CN102850717A - High thermal conductivity phenolic resin and preparation method - Google Patents
High thermal conductivity phenolic resin and preparation method Download PDFInfo
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- CN102850717A CN102850717A CN2012103662531A CN201210366253A CN102850717A CN 102850717 A CN102850717 A CN 102850717A CN 2012103662531 A CN2012103662531 A CN 2012103662531A CN 201210366253 A CN201210366253 A CN 201210366253A CN 102850717 A CN102850717 A CN 102850717A
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- phenolic resin
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- heat conduction
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Abstract
The invention relates to a high thermal conductivity phenolic resin composite material and a preparation method and belongs to the field of composite materials. The composite material is prepared by a thermoplastic phenolic resin matrix, a thermal conductivity filler and a curing agent. The preparation method of the composite material component includes using an ethanol solvent to dissolve the thermoplastic phenolic resin matrix and the curing agent, adding the thermal conductivity filler, evenly stirring the mixture, and then drying the mixture in a dryer to obtain precursor powders; and preheating the precursor powders in a pressing machine at the temperature of 80-120 DEG C for 20-40 minutes, then subjecting the precursor powders to hot pressing at the temperatures of 140-160 DEG C under the pressure of 20-40 MPa for 20-40 minutes, and finally subjecting the precursor powders to hot pressing at the temperatures of 170-200 DEG C under the pressure of 20-40 MPa for 20-40 minutes. The obtained high thermal conductivity phenolic resin has super-high thermal conductivity performances, so that the high thermal conductivity phenolic resin is a good material for producing plate heat exchangers and the like and can be widely applied to fields of automobiles, electronics, appliance facilities and the like.
Description
Technical field
The present invention relates to a kind of high heat conduction phenolic resin composite and preparation method, the heat conductivility that prepared high heat conduction phenolic resin composite has superelevation, be the good material of making plate-type heat exchanger etc., and can be widely used in the fields such as automobile, electronics, household electrical appliances facility.
Background technology
Along with science and technology and industrial development, thermally conductive material is widely used in electric, electronic information, the fields such as heat exchange engineering.Traditional thermally conductive material major part is metal (Ag, Cu and Al etc.) and metal oxide (Al
2O
3With MgO etc.).Yet the erosion resistance of most metals material is poor, although adopt the technology such as corrosion protection coating and alloy, has improved the corrosion resistance of metal, greatly reduces the heat conductivility of material, thereby limits it in the application in the fields such as chemical industry.Macromolecular material is because it has good mechanical property and corrosion resistance nature, be widely used for replacing traditional metallic substance by people, but macromolecular material is the poor conductor of heat, causes that people pay close attention to more and more widely so improve the heat conductivility of macromolecular material.
Improve the macromolecular material heat conductivility and mainly contain following two kinds of approach: a kind of is synthetic intrinsic heat-conducting polymer material with high thermal conductivity coefficient, as polyaniline, polyacetylene and poly-adjoining with good heat conductive performance are coughed up etc.But these kinds heat-conducting polymer material synthesis technique is loaded down with trivial details, processing difficulties, therefore limits its large-scale application.Another kind is to use metal or the Inorganic Fillers Filled polymer materials with high thermal conductivity.This method has cheap and the advantage such as easy machine-shaping, to be applied to some special dimension.
In mineral filler, the thermal conductivity of graphite and metal approach.Graphite is a kind of mineral that extensively are present in occurring in nature, with electronics, the acting in conjunction of phonon double mechanism and have good thermal conductivity.The develop and spread of carbon fiber, carbon nanotube makes the Remarkable Progress On Electric Artificial progress of heat-conductive composite material, but because of expensive, can only use in high-tech sector.Therefore seek new method, adopt different filler combination modes, use a small amount of carbon fiber, the thermally conductive material that carbon nanotube just can obtain excellent performance becomes the focus of research.
Summary of the invention
The object of the invention is to, for the deficiencies in the prior art, provide a kind of high heat conduction phenolic resin composite and preparation method.Take novolac resin as matrix, add heat conductive filler, solidifying agent stirs, drying, the press compressing tablet obtains having the phenolic resin composite of the heat conductivility of superelevation.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of high heat conduction phenolic resin composite, it includes (mass fraction):
100 parts of novolac resin matrixes
10 ~ 400 parts of heat conductive fillers
5 ~ 20 parts in solidifying agent
85 ~ 120 ℃ of described novolac resin matrix softening temperatures.
