CN113480830A - Method for preparing heat-conducting composite material by utilizing melamine formaldehyde foam - Google Patents
Method for preparing heat-conducting composite material by utilizing melamine formaldehyde foam Download PDFInfo
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- CN113480830A CN113480830A CN202110681814.6A CN202110681814A CN113480830A CN 113480830 A CN113480830 A CN 113480830A CN 202110681814 A CN202110681814 A CN 202110681814A CN 113480830 A CN113480830 A CN 113480830A
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- Prior art keywords
- melamine formaldehyde
- heat
- foam
- composite material
- formaldehyde foam
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 29
- 239000006260 foam Substances 0.000 title claims abstract description 29
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003822 epoxy resin Substances 0.000 claims abstract description 11
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 11
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical group CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 5
- CSHJJWDAZSZQBT-UHFFFAOYSA-N 7a-methyl-4,5-dihydro-3ah-2-benzofuran-1,3-dione Chemical group C1=CCCC2C(=O)OC(=O)C21C CSHJJWDAZSZQBT-UHFFFAOYSA-N 0.000 claims description 5
- 239000003570 air Substances 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 239000000945 filler Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 6
- 229920001940 conductive polymer Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Phenolic Resins Or Amino Resins (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a method for preparing a heat-conducting composite material by utilizing melamine formaldehyde foam, which utilizes the abundant micro-pore structure of the melamine formaldehyde foam to obtain a carbon foam structure material which is easy to prepare and low in cost after carbonizing the melamine formaldehyde foam; after the carbon foam is mixed with the epoxy resin, the carbon foam structure is used as a heat-conducting filler while the advantages of high mechanical strength and excellent processability of the matrix epoxy resin are maintained, and the heat-conducting composite material with better heat-conducting property is obtained. The method can also compress the three-dimensional network structure carbon foam obtained after high-temperature carbonization, improve the density of the carbon foam and obtain the material with better heat-conducting property. The preparation method is low in cost and simple and feasible in process flow, and the obtained composite material has the advantages of heat conductivity coefficient of 0.49-0.71W/(m.K), tensile strength of 28.81-53.91 MPa, elastic modulus of 97.2-241.2 MPa and excellent mechanical property.
Description
Technical Field
The invention relates to a method for preparing a heat-conducting composite material by utilizing melamine formaldehyde foam, belonging to the field of composite materials.
Background
With the continuous progress of electronic technology, various electronic devices are developed toward integration and miniaturization, the power density of the electronic devices is remarkably improved, the heat productivity of the electronic devices is improved, the temperature is increased, and the stability of the devices is threatened. In various electronic devices today, the polymer material accounts for a considerable proportion of the total material composition, so how to develop a polymer material with good thermal conductivity is of great significance.
The polymer material has various excellent performances, but has many defects, such as poor heat resistance, high price and the like, and in the field of heat conduction materials, the pure polymer material has small heat conduction coefficient and cannot be directly used as a heat conduction material. The polymer material is used as a substrate, and a proper inorganic filler is selected as a heat-conducting filler, so that the polymer material has good comprehensive properties of heat conduction, impact toughness, mechanical strength, excellent processability, low cost and the like, and becomes a heat-conducting polymer material with good heat-conducting property, and the polymer material can be widely applied to the fields of electricians, LED lighting, chemical heat exchangers and the like. The industrial demand of the high polymer heat conduction material is gradually increased, but the research on the high polymer heat conduction material is difficult to keep up with the industrial demand.
At present, most of the technical routes for improving the thermal conductivity of the polymer material are to fill the polymer material with a thermal conductive filler with a high thermal conductivity coefficient, including filling one or more types and shapes of fillers, but these methods are complex in preparation process, relatively high in cost of the filler, and can seriously affect other properties of the material. Therefore, research on the heat conductive polymer material is being intensively conducted so as to be better applied to industrial production.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a heat-conducting composite material by utilizing melamine formaldehyde foam.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a composite material by using melamine formaldehyde foam, comprising the following steps:
(1) the use density is 5 to 9kg/m3The melamine formaldehyde foam is cleaned by compressed air, impurities and dust on the surface are blown off, and the melamine formaldehyde foam is cut into the size of 3-10 cm multiplied by 3-5 cm multiplied by 1-2 cm;
(2) carbonizing the melamine formaldehyde foam treated in the step (1) in a nitrogen atmosphere to obtain three-dimensional network structure carbon foam;
(3) uniformly mixing epoxy resin, a curing agent and an accelerator to obtain a mixture; and (3) mixing the mixture with the three-dimensional network structure carbon foam obtained in the step (2) in a mold according to the weight ratio of 30-80: 1, mixing, placing in a vacuum drying oven, and soaking for 1 hour at 80 ℃ under vacuum; and after the impregnation is finished, curing at high temperature to obtain a composite material finished product.
