal conductivity
- thermal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- C09J11/02—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
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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
-
- 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
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
Abstract
The invention relates to a high-thermal-conductivity epoxy pouring sealant and a preparation method thereof, and particularly relates to a high-thermal-conductivity epoxy pouring sealant for a dry-type transformer and a preparation method thereof. The pouring sealant is a mixture consisting of bisphenol A diglycidyl ether epoxy resin, epoxy resin REDG-80 containing tert-butyl glycidyl ether, multifunctional glycidyl amine epoxy resin, an active toughening agent, a curing agent, a coupling agent and a heat-conducting inorganic filler in a mass ratio of 100: 5-10: 50-100: 1-5: 100-160. On the other hand, the invention also provides a preparation method of the high-thermal-conductivity epoxy pouring sealant. The preparation process provided by the invention is simple and environment-friendly, and the obtained product has excellent comprehensive performance, is very suitable for encapsulation of high-thermal-conductivity epoxy glue for dry-type transformers, and has good application prospect.
Description
Technical Field
The invention belongs to the field of high-thermal-conductivity electrical insulating materials, particularly relates to a high-thermal-conductivity epoxy pouring sealant and a preparation method thereof, and particularly relates to a high-thermal-conductivity epoxy pouring sealant for a dry-type transformer and a preparation method thereof.
Background
With the continuous development of economy in China, the demand of people on power consumption in work and life is ever increasing, and therefore the load borne by the transformer is also increasing. The encapsulated dry-type transformer plays an important role in the operation of a power grid as a type of transformer suitable for outdoor use. In the working process of the transformer, part of electric energy is converted into heat energy, and if the transformer cannot dissipate heat in time, circuit faults or transformer fire is easily caused. The thermal conductivity of the currently used dry-type transformer casting material is between 0.45 and 0.60W/(m.K) (the thermal conductivity of iron is 1046.67W/(m.K) under a standard state), and the thermal conductivity of the casting material is low, so that the heat dissipation efficiency of the whole transformer is low, and therefore, the improvement of the thermal conductivity of the casting glue for the dry-type transformer is a research target with practical value.
Since the structure of the epoxy resin contains a polar group and an epoxy group, the adhesive strength is good. The epoxy resin potting compound has the advantages of good dielectric property, heat resistance, corrosion resistance, mechanical property and the like, so that the epoxy resin potting compound is most widely used in the field of potting. The cured epoxy potting material has a better protection effect on the device against external impact, so that the overall performance of the device is optimized. Meanwhile, after the device is internally potted, the device is prevented from being in direct contact with air and moisture, and the waterproof and moistureproof performance of the device is improved. The insulating performance between the device and the line is also improved.
Relevant references and reports are as follows, the entire contents of these references being incorporated by reference into the present invention:
wanke, Yuxin Hai, Xuyonfen [ adhesive, 2013,34(02):63-65 ] reviewed the progress of the research on high temperature resistant epoxy adhesives.
Li Chengdei [ chemical industry, 2015,33(11):12-14 ] studied a new epoxy resin material for insulating encapsulation of electronic and electrical devices.
Dahlian [ electronic world, 2014(03):120-121] researches a new epoxy resin encapsulation process for improving the electrical performance of encapsulated electronic products.
Chiffon [ Harbin university of Physician 2011 academic thesis ] studied the preparation and performance of epoxy electronic potting materials.
Yan-Jun Wan, Wen-Hu Yang, Shu-Hui Yu, Rong Sun, Ching-Ping Wong, Wei-HsinLiao. [ compositions Science and Technology,2016,122.] are used for improving the dielectric property and the thermal stability of the epoxy composite material and researching the functionalization of the graphene covalent polymer.
Weiwenkang, Yu Xinhai, Li Yu Wan [ Chinese adhesive, 2019,28(05):18-20+30 ] developed a high-performance epoxy resin adhesive with excellent comprehensive performance.
Systematic studies on the preparation and performance characterization of epoxy matrix resins were performed by weiwenkang, yuxin hai [ chinese adhesives, 2019,28(02):12-15 ].
The boundary phoenix, Caizinglin, leaf pungent, Linshiyun, Yu Xinhai [ adhesive, 2019,40(05):92-95 ] uses carboxyl-terminated nitrile rubber to toughen and modify epoxy resin for research.
