CN108117717A - A kind of graphene/phenolic resin high heat conducting nano composite material and preparation method thereof - Google Patents
A kind of graphene/phenolic resin high heat conducting nano composite material and preparation method thereof Download PDFInfo
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- CN108117717A CN108117717A CN201611060274.5A CN201611060274A CN108117717A CN 108117717 A CN108117717 A CN 108117717A CN 201611060274 A CN201611060274 A CN 201611060274A CN 108117717 A CN108117717 A CN 108117717A
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention relates to a kind of graphene/phenolic resin high heat conducting nano composite materials and preparation method thereof, belong to engineering plastics field.The composite material is mainly made of phenolic resin as matrix and modified nano graphite alkene or modified graphene oxide, and a kind of processing procedure mode of purpose offer is simple, the production time is brief, processing performance is excellent and the polyamide/graphite alkene nanocomposite of tool high thermal conductivity.Preparation method of the present invention and its each composition degree are：(1) 45% 86% phenolic resin, 10% 50% graphene or graphene oxide, 0.1% 2% silane coupling agent are taken, 5% 20% curing agent, graphene/phenolic resin blending master batch is made using journey in short-term, high speed grinding dispersion technology.Graphene/phenolic resin high heat conducting nano composite material provides thermal conductivity, tough material property, heat and the chemical stability of excellent benefit, can be widely applied in the fields such as industrial emissions device auto-parts, LED heat sinking back-plates or radiating module, electric equipment products spare and accessory parts.
Description
Technical field
The invention belongs to a kind of engineering plastics fields to relate to, and a kind of particularly graphene/phenolic resin high heat conducting nano is compound
Material and preparation method thereof.
Background technology
In science and technology electronics with rapid changepl. never-ending changes and improvements and opto-electronics, used thermal conductivity of material is all to receive pass all the time
Note and the subject under discussion of research.Constantly expand in consumer electrical product and LED illumination market and device development technique persistently promotes it
Under, derivative is important heat dissipation problem.High molecular material has low light weight, production cost, corrosion resistance, tough
The advantages that physical property and excellent processability, can realize the lightening target of electronic product easily.Therefore, through the present invention with simple
Processing procedure mode and the brief production time, obtain and answered with graphene/phenolic resin high heat conducting nano of high thermal conductivity
Condensation material.
Phenolic resin, English name are that Phenolic resin are artificial synthesized heat with the longest history in all plastics
Thermosetting resin, it is more because being used in electrical equipment, therefore be commonly called as bakelite.Phenolic resin is generally by phenol and formaldehyde through condensation reaction
The mixed composition of the auxiliary agents such as curing agent, inorganic filling material, physical property reinforcing material and colorant is added in afterwards.Phenolic resin advantage includes
Heat-resistant deforming temperature height, fine corrosion resistance, tool electrical insulating property, excellent mechanical mechanics property, low combustible, processing and forming
The advantages that property is good, cheap.It is widely used in machinery, auto-parts, electronic apparatus consumer products, chemical industry equipment and aviation
The fields of grade.However, in order to which the phenolic resin as heat insulator is made to become good heat conductor, it usually needs addition is largely led
It is uniform that hot filler or inorganic alloys conductor and the complicated processing procedure of transmission can just make phenolic resin obtain stable production batch
Degree and excellent heat conductivility.
Grapheme material passes through that researches show that possess the substance of highest coefficient of heat transfer in application material in the world at present, be approximately
14 times of copper, 3.5 times of graphite, and with very excellent mechanical property and chemical stability.Therefore graphene is considered most
It is suitble to solve current LED illumination and consumer electrical product heat dissipation problem.
The content of the invention
One of the objects of the present invention is to provide a kind of graphene/phenolic resin high heat conducting nano composite materials, solve
The complicated procedure for producing that existing phenolic resin heat-conductive composite material is faced, and excellent processing performance of having is showed with physical property
Power.
Purpose to realize the present invention, using following technical proposal：
A kind of graphene/phenolic resin high heat conducting nano composite material, raw material composition and its weight percent content are as follows：
The phenolic resin is formed using phenol, cresols, xylenol, resorcinol one of which as prepared by principal component
The graphene or graphene oxide are the graphene of size 50nm -100nm or graphene oxide microplate powder.
The silane coupling agent for γ-aminopropyl triethoxysilane amido functional group silane or γ-(2,
The third oxygen of 3- epoxies) propyl trimethoxy silicane epoxy functionality silane.
The curing agent is hexamethylenetetramine.