The purity of the nitrogen is 99.999 percent, and the flow rate is 0.5L/min.
The temperature program during the carbonization treatment is set as follows: raising the temperature from room temperature to 400 ℃ at the speed of 5-10 ℃/min, preserving the heat for 30-60 min, raising the temperature from 400 ℃ to 700 ℃ at the speed of 5-10 ℃/min, and preserving the heat for 2 hours.
The curing agent is modified methyl tetrahydrophthalic anhydride, and the accelerator is 2-ethyl-4-methylimidazole.
The epoxy resin: curing agent: the weight ratio of the accelerator is 10: 8-9: 0.1.
the concrete method for curing is as follows: the mixture is placed at 80-120 ℃ for 2-4 hours, and then placed at 150-180 ℃ for 5-8 hours for curing.
And (2) further compressing the obtained carbon foam with the three-dimensional network structure, and compressing the thickness of the carbon foam to be half of the thickness of the carbonized carbon foam by using a flat pressing plate.
The invention has the beneficial effects that:
the invention provides a method for preparing a composite material by utilizing melamine formaldehyde foam, which is characterized in that rich micro-pore structures contained in the melamine formaldehyde foam are utilized and carbonized to obtain a carbon foam structural material which is easy to prepare and low in cost; after the carbon foam is mixed with the epoxy resin, the carbon foam structure is used as a heat-conducting filler while the advantages of high mechanical strength and excellent processability of the matrix epoxy resin are maintained, and the heat-conducting composite material with better heat-conducting property is obtained. The method can also compress the three-dimensional network structure carbon foam obtained after high-temperature carbonization, improve the density of the carbon foam and obtain the material with better heat-conducting property.
The preparation method is low in cost and simple and feasible in process flow, and the obtained composite material has the advantages of heat conductivity coefficient of 0.49-0.71W/(m.K), tensile strength of 28.81-53.91 MPa, elastic modulus of 97.2-241.2 MPa and excellent mechanical property.
Detailed Description
The following examples further illustrate the embodiments of the present invention in detail.
Example one
A method for preparing a composite material by using melamine formaldehyde foam, comprising the following steps:
(1) the used density is 5kg/m3The melamine foam (Sichuan super poly new material Co., Ltd.) is cleaned by compressed air, and after impurities and dust on the surface are blown off, the melamine foam is cut into the size of 10cm multiplied by 5cm multiplied by 1 cm;
(2) carbonizing the melamine formaldehyde foam treated in the step (1) in a nitrogen atmosphere with the purity of 99.999% and the flow of 0.5L/min, wherein the temperature program is as follows: heating from room temperature to 400 ℃ at the speed of 10 ℃/min, preserving heat for 60min, heating from 400 ℃ to 700 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and obtaining carbon foam with a three-dimensional network structure;
(3) epoxy resin JY-257 (epoxy value is 0.53-0.55 mol/100g), curing agent modified methyl tetrahydrophthalic anhydride and accelerator 2-ethyl-4-methylimidazole according to the weight ratio of 10: 9: 0.1, mixing uniformly to obtain a mixture; mixing the mixture and the three-dimensional network structure carbon foam obtained in the step (2) according to the weight ratio of 50: 1, uniformly mixing in a mould, placing in a vacuum drying oven, and soaking for 1 hour at 80 ℃ under vacuum. And then respectively placing the materials at 120 ℃ for 3 hours and 150 ℃ for 5 hours for curing, and obtaining a composite material finished product after curing.