Wufeng, Yuxin Hai, Zhongxing Ping (adhesive 2016,37(05): 53-56.) studied to prepare a novel high temperature resistant two-component epoxy adhesive system.
Modification studies of epoxy resins with bismaleimide resins were carried out in Rozhou, Yu Xin Hai, Chen chiffon, Chen Ji Wei, Liu Wan chapter, Tangxing [ adhesive, 2015,36(12):56-59 ].
The preparation and the performance of the high-temperature-resistant epoxy potting compound are researched by yaona, Ligang and Lireamin [ thermosetting resin, 2014,29(04):31-33 ].
The preparation and performance of solvent-free high-temperature-resistant epoxy resin are researched by Tongmai, Yu Xinhai, Chen Jiwei, Liu Wan chapter and Tang Xin [ insulating materials, 2016,49(02):18-21+27 ].
Yu Xinhai, Xujie, Shenhaiping [ insulating materials, 2016,49(07):36-40 ] studied the performance of polyphenylene ether resin systems for copper clad laminates and composites thereof.
Guo Xiang, Yu Xin Hai, Liu Wan chapter [ adhesive, 2014,35(09):56-60 ] studied the high temperature epoxy adhesives and their curing kinetics.
The kinetics and properties of epoxy potting material curing reaction were studied, in the light of book-waiting, spamming, Zhao-novelty, and yellow jade silk-ups [ thermosetting resins, 2009,24(06):26-29 ].
Yu Xinhai, Chen chiffon, Chen Ji Wei, Liu Wan chapter, Tang Xin [ insulating material, 2016,49(01):25-28+33 ] studied the preparation of high temperature resistant epoxy resin and its curing kinetics.
A novel high-temperature-resistant polyimide modified epoxy adhesive system is developed from Yu Xinhai, Sun Mega [ insulating materials, 2017,50(10):6-9 ].
A novel high-temperature resistant solvent-free epoxy adhesive is developed from Yu Xinhai, Guo Xiang, Chengji Wei, Liu Wan chapter and Hubin [ adhesive, 2014,35(01):33-35+39 ].
The structural design and the performance of the epoxy resin-based high-thermal-conductivity micro-nano composite insulating material are researched by mamarii (Beijing university of transportation, academic paper of 2019).
Xudan (southwestern science and technology university, 2016 academic paper) researches the preparation and the performance of the high-filling-amount nano Al _2O _ 3/epoxy resin composite material.
Li junming, yu xin hai, luodaming [ insulating material, 2013,46(02):25-28+37 ] reviewed the application of thermally conductive fillers in insulating polymer materials.
Evergreen ai spring (Wuhan university, 2011 academic thesis]Spherical SiO for packaging silicon chip2The preparation process and the performance of the epoxy resin composite material are researched.
Disclosure of Invention
The invention provides a high-thermal-conductivity epoxy pouring sealant and a preparation method thereof, which are used for meeting the use requirements of a high-performance dry-type transformer. The preparation method is simple in preparation process, environment-friendly, and excellent in comprehensive performance of the obtained product, is very suitable for encapsulation of high-thermal-conductivity epoxy glue for dry transformers, and has good application prospects.
The high-thermal-conductivity epoxy pouring sealant is a mixture consisting of bisphenol A diglycidyl ether epoxy resin, tert-butyl glycidyl ether-containing epoxy resin REDG-80, multifunctional glycidyl amine epoxy resin, an active toughening agent, a curing agent, a coupling agent and a thermal-conductivity inorganic filler in a mass ratio of 100: 5-10: 50-100: 1-5: 100-160.
Wherein, the epoxy resin REDG-80 containing tert-butyl glycidyl ether is preferably the epoxy resin obtained by the ring-opening reaction and alkali liquor desalting ring-closing reaction of 2, 5-di-tert-butyl hydroquinone and epichlorohydrin.
Further, the multifunctional glycidyl amine type epoxy resin is selected from N, N, N ', N' -tetraglycidyl-2, 2-bis [4- (4-aminophenoxy) phenyl ] propane TGBAPP, N, N, N ', N' -tetraglycidyl-4, 4 '-diaminodiphenylmethane TGDDM, N, N, N', N '-tetraglycidyl-4, 4' -diaminodiphenylsulfone TGDDS, one or more of N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenyl ether TGDDE, N, N, N ', N ' -tetraglycidyl-1, 4-diaminobenzene TGPPDA and N, N, N ', N ' -tetraglycidyl-1, 3-diaminobenzene TGMPDA.