The preparation method comprises the following steps：The phenolic resin that formula is provided described in claim 1 is obtained extremely to reveal
Point drying equipment in temperature-20-- 40 DEG C time 4-12 it is small when water removal operation is dried.Obtain claim 1
The formula provided silane coupling agent, graphene or graphene oxide are inserted in nitrogen filled protection homogenizer, with rotating speed
800-2200 rpm, 80-120 DEG C of temperature, 5-15 minutes time carried out graphene or graphene oxide modification connects
Branch processing procedure.
The there is provided curing agent of formula described in claim 1 and the phenolic resin described in (1) step and the are provided
(2) modified graphene of step or modified graphene oxide are inserted in nitrogen filled protection high speed grinding dispersion machine with temperature 50
- 110 DEG C, 5-15 minutes time carry out being kneaded primary solidification processing procedure, graphene/phenolic resin blending master batch is made.
Obtain the graphene/phenolic resin blending master batch of (3) step.Insert injection-type compacting shape machine or injection molding machine
In with 150-180 DEG C of temperature, 1-15 minute time curing molding to get graphene/phenolic resin high heat conducting nano
Composite products.
The present invention use it is specific using phenol, cresols, xylenol, resorcinol one of which as prepared by principal component into
The phenolic resin of excellent mechanical property, cooperation possess the graphene of high coefficient of heat transfer or graphene oxide, silane coupling agent, curing
The raw materials such as agent.It is made uniform with high stable batch using journey in short-term, the specific high speed dispersion mixing technology of high-effect and step
Property with the phenolic resin composite of excellent heat conducting performance.Simple production process of the present invention is clear and definite, processing procedure briefly stablizes and cost
The advantages that high efficiency；The product of its preparation possesses physical property sustainment rate height, processing performance is excellent and possesses stable high-efficiency heat conduction rate
Etc. multinomial excellent properties.
Specific embodiment
In order to fairly set out the technical solution of the present invention, below processing procedure case study on implementation is coordinated to carry out specifically the present invention
It is bright, but the invention is not limited in any way.
It is principal component and aldehyde condensation polymer institute that phenolic resin material, which selects phenol, cresols, xylenol, resorcinol one of which,
It is prepared, such as phenol, formaldehyde.
Graphene or graphene oxide preferred dimension are the graphene of 50nm -100nm or graphene oxide microplate powder
Body, such as product grade XC007 for being produced into new material Science and Technology Ltd. of Xiamen alkene etc..
Silane coupling agent is selected as the amido functional group silane of γ-aminopropyl triethoxysilane or γ-(2,3-
The third oxygen of epoxy) propyl trimethoxy silicane epoxy functionality silane, such as the product grade KBE- of Japanese SHIN-ETSU HANTOTAI production
903rd, KBM-403, product grade KBE-903, A-180 of the connection production of U.S.'s carbon etc..
Curing agent is selected as hexamethylenetetramine.
Embodiment one
Phenolic resin is taken into dew point drying equipment with -20 DEG C of times 6 of temperature it is small when water removal operation is dried after, according to
Phenolic resin, 46.5% modified graphene or modified graphene oxide according to weight percent composition 46.5%, 0.5%
Silane coupling agent, 6.5% curing agent were inserted in nitrogen filled protection high speed grinding dispersion machine with 90 DEG C of temperature, 5 minutes time
It carries out being kneaded primary solidification processing procedure, graphene/phenolic resin blending master batch is made.It continues foregoing graphites alkene/phenolic resin is common
Mixed master batch is inserted in injection-type compacting shape machine or injection molding machine with 155 DEG C of temperature, 2 minutes time curing molding to get stone
Black alkene/one product of phenolic resin high heat conducting nano composite material embodiment.Embodiment raw material composition is listed in table 1.
Embodiment two
Phenolic resin is taken into dew point drying equipment with -20 DEG C of times 6 of temperature it is small when water removal operation is dried after, according to
Phenolic resin, 36.8% modified graphene or modified graphene oxide according to weight percent composition 55.1%, 0.4%
Silane coupling agent, 7.7% curing agent were inserted in nitrogen filled protection high speed grinding dispersion machine with 90 DEG C of temperature, 5 minutes time
It carries out being kneaded primary solidification processing procedure, graphene/phenolic resin blending master batch is made.It continues foregoing graphites alkene/phenolic resin is common
Mixed master batch is inserted in injection-type compacting shape machine or injection molding machine with 155 DEG C of temperature, 2 minutes time curing molding to get stone
Black alkene/two product of phenolic resin high heat conducting nano composite material embodiment.Embodiment raw material composition is listed in table 1.