The thermal conductivity coefficient of the obtained composite material is 0.49W/(m.K); the tensile strength was 53.91MPa, and the elastic modulus was 241.2 MPa.
Example two
A method for preparing a composite material by using melamine formaldehyde foam, comprising the following steps:
(1) the use density is 9kg/m3The melamine formaldehyde foam is cleaned by compressed air, impurities and dust on the surface are blown off, and the melamine formaldehyde foam is cut into the size of 3cm multiplied by 1 cm;
(2) carbonizing the melamine formaldehyde foam treated in the step (1) in a nitrogen atmosphere with the purity of 99.999% and the flow of 0.5L/min, wherein the temperature program is as follows: heating from room temperature to 400 ℃ at the speed of 5 ℃/min, preserving heat for 60min, heating from 400 ℃ to 700 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, and obtaining carbon foam with a three-dimensional network structure;
(3) epoxy resin JY-257, curing agent modified methyl tetrahydrophthalic anhydride and accelerator 2-ethyl-4-methylimidazole according to the weight ratio of 10: 9: 0.1, mixing uniformly to obtain a mixture; mixing the mixture and the three-dimensional network structure carbon foam obtained in the step (2) according to the weight ratio of 50: 1, uniformly mixing in a mould, placing in a vacuum drying oven, and soaking for 1 hour at 80 ℃ under vacuum. And then respectively placing the materials at 120 ℃ for 3 hours and 150 ℃ for 5 hours for curing, and obtaining a composite material finished product after curing.
The thermal conductivity coefficient of the obtained composite material is 0.68W/(m.K); the tensile strength was 36.34MPa, and the modulus of elasticity was 134.9 MPa.
EXAMPLE III
A method for preparing a composite material by using melamine formaldehyde foam, comprising the following steps:
(1) the used density is 5kg/m3The melamine formaldehyde foam is cleaned by compressed air, impurities and dust on the surface are blown off, and the melamine formaldehyde foam is cut into the size of 3cm multiplied by 2cm multiplied by the height;
(2) carbonizing the melamine formaldehyde foam treated in the step (1) in a nitrogen atmosphere with the purity of 99.999% and the flow of 0.5L/min, wherein the temperature program is as follows: heating from room temperature to 400 ℃ at the speed of 5 ℃/min, preserving heat for 60min, heating from 400 ℃ to 700 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, and obtaining carbon foam with a three-dimensional network structure; compressing the thickness of the carbon foam to be half of the thickness of the carbonized carbon foam by using a flat pressing plate;
(3) epoxy resin JY-257, curing agent modified methyl tetrahydrophthalic anhydride and accelerator 2-ethyl-4-methylimidazole according to the weight ratio of 10: 9: 0.1, mixing uniformly to obtain a mixture; mixing the mixture and the three-dimensional network structure carbon foam obtained in the step (2) according to the weight ratio of 50: 1, uniformly mixing in a mould, placing in a vacuum drying oven, and soaking for 1 hour at 80 ℃ under vacuum. And then respectively placing the materials at 120 ℃ for 3 hours and 150 ℃ for 5 hours for curing, and obtaining a composite material finished product after curing.
The thermal conductivity coefficient of the obtained composite material is 0.71W/(m.K); the tensile strength was 28.81MPa, and the modulus of elasticity was 97.2 MPa.
Claims (7)
1. A method for preparing a composite material by utilizing melamine formaldehyde foam is characterized by comprising the following steps:
(1) the use density is 5 to 9kg/m3The melamine formaldehyde foam is cleaned by compressed air, impurities and dust on the surface are blown off, and the melamine formaldehyde foam is cut into the size of 3-10 cm multiplied by 3-5 cm multiplied by 1-2 cm;
(2) carbonizing the melamine formaldehyde foam treated in the step (1) in a nitrogen atmosphere to obtain three-dimensional network structure carbon foam;
(3) uniformly mixing epoxy resin, a curing agent and an accelerator to obtain a mixture; and (3) mixing the mixture with the three-dimensional network structure carbon foam obtained in the step (2) in a mold according to the weight ratio of 30-80: 1, mixing, placing in a vacuum drying oven, and soaking for 1 hour at 80 ℃ under vacuum; and after the impregnation is finished, curing at high temperature to obtain a composite material finished product.