Further, the active toughening agent is selected from one or more of hydroxyl-terminated polyether sulfone, hydroxyl-terminated polyphenylene oxide, amino-terminated polyetherimide, anhydride-terminated polyetherimide, maleimide-terminated polyetherimide, carboxyl-containing polyetherimide, hydroxyl-containing polyetherimide, maleimide-containing side group polyetherimide, carboxyl-containing polyimide, hydroxyl-containing polyimide, polyether polyol, maleimide-containing side group polyimide, carboxyl-terminated nitrile rubber, hydroxyl-terminated nitrile rubber, amino-terminated nitrile rubber, random carboxyl nitrile rubber and amino polymethylsiloxane.
Furthermore, the coupling agent is selected from one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane and glycidoxypropyltriethoxysilane.
Further, the curing agent is selected from one or more of hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tung oil anhydride, 2-ethyl-4-methylimidazole, DMP-30, 3 '-dimethyl-4, 4' -diaminodicyclohexylmethane, isophorone diamine, LCA-30, DBU and pentaerythritol tetramercaptopropionate. Further, the heat-conducting inorganic filler is one or more of spherical silicon dioxide powder, boron nitride powder, aluminum oxide powder and silicon carbide powder.
More preferably, the particle size of the heat-conducting inorganic filler is 0.1 to 50 micrometers.
The invention also provides a preparation method of the high-thermal-conductivity epoxy pouring sealant, which comprises the following steps:
(1) stirring bisphenol A diglycidyl ether epoxy resin, epoxy resin REDG-80 containing tert-butyl glycidyl ether, polyfunctional glycidyl amine epoxy resin and an active toughening agent at the temperature of between 80 and 100 ℃ for 0.5 to 1 hour for reaction, adding part of coupling agent and part of heat-conducting inorganic filler, and stirring and mixing uniformly to obtain a component A;
(2) stirring and mixing the curing agent, the rest of the coupling agent and the rest of the heat-conducting inorganic filler uniformly at room temperature to obtain a component B;
(3) a, B, and stirring uniformly at 50-70 ℃ to obtain the high-thermal-conductivity epoxy pouring sealant.
In the above method, preferably, the part of the coupling agent and the part of the heat-conducting inorganic filler in step (1) are 50 to 80 percent of the coupling agent and 50 to 70 percent of the heat-conducting inorganic filler; more preferably, 55 to 80% by weight of the coupling agent and 56 to 70% by weight of the thermally conductive inorganic filler.
The third aspect of the invention also provides application of the high-thermal-conductivity epoxy pouring sealant in a high-performance dry-type transformer, in particular application in encapsulation of the high-thermal-conductivity epoxy glue for the dry-type transformer.
In the present invention, the epoxy value of the bisphenol A diglycidyl ether epoxy resin is preferably 0.12 to 0.58, and more preferably 0.44 to 0.51. The hydroxyl-terminated polyether sulfone, hydroxyl-terminated polyphenylene oxide and hydroxyl-terminated nitrile rubber in the invention refers to active functional group hydroxyl at two ends of a molecular chain.
For example, the "carboxyl-terminated nitrile rubber" refers to a nitrile rubber having carboxyl groups as reactive functional groups at both ends of the molecular chain.
Similarly, the "amino terminal group", "anhydride terminal group" and "maleimide terminal group" in the "amino terminal polyetherimide, anhydride terminal polyetherimide, maleimide terminal polyetherimide and amino terminal nitrile rubber" refer to the "amino group", "anhydride group" and "maleimide terminal group" as the reactive functional groups at both ends of the molecular chain, respectively.
The high-thermal-conductivity epoxy pouring sealant provided by the invention can meet the use requirements of a high-performance dry-type transformer, the preparation process of the high-thermal-conductivity epoxy pouring sealant provided by the invention is simple, the high-thermal-conductivity epoxy pouring sealant is environment-friendly, and the product system is a solvent-free system; in addition, the high-thermal-conductivity epoxy pouring sealant provided by the invention has excellent comprehensive performance, is very suitable for the encapsulation of high-thermal-conductivity epoxy glue for dry transformers, has wide application prospect, and is easy for large-scale production.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these embodiments are provided to illustrate the general principles, major features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments. 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 epoxy resin REDG-80 containing tert-butyl glycidyl ether used in the invention is obtained by performing ring-opening reaction and alkali liquor desalting and ring-closing reaction on 2, 5-di-tert-butyl hydroquinone and epichlorohydrin, and the epoxy resin can be obtained by commercial purchase (for example, purchased from Zhejiang Yinyun New materials Co., Ltd.) or synthesis by adopting a conventional method in the field.