Described heat conductive filler comprises: natural flake graphite 10 ~ 100 μ m, spherical graphite 10 ~ 100 μ m, carbon fiber, one or more mixture fillers of the carbon nanotube of carbon nanotube and acidification.
Described solidifying agent comprises: aniline, hexamethylenetetramine or trimeric cyanamide.
A kind of high heat conduction phenolic resin composite of the present invention and preparation method comprise the steps:
Step 1: novolac resin is dissolved with alcohol solvent;
Step 2: solidifying agent is dissolved with alcohol solvent;
Step 3: novolac resin and the solidifying agent of dissolving are mixed;
Step 4: conductive filler material is added in the mixed solvent, utilize stirrer to mix;
Step 5: place baking oven dry mixed system, obtain the composite material precursor powder.
Step 6: precursor powder is 80 ~ 120 ℃ of preheating 20 ~ 40 min in press, then 140 ~ 160 ℃ of temperature, and pressure 20 ~ 40 MPa, hot pressing 20 ~ 40 min, at last 170 ~ 200 ℃ of temperature, pressure 20 ~ 40 MPa hot pressing 20 ~ 40 min.
A kind of high heat conduction phenolic resin composite of the present invention by kind and the ratio of suitable combination heat conductive filler, has the advantageous feature of high conduction.
Description of drawings
Fig. 1 is the process route chart of the high heat conduction phenolic resin composite of embodiment 1 preparation.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explanation the present invention, is not be used to limiting scope of the present invention.Comprise in the novolac resin object lesson: novolac resin (85 ~ 95 ℃ of softening temperatures), novolac resin (95 ~ 105 ℃ of softening temperatures) and novolac resin (115 ~ 120 ℃ of softening temperatures).The corresponding above softening temperature of buying difference adopts the KT-3530F of elder brother's benefit resin material Science and Technology Ltd., the PF-8001 of 2123 and Shandong Shengquan Chemical Industry Co., Ltd. of chemical experimental factory, Heng Xin, Deyang on the market.
Embodiment 1
With 100 g novolac resins (85 ~ 95 ℃ of softening temperatures), 5 g hexamethylenetetramines add respectively alcohol solvent, mix after the dissolving, add 70 g natural flake graphites (100 μ m) in mixing solutions, stir.Mixing solutions is put into drying in the baking oven, obtains the composite material precursor powder.With precursor powder 80 ℃ of preheating 20 min in press, then 140 ℃ of temperature, pressure 20 MPa hot pressing 20 min, at last 170 ℃ of temperature, pressure 20 MPa hot pressing 20 min.The sample that obtains carries out the test of heat conductivility.
Comparative Examples 1
With 100 g novolac resins (85 ~ 95 ℃ of softening temperatures), 80 ℃ of preheating 20 min in press, then 140 ℃ of temperature, pressure 20 MPa hot pressing 20 min, at last 170 ℃ of temperature, pressure 20 MPa hot pressing 20 min.The sample that obtains carries out the test of heat conductivility.
Embodiment 2
Implementation method is identical with embodiment 1, and different is to adopt novolac resin (95 ~ 105 ℃ of softening temperatures).The sample that obtains carries out the test of heat conductivility.
Embodiment 3
Implementation method is identical with embodiment 1, and different is novolac resin (115 ~ 120 ℃ of softening temperatures).The sample that obtains carries out the test of heat conductivility.
Embodiment 4
Implementation method is identical with embodiment 1, and the content of different natural flake graphite (100 μ m) is 10 g.The sample that obtains carries out the test of heat conductivility.
Embodiment 5
Implementation method is identical with embodiment 1, and the content of different is natural flake graphite (100 μ m) is 400 g.The sample that obtains carries out the test of heat conductivility.
Embodiment 6
Implementation method is identical with embodiment 1, and the content of different is hexamethylenetetramine is 20 g, and the content of natural flake graphite (100 μ m) is 400 g.The sample that obtains carries out the test of heat conductivility.