2. The method of claim 1, wherein the nitrogen has a purity of 99.999% and a flow rate of 0.5L/min.
3. The method according to claim 1, wherein the temperature program for the carbonization treatment is set to: raising the temperature from room temperature to 400 ℃ at the speed of 5-10 ℃/min, preserving the heat for 30-60 min, raising the temperature from 400 ℃ to 700 ℃ at the speed of 5-10 ℃/min, and preserving the heat for 2 hours.
4. The method of claim 1, wherein the curing agent is modified methyl tetrahydrophthalic anhydride and the accelerator is 2-ethyl-4-methylimidazole.
5. The method of claim 1, wherein the epoxy resin: curing agent: the weight ratio of the accelerator is 10: 8-9: 0.1.
6. the method of claim 1, wherein the curing is performed by: the mixture is placed at 80-120 ℃ for 2-4 hours, and then placed at 150-180 ℃ for 5-8 hours for curing.
7. The method of claim 1, wherein step (2) further comprises further compressing the resulting three-dimensional network-structured carbon foam to a thickness that is half the carbonized thickness using a flat platen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110681814.6A CN113480830A (en) | 2021-06-19 | 2021-06-19 | Method for preparing heat-conducting composite material by utilizing melamine formaldehyde foam |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110681814.6A CN113480830A (en) | 2021-06-19 | 2021-06-19 | Method for preparing heat-conducting composite material by utilizing melamine formaldehyde foam |
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| CN113480830A true CN113480830A (en) | 2021-10-08 |
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| CN202110681814.6A Pending CN113480830A (en) | 2021-06-19 | 2021-06-19 | Method for preparing heat-conducting composite material by utilizing melamine formaldehyde foam |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080275150A1 (en) * | 2007-05-01 | 2008-11-06 | Miller Douglas J | Carbon Foam With Supplemental Material |
| CN103972520A (en) * | 2014-04-18 | 2014-08-06 | 江西师范大学 | Elastic carbon foam oxygen reduction catalyst and preparation method thereof |
| US20150322230A1 (en) * | 2010-06-18 | 2015-11-12 | Basf Se | Molded parts made of carrier materials which contain foaming reactive resin |
| CN105733192A (en) * | 2016-03-21 | 2016-07-06 | 中南大学 | Foam framework enhanced polymer composite material and preparation method thereof |
| CN107601500A (en) * | 2017-11-02 | 2018-01-19 | 福州大学 | A kind of preparation method of high-specific surface area active foam Carbon Materials |
| CN112961461A (en) * | 2021-02-05 | 2021-06-15 | 吉林大学 | Organic resin composite material with 3D polyimide as heat conducting framework and preparation method thereof |
-
2021
- 2021-06-19 CN CN202110681814.6A patent/CN113480830A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080275150A1 (en) * | 2007-05-01 | 2008-11-06 | Miller Douglas J | Carbon Foam With Supplemental Material |
| CN101687646A (en) * | 2007-05-01 | 2010-03-31 | 格拉弗技术国际控股有限公司 | Carbon foam with auxiliary material |
| US20150322230A1 (en) * | 2010-06-18 | 2015-11-12 | Basf Se | Molded parts made of carrier materials which contain foaming reactive resin |
| CN103972520A (en) * | 2014-04-18 | 2014-08-06 | 江西师范大学 | Elastic carbon foam oxygen reduction catalyst and preparation method thereof |
| CN105733192A (en) * | 2016-03-21 | 2016-07-06 | 中南大学 | Foam framework enhanced polymer composite material and preparation method thereof |
| CN107601500A (en) * | 2017-11-02 | 2018-01-19 | 福州大学 | A kind of preparation method of high-specific surface area active foam Carbon Materials |
| CN112961461A (en) * | 2021-02-05 | 2021-06-15 | 吉林大学 | Organic resin composite material with 3D polyimide as heat conducting framework and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 何利华等: "三聚氰胺甲醛树脂泡沫塑料碳化研究", 《工程塑料应用》 * |
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Application publication date: 20211008 |