Example 1
Adding 100 g of bisphenol A diglycidyl ether epoxy resin (epoxy value is 0.51), 5 g of epoxy resin REDG-80 containing tert-butyl glycidyl ether (Zhejiang Yiyun New materials Co., Ltd.), 10 g of N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenyl ether TGDDE and 5 g of carboxyl-terminated nitrile butadiene rubber active toughening agent into a reactor, stirring and reacting at 80 ℃ for 1 hour, adding 0.8 g of 3-aminopropyltrimethoxysilane coupling agent, 45 g of spherical silica powder and 25 g of heat-conducting inorganic filler of alumina powder, and stirring and mixing uniformly to obtain a component A;
stirring and mixing 40 g of methyl tetrahydrophthalic anhydride, 10 g of curing agent of 2-ethyl-4-methylimidazole, 0.2 g of 3-aminopropyltrimethoxysilane coupling agent, 15 g of spherical silicon dioxide powder and 15 g of alumina powder heat-conducting inorganic filler uniformly at room temperature to obtain a component B;
a, B components are mixed and stirred evenly at 50 ℃ to obtain the high-heat-conductivity epoxy potting adhesive for the dry type transformer, which is recorded as SJ 1.
Example 2
Adding 100 g of bisphenol A diglycidyl ether epoxy resin (epoxy value is 0.44), 8 g of epoxy resin REDG-80 containing tert-butyl glycidyl ether (Zhejiang Yiyun New materials Co., Ltd.), 5 g of N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenylmethane TGDDM, 1 g of carboxyl-terminated butadiene-acrylonitrile rubber and 6 g of polyether polyol active toughening agent into a reactor, stirring and reacting at 80 ℃ for 1 hour, adding 1 g of 3-aminopropyltriethoxysilane coupling agent, 50 g of spherical silica powder and 15 g of heat-conducting inorganic filler of aluminum nitride powder, and stirring and mixing uniformly to obtain a component A;
stirring and mixing uniformly 62 g of hexahydrophthalic anhydride, 8 g of curing agent of 2-ethyl-4-methylimidazole, 0.8 g of 3-aminopropyltriethoxysilane coupling agent, 25 g of spherical silicon dioxide powder and 25 g of aluminum nitride powder heat-conducting inorganic filler at room temperature to obtain a component B;
a, B components are mixed and stirred evenly at 60 ℃, and the high heat conduction epoxy potting adhesive for the dry type transformer is obtained and is recorded as SJ 2.
Example 3
Adding 100 g of bisphenol A diglycidyl ether epoxy resin (epoxy value is 0.51), 10 g of epoxy resin REDG-80 containing tert-butyl glycidyl ether (Zhejiang Yiyun New materials Co., Ltd.), 8 g of N, N, N ', N' -tetraglycidyl-1, 3-diaminobenzene TGMPDA and 10 g of carboxyl-terminated butadiene-acrylonitrile rubber active toughening agent into a reactor, stirring and reacting at 80 ℃ for 1 hour, adding 3 g of 3-aminopropyltrimethoxysilane coupling agent, 60 g of spherical silica powder and 40 g of heat-conducting inorganic filler of boron nitride powder, and stirring and mixing uniformly to obtain a component A;
stirring and mixing 95 g of methyl tetrahydrophthalic anhydride, 5 g of curing agent of 2-ethyl-4-methylimidazole, 2 g of 3-aminopropyltrimethoxysilane coupling agent, 45 g of spherical silicon dioxide powder and 15 g of boron nitride powder heat-conducting inorganic filler uniformly at room temperature to obtain a component B;
a, B components are mixed and stirred evenly at 70 ℃, and the high heat conduction epoxy potting adhesive for the dry type transformer is obtained and is recorded as SJ 3.
