CN103602038A - Preparation method of high-heat-conductivity phenol aldehyde resin-base high polymer material - Google Patents
Preparation method of high-heat-conductivity phenol aldehyde resin-base high polymer material Download PDFInfo
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- CN103602038A CN103602038A CN201310562923.1A CN201310562923A CN103602038A CN 103602038 A CN103602038 A CN 103602038A CN 201310562923 A CN201310562923 A CN 201310562923A CN 103602038 A CN103602038 A CN 103602038A
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- aldehyde resin
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Abstract
The invention belongs to the technical field of chemical synthesis of high polymer materials, and relates to a preparation method of a high-heat-conductivity phenol aldehyde resin-base high polymer material. The method comprises the following steps: 1. carrying out ball milling on a resin base material, a curing agent and an inorganic heat-conducting filler, and refining to obtain the uniformly mixed phenol aldehyde resin-base heat-conducting plastic nanoparticles; 2. adding the phenol aldehyde resin-base heat-conducting plastic particles into an open mill, and carrying out open milling to obtain primarily cured phenol aldehyde resin-base heat-conducting plastic particles; and 3. carrying out hot pressing on the phenol aldehyde resin-base heat-conducting plastic particles in a hot pressing mold to obtain the high-heat-conductivity phenol aldehyde resin-base high polymer material. The high-heat-conductivity phenol aldehyde resin-base high polymer material has the advantages of higher heat conductivity, excellent mechanical strength and excellent machinability; and the preparation method is simple and easy to implement, and has the advantages of no volatile solvent, environment friendliness, no pollution and low production cost.
Description
Technical field
The invention belongs to the synthetic field of macromolecular material chemical industry, relate to a kind of preparation method with the alkyd resin based macromolecular material of high thermal conductivity coefficient.
Background technology
Metallic substance has the features such as physical strength is high, thermal conductivity is good, be widely used in the element such as main body, heating panel of electrical equipment, but metallic substance has, and density is large, power consumption of polymer processing is high, environmental pollution, the weak point such as expensive, in many Application Areass, by plastics, replaced gradually, especially in field of electronics, require the environment of insulation, heat radiation.In recent years, electronic devices and components and electronics are gradually to future developments such as " thin, light, little ", and the engineering plastics that exploitation has excellent heat conductivity performance and mechanical property replace metallic substance to become inevitable development trend.
High speed development along with modern electronic technology, the continuous increase of the current density in electronic component and charge capacity, the heat that electric equipment products in use produced must be diffused in external environment in time, otherwise can damage electronic component because of local superheating, reduce work-ing life, even initiation fire.Therefore, in exploitation heat conduction engineering plastics process, must note improving its heat-conductive characteristic, in general, the plastics that thermal conductivity meets or exceeds 3W/mK could meet the requirement of practical application.
In prior art, the method that improves plastics heat conductivility is mainly to utilize the inorganic materials of high heat conduction, as metal-powders such as boron nitride, silicon carbide, aluminium nitride, magnesium oxide or iron, copper, aluminium, adopt melt-mixing method to carry out filling-modified to polymkeric substance, this method often needs higher loading level (generally in 80wt% left and right) to form heat conduction network chain in polymkeric substance inside, thereby reaches good heat conductivility.But higher inorganic materials loading level has a negative impact to forming process ability and the mechanical property of polymer plastic.Lin Xiaodan etc. (CN1775860A) disclose a kind of moulded heat-conductive insulated plastics of preparing by adding heat conductive filler injection moulding, and its thermal conductivity can reach 3.5W/mK, but because proportion of filler is excessive, have reduced the mechanical strength of material.Dong Yuxin etc. (CN102936410A) have reported a kind of polyamide-based heat-conductive composite material of preparing by hydrothermal synthesis method, its thermal conductivity is up to 14.7W/mK, its inorganic heat conductive filler ratio is about 40wt%, and this material also has good tensile strength and bending strength simultaneously.Weak point is that preparation technology is comparatively complicated, and preparation cycle is longer, and raw materials for production are expensive, are unfavorable for scale operation.
By add inorganic thermally conductive material in polymkeric substance, improve the heat conductivility of plastics, its major cause is that inorganic materials easily forms heat conduction network chain in plastics.But, be subject to the impact of the factors such as grain size, irregular profile of inorganic materials, easily in plastics inner, form defect or focal point of stress, and then reduce the mechanical property of plastics.The inorganic materials of nano particle has the not available feature of a lot of conventional materials, as " small-size effect ", " surface effects ", " quantum effect " etc., is widely used in the modification of polymer plastic, and has obtained good practical application effect.In the preparation process of material, for example melt-mixing method is prepared Preparing Organic-inorganic Nano Hybrid Material, is easy to cause the reunion of nano particle, in body material, disperse inhomogeneous, thereby affect the modified effect of plastics.
