CN110669317A - Preparation method of ternary epoxy resin heat-conducting composite material - Google Patents
Preparation method of ternary epoxy resin heat-conducting composite material Download PDFInfo
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- CN110669317A CN110669317A CN201911183231.XA CN201911183231A CN110669317A CN 110669317 A CN110669317 A CN 110669317A CN 201911183231 A CN201911183231 A CN 201911183231A CN 110669317 A CN110669317 A CN 110669317A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- 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
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- 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
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- 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
Abstract
The invention belongs to the field of polymer heat-conducting composite materials, and particularly relates to a preparation method of a ternary epoxy resin heat-conducting composite material. Adding epoxy resin into the third component according to the mass parts, blending the epoxy resin and the third component at the temperature 80-160 ℃ higher than the melting point of the third component until the epoxy resin is clear, and then adding a curing agent. And continuously blending for 8-15 minutes, adding a heat-conducting filler and other auxiliaries, continuously stirring for 5-15 minutes, transferring, vacuumizing and removing bubbles. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material. The third component is introduced in the process of preparing epoxy resin, so that the dispersion effect of the filler in the epoxy resin can be promoted, and the interface thermal resistance between the filler and the epoxy resin is reduced. Under the condition of the same addition amount, the prepared composite material has a higher thermal conductivity coefficient than that of the direct thermal conductive filler.
Description
Technical Field
The invention belongs to the field of polymer heat-conducting composite materials, and particularly relates to a preparation method of a ternary epoxy resin heat-conducting composite material.
Background
Traditional heat conduction material mainly uses metal and ceramic material as leading, however along with the development of science and technology, modern electronic equipment's energy density is bigger and bigger, and the structure is more and more complicated, and traditional heat conduction material is difficult to satisfy the heat dissipation demand of modern equipment in all sides. The polymer material is gradually replacing the traditional heat conduction material due to the characteristics of complex and changeable structure, various types, excellent processing performance and the like, and is applied to various industries. However, most of the pure polymer materials are not good thermal conductors, and the thermal conductivity of most of the polymer materials is low. Therefore, the preparation of the polymer composite material by adding the high thermal conductive filler is one of the most important means for improving the thermal conductivity of the polymer material. Common heat-conducting fillers are carbon materials (graphene and carbon nanotubes), ceramic materials (boron nitride and aluminum oxide), metal materials (copper and silver), and the like. The addition amount, type, dispersion state and arrangement behavior of the filler influence the heat conductivity of the composite material. In addition, different thermally conductive fillers will also affect other properties of the composite. For example, common nano-fillers may have a certain mechanical reinforcing effect on the composite material, some ceramic fillers such as boron nitride, alumina and silica may endow the composite material with electrical insulation, and conductive carbon materials and metal materials may improve the electrical conductivity of the composite material. Different fillers are selected in a targeted manner, and the prepared polymer composite material can meet the heat conduction creep of different occasions. However, the preparation of highly thermally conductive composite materials still faces some challenges, such as the interface problem between the filler and the polymer, and the dispersion and orientation problem of the filler.
Disclosure of Invention
The invention aims to provide a heat-conducting epoxy resin composite material, and when the epoxy resin composite material is prepared, a third component is introduced, so that the dispersion effect of a filler in epoxy resin is promoted, the interface incompatibility of filler particles in matrix resin is improved, the interface thermal resistance is reduced, the heat-conducting capacity of the composite material is improved, and the requirements of the application field of the high-heat-conducting epoxy resin composite material are met.
The invention also aims to provide a preparation method of the epoxy resin composite material.
In order to achieve the purpose, the invention provides the following technical scheme:
1) the composition comprises the following components in parts by mass:
the epoxy resin refers to one or a mixture of more of bisphenol A type, bisphenol F type and liquid crystal type epoxy resin in any proportion.
The curing agent refers to aliphatic amine, aromatic amine or acid anhydride.
The third component is polyethylene glycol, lauric acid, myristic acid, palmitic acid or stearic acid.
The heat-conducting filler is one or a mixture of more of boron nitride, graphene, nano graphite sheets, aluminum nitride and aluminum oxide in any proportion.