Embodiment 7
Implementation method is identical with embodiment 1, and different is with precursor powder 120 ℃ of preheating 40 min in mould, then 160 ℃ of temperature, and pressure 40 MPa hot pressing 40 min, at last 200 ℃ of temperature, pressure 40 MPa hot pressing 40 min.The sample that obtains carries out the test of heat conductivility.
Embodiment 8
Implementation method is identical with embodiment 1, and different is to change solidifying agent into aniline, and the sample that obtains carries out the test of heat conductivility.
Embodiment 9
Implementation method is identical with embodiment 1, and different is to change solidifying agent into trimeric cyanamide, and the sample that obtains carries out the test of heat conductivility.
Embodiment 10
Implementation method is identical with embodiment 1, and different is changes the size of natural flake graphite into 10 μ m, and the sample that obtains carries out the test of heat conductivility.
Embodiment 11
Implementation method is identical with embodiment 1, and different is to change natural flake graphite into spherical graphite, and diameter is 10 μ m, and the sample that obtains carries out the test of heat conductivility.
Embodiment 12
Implementation method is identical with embodiment 1, and different is to change natural flake graphite into spherical graphite, and diameter is 100 μ m, and the sample that obtains carries out the test of heat conductivility.
Embodiment 13
Implementation method is identical with embodiment 1, and different is that the natural flake graphite that will add changes carbon fiber into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 14
Implementation method is identical with embodiment 1, and different is that the natural flake graphite that will add changes carbon nanotube into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 15
Implementation method is identical with embodiment 1, and the natural flake graphite that different is will add changes the carbon nanotube of acidifying into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 16
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of 60 g crystalline flake graphites (10 μ m) and 10 g spherical graphites (10 μ m) into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 17
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of 60 g crystalline flake graphites (100 μ m) and 10 g spherical graphites (10 μ m) into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 18
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of 60 g crystalline flake graphites (100 μ m) and 10 g spherical graphites (100 μ m) into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 19
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of 60 g crystalline flake graphites (100 μ m) and 10 g carbon fibers into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 20
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of 60 g crystalline flake graphites (100 μ m) and 10 g carbon nanotubes into, and the sample that obtains carries out the test of heat conductivility.
Embodiment 21
Implementation method is identical with embodiment 1, and the 70 g natural flake graphites (100 μ m) that different is will add change the mixture of the carbon nanotube of 60 g crystalline flake graphites (100 μ m) and 10 g acidifyings into, and the sample that obtains carries out the test of heat conductivility.
Following table is the heat conductivility table of the high heat conduction phenolic resin material of the present invention embodiment:
Claims (5)
1. one kind high heat conduction phenolic resin composite is characterized in that, by the novolac resin matrix, heat conductive filler and solidifying agent are made, and described mass fraction consumption is as follows:
100 parts of novolac resin matrixes
10 ~ 400 parts of heat conductive fillers
5 ~ 20 parts in solidifying agent.
2. according to a kind of high heat conduction phenolic resin composite described in the claim 1, it is characterized in that, described novolac resin matrix softening temperature is 85 ~ 120 ℃.
3. according to a kind of high heat conduction phenolic resin composite described in the claim 1, it is characterized in that, described heat conductive filler comprises: natural flake graphite 10 ~ 100 μ m, spherical graphite 10 ~ 100 μ m, carbon fiber, one or more mixture fillers of the carbon nanotube of carbon nanotube and acidification.
4. according to a kind of high heat conduction phenolic resin composite described in the claim 1, it is characterized in that, described solidifying agent comprises: aniline, hexamethylenetetramine or trimeric cyanamide.