Example 4
SJ1, SJ2, SJ3 prepared in examples 1-3 were sampled according to the following performance test requirements and the curing process was: heating from room temperature to 100 ℃, keeping the temperature for reaction for 2 hours, continuing to heat to 150 ℃, keeping the temperature for reaction for 1 hour, continuing to heat to 180 ℃, keeping the temperature for reaction for 1.5 hours, and naturally cooling to room temperature to obtain the required test sample, wherein the specific performance test data are shown in table 1.
And (3) testing the heat conductivity coefficient: the thermal conductivity is carried out in accordance with ISO 8894-1. Pouring the packaging material into a die with the diameter of 110mm for curing, so that the surface of the packaging material is flat and bubble-free, testing the thermal conductivity coefficient of the packaging material by using a DRL-III thermal conductivity coefficient tester for three times, and taking an average value.
And (3) volume resistivity test: uniformly placing the packaging material in three circular molds with the diameter of 110mm, uniformly arranging the packaging material with the minimum thickness of 1mm, and naturally cooling and taking down the packaging material after solidification. The resistance was measured by using a ZC36 insulation resistance tester manufactured by Shanghai Anbiao electronics Co., Ltd, and the thickness of the sample was measured. According to the formula ρ v — R × S/h, h is the thickness of the sample (i.e., the distance between the two poles); s is the area of the electrode, and ρ v is in Ω · m.
And (3) dielectric loss test: a sample with the diameter of 110mm and the uniform minimum thickness of 1mm is placed on a clamp, and a dielectric test is carried out by using an S6000-H + type dielectric loss tester of Shanghai' an electronic Limited company, with the test voltage of 1 kV.
And (3) breakdown field strength test: and testing the breakdown field intensity of a sample with the diameter of 110mm, the uniformity and the minimum thickness of 1mm by using an HT-50C type breakdown voltage tester, measuring the thickness of the sample at the breakdown position, and calculating the breakdown field intensity of the unit material.
And (3) testing mechanical properties: three specimens with the specification of 100mm 10mm 4mm are prepared, and the bending strength of the material is tested by an M-4050 type microcomputer-controlled electronic universal testing machine of Shenzhen Ruigel instruments, wherein the bending strength is calculated by a formula P of 3FL/2AB2, wherein F is the ultimate load force, L is the distance between fulcrums, A is the width of the sample, and B is the thickness of the sample.
Moisture absorption test: pouring the packaging material into a 45mm 9mm mould for solidification, weighing the dry weight G1 after cooling, placing the packaging material in water at 100 ℃ for 1 hour, and quickly wiping the packaging material to weigh the wet weight G2. The water absorption was calculated from the formula W (%) ═ (G2-G1)/G1 × 100%.
The test results are shown in table 1.
Table 1: high thermal conductivity epoxy pouring sealant condensate performance data
Claims (10)
1. The high-thermal-conductivity epoxy pouring sealant is characterized by being a mixture consisting of bisphenol A diglycidyl ether epoxy resin, tert-butyl glycidyl ether-containing epoxy resin REDG-80, multifunctional glycidyl amine epoxy resin, an active toughening agent, a curing agent, a coupling agent and a thermal-conductivity inorganic filler in a mass ratio of 100: 5-10: 50-100: 1-5: 100-160.
2. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the epoxy resin REDG-80 containing tert-butyl glycidyl ether is an epoxy resin obtained by a ring-opening reaction and an alkali lye desalting ring-closing reaction of 2, 5-di-tert-butyl hydroquinone and epichlorohydrin.
3. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the multifunctional glycidyl amine type epoxy resin is selected from the group consisting of N, N, N ', N ' -tetraglycidyl-2, 2-bis [4- (4-aminophenoxy) phenyl ] propane TGBAPP, N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenylmethane TGDDM, N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenylsulfone TGDDS, N, N, N ', N ' -tetraglycidyl-4, 4 ' -diaminodiphenylether TGDDE, N, N, N ', N ' -tetraglycidyl-1, 4-diaminobenzene TGPPDA, N, N ', N ' -tetraglycidyl-1, one or more of 3-diaminobenzene TGMPDA.
4. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the active toughening agent is selected from one or more of hydroxyl-terminated polyethersulfone, hydroxyl-terminated polyphenylene oxide, amino-terminated polyetherimide, anhydride-terminated polyetherimide, maleimide-terminated polyetherimide, carboxyl-containing polyetherimide, hydroxyl-containing polyetherimide, maleimide-side group-containing polyetherimide, carboxyl-containing polyimide, hydroxyl-containing polyimide, polyether polyol, maleimide-side group-containing polyimide, carboxyl-terminated nitrile rubber, hydroxyl-terminated nitrile rubber, amino-terminated nitrile rubber, random carboxyl nitrile rubber and amino polymethylsiloxane.
5. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the coupling agent is one or more selected from the group consisting of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, and glycidoxypropyltriethoxysilane.
6. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the curing agent is one or more selected from hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tung oil anhydride, 2-ethyl-4-methylimidazole, DMP-30, 3 '-dimethyl-4, 4' -diaminodicyclohexylmethane, isophorone diamine, LCA-30, DBU, pentaerythritol tetramercaptopropionate.
7. The high thermal conductivity epoxy potting adhesive of claim 1, wherein the thermal conductivity inorganic filler is one or more selected from spherical silica powder, boron nitride powder, aluminum oxide powder and silicon carbide powder.
8. The high thermal conductivity epoxy potting adhesive as claimed in any one of claims 1 to 7, wherein the particle size of the thermal conductive inorganic filler is 0.1 to 50 μm.
9. The preparation method of the high-thermal-conductivity epoxy pouring sealant as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
(1) stirring bisphenol A diglycidyl ether epoxy resin, epoxy resin REDG-80 containing tert-butyl glycidyl ether, polyfunctional glycidyl amine epoxy resin and an active toughening agent at the temperature of between 80 and 100 ℃ for 0.5 to 1 hour, adding 50 to 80 percent of coupling agent and 50 to 70 percent of heat-conducting inorganic filler, and stirring and mixing uniformly to obtain a component A;
(2) stirring and mixing the curing agent, the rest of the coupling agent and the rest of the heat-conducting inorganic filler uniformly at room temperature to obtain a component B;
(3) a, B and stirring at 50-70 deg.C.
10. Use of the high thermal conductivity epoxy potting adhesive according to any one of claims 1 to 7 for potting a dry-type transformer.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010249546.6A CN111303815A (en) | 2020-04-01 | 2020-04-01 | High-thermal-conductivity epoxy pouring sealant and preparation method thereof |
PCT/CN2020/111052 WO2021196513A1 (en) | 2020-04-01 | 2020-08-25 | Highly thermally conductive epoxy pouring sealant and preparation method therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010249546.6A CN111303815A (en) | 2020-04-01 | 2020-04-01 | High-thermal-conductivity epoxy pouring sealant and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111303815A true CN111303815A (en) | 2020-06-19 |
Family
ID=71159090
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010249546.6A Pending CN111303815A (en) | 2020-04-01 | 2020-04-01 | High-thermal-conductivity epoxy pouring sealant and preparation method thereof |
Country Status (2)
Country | Link |
---|---|
CN (1) | CN111303815A (en) |
WO (1) | WO2021196513A1 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111925763A (en) * | 2020-07-17 | 2020-11-13 | 华中科技大学 | Anti-cracking epoxy pouring sealant with improved heat-conducting property |
WO2021196510A1 (en) * | 2020-03-31 | 2021-10-07 | 苏州巨峰电气绝缘***股份有限公司 | High thermal conductivity electrical insulation packaging material and preparation method therefor |
WO2021196513A1 (en) * | 2020-04-01 | 2021-10-07 | 苏州巨峰电气绝缘***股份有限公司 | Highly thermally conductive epoxy pouring sealant and preparation method therefor |
CN114853983A (en) * | 2022-05-23 | 2022-08-05 | 嘉兴南洋万事兴化工有限公司 | Toughening modified epoxy curing agent for dry-type transformer and preparation method thereof |