The other auxiliary agents are curing accelerator tertiary amine, imidazole and quaternary ammonium salt.
2) The preparation method comprises the following steps:
adding epoxy resin into the third component according to the mass parts, blending the epoxy resin and the third component at the temperature 80-160 ℃ higher than the melting point of the third component until the epoxy resin is clear, and then adding a curing agent. And continuously blending for 8-15 minutes, adding a heat-conducting filler and other auxiliaries, continuously stirring for 5-15 minutes, transferring, vacuumizing and removing bubbles. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
The blending refers to a method of stirring and blending in a solvent and then drying, or ball milling and blending by a ball mill. The diluent acetone or butanone can be added during blending.
The third component is introduced in the process of preparing epoxy resin, so that the dispersion effect of the filler in the epoxy resin can be promoted, and the interface thermal resistance between the filler and the epoxy resin is reduced. Under the condition of the same addition amount, the prepared composite material has a higher thermal conductivity coefficient than that of the direct thermal conductive filler.
Drawings
FIG. 1 is a comparison of the thermal conductivity of the epoxy resin composite prepared in example 1 with that of an epoxy resin composite prepared under the same conditions without blending a third component.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
30g of 3,3', 5' -tetramethylbiphenyl bisphenol diglycidyl ether is weighed, 70g of polyethylene glycol (Mn ═ 4000) is added, stirring is carried out at 110 ℃ until the mixture is clear and transparent, and then 8.4g of diaminodiphenylmethane is added. Stirring was continued for 10 minutes, 72g of boron nitride was added, stirring was continued for 12 minutes, and transfer and vacuum-pumping were performed to remove air bubbles. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
Example 2:
60g of 3,3', 5' -tetramethylbiphenyl bisphenol diglycidyl ether is weighed, 40g of polyethylene glycol (Mn 8000) is added, stirring is carried out at 105 ℃ until the mixture is clear and transparent, and then 16.8g of diaminodiphenylmethane is added. Stirring was continued for about 10 minutes, 72g of graphene was added, and ball milling was performed by a planetary ball mill for 15 minutes. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
Example 3:
60g of bisphenol F epoxy resin is weighed, 30g of polyethylene glycol (Mn ═ 4000) is added, stirring is carried out at 100 ℃ until the mixture is clear and transparent, then 16.8g of diaminodiphenylmethane is added, stirring is carried out for 15 minutes, 50g of boron nitride is added, and stirring is carried out for 10 minutes. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
Example 4:
60g of bisphenol A epoxy resin (E51) is weighed, 30g of polyethylene glycol (Mn ═ 4000) is added, stirring is carried out at 90 ℃ until the mixture is clear and transparent, 15g of diaminodiphenylmethane is added, stirring is continued for 10 minutes, 120g of a mixture of boron nitride and alumina (mass ratio, boron nitride: alumina ═ 5:1) is added, and ball milling is carried out by a planetary ball mill for 5 minutes. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
Example 5:
60g of bisphenol A epoxy resin (E51) is weighed, 20g of polyethylene glycol (Mn ═ 4000) is added, stirring is carried out at 90 ℃ until the mixture is clear and transparent, 50g of methyl tetrahydrophthalic anhydride and 50g of promoter DMP-301.5 g are added, stirring is carried out for about 10 minutes, 100g of a mixture of aluminum nitride and graphene (mass ratio, aluminum nitride: graphene ═ 1:4) is added, and stirring is carried out for 10 minutes. Pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of a ternary epoxy resin heat-conducting composite material is characterized by comprising the following steps:
1) the composition comprises the following components in parts by mass:
2) the preparation method comprises the following steps:
adding epoxy resin into the third component according to the mass parts, blending the epoxy resin and the third component at the temperature 80-160 ℃ higher than the melting point of the third component until the epoxy resin is clear, and then adding a curing agent; continuously blending for 8-15 minutes, adding a heat-conducting filler and other auxiliaries, continuously stirring for 5-15 minutes, transferring, vacuumizing and removing bubbles; pouring into a mould, curing and molding, and demoulding to prepare the high-thermal-conductivity epoxy composite material.