5. according to the preparation method of a kind of high heat conduction phenolic resin composite described in the claim 1, it is characterized in that, may further comprise the steps: respectively novolac resin and solidifying agent are dissolved with alcohol solvent, add heat conductive filler, stirring, it is dry to be placed in the baking oven, obtains precursor powder; With precursor powder 80 ~ 120 ℃ of preheating 20 ~ 40 min in press, then 140 ~ 160 ℃ of temperature, pressure 20 ~ 40 MPa hot pressing 20 ~ 40 min, at last 170 ~ 200 ℃ of temperature, pressure 20 ~ 40 MPa hot pressing 20 ~ 40 min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236826A (en) * | 2015-10-30 | 2016-01-13 | 西南科技大学 | Preparation method of thermo-conductive insulation composite material |
| CN105802125A (en) * | 2016-03-02 | 2016-07-27 | 武汉理工大学 | Flame-retardant high-temperature-resistant boron phenolic resin composition and preparation method thereof |
| CN106479111A (en) * | 2016-09-21 | 2017-03-08 | 芜湖扬展新材料科技服务有限公司 | A kind of high-termal conductivity is double to exceed the preparation method oozing structure three-phase composite material |
| CN106832755A (en) * | 2017-03-23 | 2017-06-13 | 樊劲松 | A kind of preparation of water heater transducing core |
| CN106987091A (en) * | 2017-05-18 | 2017-07-28 | 安徽普瑞普勒传热技术有限公司 | A kind of shell-and-tube heat exchanger heat exchange material |
| CN107418203A (en) * | 2017-06-08 | 2017-12-01 | 安徽普瑞普勒传热技术有限公司 | A kind of heat exchanger heat exchange material and its production technology |
| CN107618123A (en) * | 2017-09-30 | 2018-01-23 | 华中科技大学 | A kind of preparation method and product of polyethylene crystalline flake graphite composite |
| WO2019037564A1 (en) * | 2017-08-25 | 2019-02-28 | 四川依菲兰科技有限公司 | Non-metal composite nano heat dissipation material and preparation method therefor |
| CN114350107A (en) * | 2022-01-19 | 2022-04-15 | 哈尔滨工业大学无锡新材料研究院 | Rapidly-formed anisotropic heat-conducting composite material and preparation method thereof |
| CN114410060A (en) * | 2021-12-23 | 2022-04-29 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927936A (en) * | 2005-09-08 | 2007-03-14 | 山东大学 | Modified phenolic resin/graphite based conducting composite material and preparation process thereof |
-
2012
- 2012-09-27 CN CN2012103662531A patent/CN102850717A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927936A (en) * | 2005-09-08 | 2007-03-14 | 山东大学 | Modified phenolic resin/graphite based conducting composite material and preparation process thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236826A (en) * | 2015-10-30 | 2016-01-13 | 西南科技大学 | Preparation method of thermo-conductive insulation composite material |
| CN105802125A (en) * | 2016-03-02 | 2016-07-27 | 武汉理工大学 | Flame-retardant high-temperature-resistant boron phenolic resin composition and preparation method thereof |
| CN106479111A (en) * | 2016-09-21 | 2017-03-08 | 芜湖扬展新材料科技服务有限公司 | A kind of high-termal conductivity is double to exceed the preparation method oozing structure three-phase composite material |
| CN106832755A (en) * | 2017-03-23 | 2017-06-13 | 樊劲松 | A kind of preparation of water heater transducing core |
| CN106987091A (en) * | 2017-05-18 | 2017-07-28 | 安徽普瑞普勒传热技术有限公司 | A kind of shell-and-tube heat exchanger heat exchange material |
| CN107418203A (en) * | 2017-06-08 | 2017-12-01 | 安徽普瑞普勒传热技术有限公司 | A kind of heat exchanger heat exchange material and its production technology |
| WO2019037564A1 (en) * | 2017-08-25 | 2019-02-28 | 四川依菲兰科技有限公司 | Non-metal composite nano heat dissipation material and preparation method therefor |
| CN107618123A (en) * | 2017-09-30 | 2018-01-23 | 华中科技大学 | A kind of preparation method and product of polyethylene crystalline flake graphite composite |
| CN114410060A (en) * | 2021-12-23 | 2022-04-29 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
| CN114410060B (en) * | 2021-12-23 | 2023-09-19 | 厦门泰启力飞科技有限公司 | Face cover of camera device and preparation method thereof |
| CN114350107A (en) * | 2022-01-19 | 2022-04-15 | 哈尔滨工业大学无锡新材料研究院 | Rapidly-formed anisotropic heat-conducting composite material and preparation method thereof |
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Application publication date: 20130102 |