CN116554836A (en) * | 2023-05-22 | 2023-08-08 | 华宇新能源科技有限公司 | Lead-acid storage battery sealant and preparation method thereof |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113461901A (en) * | 2021-06-29 | 2021-10-01 | 深圳市金菱通达电子有限公司 | A cluster of telechelic active functional group compositions, methods of manufacture and uses thereof |
CN114395354B (en) * | 2022-01-25 | 2023-11-03 | 苏州英田电子科技有限公司 | Low-shrinkage epoxy structural adhesive |
CN115093818B (en) * | 2022-06-27 | 2023-08-11 | 浙江亦龙新材料有限公司 | Electronic grade adhesive and preparation method thereof |
CN115433533A (en) * | 2022-09-05 | 2022-12-06 | 烟台德邦科技股份有限公司 | Room-temperature fast-curing high-temperature-resistant chemical-corrosion-resistant epoxy industrial repairing agent |
CN115595113B (en) * | 2022-09-19 | 2023-11-17 | 湖北回天新材料股份有限公司 | Epoxy modified silicone joint adhesive and preparation method thereof |
JP2024048375A (en) * | 2022-09-27 | 2024-04-08 | ザ・グッドイヤー・タイヤ・アンド・ラバー・カンパニー | Coupling systems for silica-containing rubber compounds. |
CN115595104A (en) * | 2022-10-27 | 2023-01-13 | 佛山清立新材料科技有限公司(Cn) | Epoxy packaging adhesive and preparation method and application thereof |
CN115537162A (en) * | 2022-11-01 | 2022-12-30 | 上海科蓝柏新材料科技有限公司 | Heat-conducting epoxy pouring sealant suitable for heat-radiating copper pipe embedding process and preparation method thereof |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011026383A (en) * | 2009-07-22 | 2011-02-10 | Sony Chemical & Information Device Corp | Heat curing type thermally conductive adhesive composition |
CN101974302A (en) * | 2010-10-19 | 2011-02-16 | 烟台德邦电子材料有限公司 | Low-viscosity and high-heat conduction epoxy resin electronic potting adhesive |
CN101974208A (en) * | 2010-08-20 | 2011-02-16 | 广东生益科技股份有限公司 | High thermal conductivity resin composition and high thermal conductivity coated metal foil board manufactured by using same |
CN102260480A (en) * | 2011-07-13 | 2011-11-30 | 东华大学 | High-temperature-resistant modified epoxy resin adhesive and preparation method thereof |
CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
CN107163888A (en) * | 2017-07-07 | 2017-09-15 | 东莞市德聚胶接技术有限公司 | Epoxy resin embedding adhesive and preparation method thereof |
CN208789178U (en) * | 2018-07-05 | 2019-04-26 | 苏州巨峰电气绝缘***股份有限公司 | A kind of transformer insulating materials |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003213089A (en) * | 2002-01-28 | 2003-07-30 | Matsushita Electric Works Ltd | Epoxy resin composition for semiconductor sealing use and semiconductor device |
CN111303815A (en) * | 2020-04-01 | 2020-06-19 | 苏州巨峰电气绝缘***股份有限公司 | High-thermal-conductivity epoxy pouring sealant and preparation method thereof |
-
2020
- 2020-04-01 CN CN202010249546.6A patent/CN111303815A/en active Pending
- 2020-08-25 WO PCT/CN2020/111052 patent/WO2021196513A1/en active Application Filing
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011026383A (en) * | 2009-07-22 | 2011-02-10 | Sony Chemical & Information Device Corp | Heat curing type thermally conductive adhesive composition |
CN101974208A (en) * | 2010-08-20 | 2011-02-16 | 广东生益科技股份有限公司 | High thermal conductivity resin composition and high thermal conductivity coated metal foil board manufactured by using same |
CN101974302A (en) * | 2010-10-19 | 2011-02-16 | 烟台德邦电子材料有限公司 | Low-viscosity and high-heat conduction epoxy resin electronic potting adhesive |
CN102260480A (en) * | 2011-07-13 | 2011-11-30 | 东华大学 | High-temperature-resistant modified epoxy resin adhesive and preparation method thereof |
CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
CN107163888A (en) * | 2017-07-07 | 2017-09-15 | 东莞市德聚胶接技术有限公司 | Epoxy resin embedding adhesive and preparation method thereof |
CN208789178U (en) * | 2018-07-05 | 2019-04-26 | 苏州巨峰电气绝缘***股份有限公司 | A kind of transformer insulating materials |
Non-Patent Citations (4)
Title |
---|
倪礼忠 等: "《聚合物基复合材料》", 28 February 2007, 上海:华东理工大学出版社 * |
王德中 主编: "《环氧树脂生产与应用》", 30 June 2001, 北京:化学工业出版社 * |
高春林 等: "对苯二酚二缩水甘油醚的合成研究", 《精细与专用化学品》 * |
黄艳娜等: "高导热低黏度环氧树脂灌封胶 ", 《化学与黏合》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2021196510A1 (en) * | 2020-03-31 | 2021-10-07 | 苏州巨峰电气绝缘***股份有限公司 | High thermal conductivity electrical insulation packaging material and preparation method therefor |