Summary of the invention
For shortcomings and deficiencies of the prior art, the object of this invention is to provide and a kind ofly take novolac resin as body material, by adding solidifying agent and inorganic heat conductive filler nanoparticle, through hot-forming, prepare heat conductivility, mechanical property and processing characteristics good, production prices are cheap, and are suitable as the method for the heat-conductive composite material of electronic apparatus heat dissipation element.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of alkyd resin based macromolecular material of high thermal conductivity coefficient, comprises the steps:
(1) by reisn base material, solidifying agent, inorganic heat conductive filler (45～100) in mass ratio: (5～10): (30～50) weigh respectively after proportioning, first inorganic heat conductive filler is carried out in mechanical ball milling device to ball milling, refinement, Ball-milling Time is no more than 3 hours; Inorganic heat conductive filler, solidifying agent after ball milling are joined in phenolic resin as matrix resin material, continue ball mill mixing, the time is no more than 2 hours; After finishing, ball milling obtains the mixed uniformly alkyd resin based heat-conducting plastic particle of nano particle;
(2) alkyd resin based heat-conducting plastic particle prepared in step (1) is joined in mill and opens refining, mixing temperature is controlled at 100～150 ℃, and opening the refining time is 5～15 minutes.Open after refining finishes, obtain the alkyd resin based heat-conducting plastic particle of primary solidification;
(3) by resulting alkyd resin based heat-conducting plastic particle in step (2) in heat pressing and molding mold, carry out hot-forming, temperature is controlled at 150～160 ℃ of scopes, pressure-controlling is in 10～30MPa scope, time is controlled at 5～10 minutes scopes, prepares the alkyd resin based macromolecular material of high thermal conductivity coefficient.
Solidifying agent described in step (1) is hexamethylenetetramine.
Inorganic heat conductive filler described in step (1) comprises according to quality proportioning (10～50): (5～30): (5～10): (5～10): (1～5): the graphite of (1～5), metal powder, quartz, silicon carbide, boron nitride, magnesium oxide mix and forms; Described inorganic heat conductive filler is after ball milling, and particle size is about 100～500 nanometers.
Inorganic heat conductive filler described in step (1) is by according to quality proportioning (10～50): (5～30): (5～10): (5～10): the graphite of (1～5), metal powder, quartz, silicon carbide, boron nitride are mixed and formed; Described inorganic heat conductive filler is after ball milling, and particle size is about 100～500 nanometers.
Compared with prior art, advantage of the present invention is: apply alkyd resin based heat-conductive composite material prepared by method of the present invention and have higher thermal conductivity, good mechanical strength and processability, can realize the processing modes such as mold pressing, injection moulding and extrusion moulding; Secondly, preparation method of the present invention is simple, containing volatile solvent, not environment friendly and pollution-free, low production cost.Utilize heat-conducting plastic prepared by method of the present invention after overmolding, to can be used for electronic apparatus and LED light fixture heat dissipation element, improve the heat dispersion of product, extend its work-ing life.
Embodiment
Embodiment 1
The resol that is 50:5:30 by quality proportioning, hexamethylenetetramine, inorganic heat conductive filler weigh after proportioning, first inorganic heat conductive filler are carried out in mechanical ball milling device to ball milling, refinement, Ball-milling Time 2.5 hours; Inorganic heat conductive filler nano powder particle size after ball milling is about 100 nanometers, joins in phenolic resin as matrix resin material, adds solidifying agent hexamethylenetetramine simultaneously, continues ball mill mixing, and the time is no more than 2 hours; After finishing, ball milling obtains the mixed uniformly alkyd resin based heat-conducting plastic particle of nano particle; Primary solidification in mill, temperature is controlled at 120 ℃ of left and right; Then moulding in hot pressing die, prepares heat-conductive composite material, and hot pressing temperature is controlled at 150 ℃ of left and right, prepares the alkyd resin based macromolecular material of high thermal conductivity coefficient of the present invention; Wherein in inorganic heat conductive filler, graphite, iron powder, quartz, silicon carbide, boron nitride, magnesian mass ratio are 50:20:10:5:5:5; The alkyd resin based macromolecular material thermal conductivity of the high thermal conductivity coefficient that the present embodiment is prepared is 3.7W/mK.
Embodiment 2
The resol that is 95:10:50 by quality proportioning, hexamethylenetetramine, inorganic heat conductive filler weigh after proportioning, first inorganic heat conductive filler are carried out in mechanical ball milling device to ball milling, refinement, Ball-milling Time 2.5 hours; Inorganic heat conductive filler nano powder particle size after ball milling is about 100 nanometers, joins in phenolic resin as matrix resin material, adds solidifying agent hexamethylenetetramine simultaneously, continues ball mill mixing, and the time is no more than 2 hours; After finishing, ball milling obtains the mixed uniformly alkyd resin based heat-conducting plastic particle of nano particle; Primary solidification in mill, temperature is controlled at 100 ℃ of left and right; Then moulding in hot pressing die, prepares heat-conductive composite material, and hot pressing temperature is controlled at 160 ℃ of left and right, prepares the alkyd resin based macromolecular material of high thermal conductivity coefficient of the present invention; Wherein in inorganic heat conductive filler, the mass ratio of graphite, aluminium powder, quartz, carbon nanotube, boron nitride is 50:15:10:5:5; The alkyd resin based macromolecular material thermal conductivity of the high thermal conductivity coefficient that the present embodiment is prepared is 5.8W/mK.