2. The method for preparing the ternary epoxy resin heat-conducting composite material as claimed in claim 1, wherein the epoxy resin is one or a mixture of bisphenol A type, bisphenol F type and liquid crystal type epoxy resin in any proportion.
3. The method for preparing the ternary epoxy resin heat-conducting composite material as claimed in claim 1, wherein the curing agent is aliphatic amine, aromatic amine or acid anhydride.
4. The method for preparing the ternary epoxy resin heat-conducting composite material as claimed in claim 1, wherein the third component is polyethylene glycol, lauric acid, myristic acid, palmitic acid or stearic acid.
5. The method for preparing a ternary epoxy resin heat-conducting composite material as claimed in claim 1, wherein the heat-conducting filler is one or a mixture of more of boron nitride, graphene, graphite nanoplatelets, aluminum nitride and aluminum oxide in any proportion.
6. The preparation method of the ternary epoxy resin heat-conducting composite material as claimed in claim 1, wherein the other auxiliary agents are curing accelerators tertiary amine, imidazoles and quaternary ammonium salt.
7. The method for preparing a ternary epoxy resin heat-conducting composite material according to claim 1, wherein the blending is performed by stirring and blending in a solvent, and then drying or ball milling and blending by a ball mill. The diluent acetone or butanone can be added during blending.
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| CN201911183231.XA CN110669317A (en) | 2019-11-27 | 2019-11-27 | Preparation method of ternary epoxy resin heat-conducting composite material |
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| CN201911183231.XA CN110669317A (en) | 2019-11-27 | 2019-11-27 | Preparation method of ternary epoxy resin heat-conducting composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402847A (en) * | 2021-06-29 | 2021-09-17 | 福建师范大学泉港石化研究院 | Low-filling high-thermal-conductivity polymer composite material and preparation method thereof |
| CN113583388A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学泉港石化研究院 | Heat-conducting epoxy resin composite material and preparation method thereof |
| CN115975607A (en) * | 2022-12-30 | 2023-04-18 | 蜂巢能源科技(无锡)有限公司 | Heat absorption composite material, heat absorption composite structure and preparation method thereof, and lithium ion battery unit |
| WO2023089326A1 (en) * | 2021-11-18 | 2023-05-25 | Senergy Innovations Limited | Conductive polymer composite |
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| CN101230256A (en) * | 2008-01-04 | 2008-07-30 | 华南理工大学 | Method for preparing polyethylene glycol and epoxy resin formed composite phase-change materials |
| US20140107256A1 (en) * | 2012-10-16 | 2014-04-17 | Guangdong Shengyi Sci. Tech Co., Ltd. | Thermoset resin composition and its use |
| CN108395182A (en) * | 2018-05-18 | 2018-08-14 | 湖北工业大学 | A kind of compound heat accumulation temperature control ecology base material and preparation method thereof |
-
2019
- 2019-11-27 CN CN201911183231.XA patent/CN110669317A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN101230256A (en) * | 2008-01-04 | 2008-07-30 | 华南理工大学 | Method for preparing polyethylene glycol and epoxy resin formed composite phase-change materials |
| US20140107256A1 (en) * | 2012-10-16 | 2014-04-17 | Guangdong Shengyi Sci. Tech Co., Ltd. | Thermoset resin composition and its use |
| CN108395182A (en) * | 2018-05-18 | 2018-08-14 | 湖北工业大学 | A kind of compound heat accumulation temperature control ecology base material and preparation method thereof |
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| 周文英等: "《导热高分子材料》", 30 April 2014, 国防工业出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402847A (en) * | 2021-06-29 | 2021-09-17 | 福建师范大学泉港石化研究院 | Low-filling high-thermal-conductivity polymer composite material and preparation method thereof |
| CN113583388A (en) * | 2021-06-29 | 2021-11-02 | 福建师范大学泉港石化研究院 | Heat-conducting epoxy resin composite material and preparation method thereof |
| WO2023089326A1 (en) * | 2021-11-18 | 2023-05-25 | Senergy Innovations Limited | Conductive polymer composite |
| CN115975607A (en) * | 2022-12-30 | 2023-04-18 | 蜂巢能源科技(无锡)有限公司 | Heat absorption composite material, heat absorption composite structure and preparation method thereof, and lithium ion battery unit |
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