WO2021196513A1 (en) * | 2020-04-01 | 2021-10-07 | 苏州巨峰电气绝缘***股份有限公司 | Highly thermally conductive epoxy pouring sealant and preparation method therefor |
CN111925763A (en) * | 2020-07-17 | 2020-11-13 | 华中科技大学 | Anti-cracking epoxy pouring sealant with improved heat-conducting property |
CN111925763B (en) * | 2020-07-17 | 2021-06-11 | 华中科技大学 | Anti-cracking epoxy pouring sealant with improved heat-conducting property |
CN114853983A (en) * | 2022-05-23 | 2022-08-05 | 嘉兴南洋万事兴化工有限公司 | Toughening modified epoxy curing agent for dry-type transformer and preparation method thereof |
CN116554836A (en) * | 2023-05-22 | 2023-08-08 | 华宇新能源科技有限公司 | Lead-acid storage battery sealant and preparation method thereof |
CN116554836B (en) * | 2023-05-22 | 2023-11-14 | 华宇新能源科技有限公司 | Lead-acid storage battery sealant and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
WO2021196513A1 (en) | 2021-10-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111303815A (en) | High-thermal-conductivity epoxy pouring sealant and preparation method thereof | |
CN111234752A (en) | High-thermal-conductivity electrical insulation packaging material and preparation method thereof | |
CN104293229B (en) | Conductive adhesive and preparation method thereof | |
CN102702743B (en) | High-toughness high-heat-conduction epoxy-imine resin system and preparation method and application thereof | |
KR20170046685A (en) | Composition for heat-dissipation members, heat-dissipation member, electronic device and heat-dissipation member production method | |
CN102212269B (en) | Insulative potting composite material with high thermal conductivity and preparation method thereof | |
CN102191002A (en) | High-humidity and high-temperature resisting single component epoxy adhesive and its preparation method | |
CN108997754A (en) | A kind of polyimides high-temperature dielectric composite membrane and preparation method thereof | |
KR20100113984A (en) | Thermal conductive adhesive | |
CN112300536A (en) | Heat-resistant composite dielectric with high dielectric and high heat conductivity | |
KR20180118740A (en) | COMPOSITION FOR LOWER THERMAL EXPRESSION MEMBER, LOWER THERMAL EXPRESSION MEMBER, ELECTRONIC APPARATUS | |
CN102391818A (en) | Insulated thermal conductive adhesive and preparation method thereof | |
CN112745792A (en) | Preparation method of high-strength weather-resistant pouring sealant | |
Vaganova et al. | Synthesis and characterization of epoxy-anhydride polymers modified by polyfluoroaromatic oligoimides | |
KR20180113625A (en) | Composition for heat radiation member, heat radiation member, electronic apparatus, method for manufacturing composition for heat radiation member, method for manufacturing heat radiation member | |
CN110358485A (en) | A kind of high-thermal-conductivity epoxy resin binder and its preparation method and application for low temperature | |
CN114103305B (en) | high-Tg high-heat-conductivity metal-based copper-clad plate and processing technology thereof | |
CN108297508B (en) | Heat conducting plate and preparation method and application thereof | |
CN114148048A (en) | High-heat-dissipation aluminum-based copper-clad plate and preparation method thereof | |
CN106084222B (en) | Intrinsical high thermal conductivity polyimides and preparation method containing polyacetylene chain structure | |
CN103756253B (en) | Low dielectric constant hollow carbon sphere/epoxy resin composite material and preparation method thereof | |
CN109627472A (en) | A kind of high tensile modulus of elasticity Kapton of high thermal conductivity and preparation method thereof | |
CN110184009A (en) | A kind of preparation method of epoxy resin-matrix thermal conductive insulation glue | |
Gao et al. | Curing kinetics, thermal, mechanical, and dielectric properties based on o‐cresol formaldehyde epoxy resin with polyhedral oligomeric (N‐aminoethyl‐γ‐amino propyl) silsesquioxane | |
CN110128821A (en) | A kind of high thermal conductivity low-k bismaleimide-triazine resin and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200619 |