Claims (4)
1. a preparation method for the alkyd resin based macromolecular material of high thermal conductivity coefficient, is characterized in that: comprise the steps:
(1) by reisn base material, solidifying agent, inorganic heat conductive filler (45～100) in mass ratio: (5～10): (30～50) weigh respectively after proportioning, first inorganic heat conductive filler is carried out in mechanical ball milling device to ball milling, refinement, Ball-milling Time is no more than 3 hours; Inorganic heat conductive filler, solidifying agent after ball milling are joined in phenolic resin as matrix resin material, continue ball mill mixing, the time is no more than 2 hours; After finishing, ball milling obtains the mixed uniformly alkyd resin based heat-conducting plastic particle of nano particle;
(2) alkyd resin based heat-conducting plastic particle prepared in step (1) is joined in mill and opens refining, mixing temperature is controlled at 100～150 ℃, and opening the refining time is 5～15 minutes.Open after refining finishes, obtain the alkyd resin based heat-conducting plastic particle of primary solidification;
(3) by resulting alkyd resin based heat-conducting plastic particle in step (2) in heat pressing and molding mold, carry out hot-forming, temperature is controlled at 150～160 ℃ of scopes, pressure-controlling is in 10～30MPa scope, time is controlled at 5～10 minutes scopes, prepares the alkyd resin based macromolecular material of high thermal conductivity coefficient.
2. the preparation method of the alkyd resin based macromolecular material of high thermal conductivity coefficient according to claim 1, is characterized in that: the solidifying agent described in step (1) is hexamethylenetetramine.
3. the preparation method of the alkyd resin based macromolecular material of high thermal conductivity coefficient according to claim 1, is characterized in that: inorganic heat conductive filler described in step (1) comprises according to quality proportioning (10～50): (5～30): (5～10): (5～10): (1～5): the graphite of (1～5), metal powder, quartz, silicon carbide, boron nitride, magnesium oxide mix and forms.
4. the preparation method of the alkyd resin based macromolecular material of high thermal conductivity coefficient according to claim 3, is characterized in that: described inorganic heat conductive filler is by according to quality proportioning (10～50): (5～30): (5～10): (5～10): the graphite of (1～5), metal powder, quartz, silicon carbide, boron nitride are mixed and formed.
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| CN201310562923.1A CN103602038A (en) | 2013-11-07 | 2013-11-07 | Preparation method of high-heat-conductivity phenol aldehyde resin-base high polymer material |
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Cited By (5)
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| CN106629650A (en) * | 2016-09-23 | 2017-05-10 | 武汉理工大学 | Method for preparing monodisperse phenolic resin microspheres and porous carbon microspheres in macroscopic quantity |
| CN107057272A (en) * | 2016-12-11 | 2017-08-18 | 安徽兆利光电科技有限公司 | A kind of LED wiring board |
| CN108587048A (en) * | 2018-04-03 | 2018-09-28 | 商洛学院 | A kind of LED lamp bead pedestal |
| CN111234452A (en) * | 2020-03-18 | 2020-06-05 | 常熟东南塑料有限公司 | Insulating heat-conducting phenolic moulding plastic |
| WO2020183449A1 (en) * | 2019-03-14 | 2020-09-17 | Israel Aerospace Industries Ltd. | Composite material with enhanced thermal conductivity and method for fabrication thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106629650A (en) * | 2016-09-23 | 2017-05-10 | 武汉理工大学 | Method for preparing monodisperse phenolic resin microspheres and porous carbon microspheres in macroscopic quantity |
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| CN107057272A (en) * | 2016-12-11 | 2017-08-18 | 安徽兆利光电科技有限公司 | A kind of LED wiring board |
| CN108587048A (en) * | 2018-04-03 | 2018-09-28 | 商洛学院 | A kind of LED lamp bead pedestal |
| WO2020183449A1 (en) * | 2019-03-14 | 2020-09-17 | Israel Aerospace Industries Ltd. | Composite material with enhanced thermal conductivity and method for fabrication thereof |
| IL265374B1 (en) * | 2019-03-14 | 2023-07-01 | Israel Aerospace Ind Ltd | Composite material with increase thermal conductivity and method for manufacture thereof |
| CN111234452A (en) * | 2020-03-18 | 2020-06-05 | 常熟东南塑料有限公司 | Insulating heat-conducting phenolic moulding plastic |
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Application publication date: 20140226 |