Embodiment three
Phenolic resin is taken into dew point drying equipment with -20 DEG C of times 6 of temperature it is small when water removal operation is dried after, according to
Phenolic resin, 27.2% modified graphene or modified graphene oxide according to weight percent composition 63.6%, 0.3%
Silane coupling agent, 8.9% curing agent were inserted in nitrogen filled protection high speed grinding dispersion machine with 90 DEG C of temperature, 5 minutes time
It carries out being kneaded primary solidification processing procedure, graphene/phenolic resin blending master batch is made.It continues foregoing graphites alkene/phenolic resin is common
Mixed master batch is inserted in injection-type compacting shape machine or injection molding machine with 155 DEG C of temperature, 2 minutes time curing molding to get stone
Black alkene/three product of phenolic resin high heat conducting nano composite material embodiment.Embodiment raw material composition is listed in table 1.
Example IV
Phenolic resin is taken into dew point drying equipment with -20 DEG C of times 6 of temperature it is small when water removal operation is dried after, according to
Phenolic resin, 18% modified graphene or modified graphene oxide, 0.2% silicon according to weight percent composition 71.8%
Alkane coupling agent, 10% curing agent are inserted in nitrogen filled protection high speed grinding dispersion machine and carried out with 90 DEG C of temperature, 5 minutes time
Primary solidification processing procedure is kneaded, graphene/phenolic resin blending master batch is made.It continues foregoing graphites alkene/phenolic resin blending is female
Grain insert in injection-type compacting shape machine or injection molding machine with 155 DEG C of temperature, 2 minutes time curing molding to get graphene/
Phenolic resin high heat conducting nano composite material example IV product.Embodiment raw material composition is listed in table 1.
Embodiment five
Phenolic resin is taken into dew point drying equipment with -20 DEG C of times 6 of temperature it is small when water removal operation is dried after, according to
Phenolic resin, 8.8% modified graphene or modified graphene oxide, 0.1% silicon according to weight percent composition 79.9%
Alkane coupling agent, 11.2% curing agent insert in nitrogen filled protection high speed grinding dispersion machine with 90 DEG C of temperature, 5 minutes time into
Row is kneaded primary solidification processing procedure, and graphene/phenolic resin blending master batch is made.It continues foregoing graphites alkene/phenolic resin blending
Master batch is inserted in injection-type compacting shape machine or injection molding machine with 155 DEG C of temperature, 2 minutes time curing molding to get graphite
Alkene/five product of phenolic resin high heat conducting nano composite material embodiment.Embodiment raw material composition is listed in table 1.
1 each embodiment of table prepares formula for raw stock used in graphene/phenolic resin composite and forms
| Form % | Phenolic resin | Modified graphene or modified graphene oxide | Silane coupling agent | Curing agent |
| Embodiment one | 46.5 | 46.5 | 0.5 | 6.5 |
| Embodiment two | 55.1 | 36.8 | 0.4 | 7.7 |
| Embodiment three | 63.6 | 27.2 | 0.3 | 8.9 |
| Example IV | 71.8 | 18 | 0.2 | 10 |
| Embodiment five | 79.9 | 8.8 | 0.1 | 11.2 |
As shown in table 2, properties inspection is carried out to embodiment ㄧ to five using ASTM examination criterias.
Composite material inspection result prepared by 2 each embodiment of table
| Inspection project | Unit | Embodiment one | Embodiment two | Embodiment three | Example IV | Embodiment five |
| Proportion | 1.58 | 1.56 | 1.52 | 1.48 | 1.42 | |
| Tensile strength | Kgf/mm2 | 11.8 | 8.1 | 6.3 | 5.8 | 5.6 |
| Folding strength | Kgf/mm2 | 7.2 | 7.7 | 8.0 | 9.5 | 9.5 |
| Impact strength | Kgfcm/cm2 | 2.2 | 2.7 | 3.1 | 3.5 | 3.5 |
| Flame resistance | UL-94 | V-0/0.6mm | V-0/0.6mm | V-0/0.6mm | V-0/0.6mm | V-0/0.6mm |
| Thermal conductivity factor | W/m.K | 29.2 | 19.8 | 13.4 | 9.8 | 5.5 |
Illustrate hereby, above example and used raw material, formula are only the present invention preferably special case, not right with this
The scope of patent of the present invention is limited.
Claims (6)
- A kind of 1. graphene/phenolic resin high heat conducting nano composite material and preparation method thereof, it is characterised in that the composite material Raw material composition and its weight percent content it is as follows：
Phenolic resin 45–86% Graphene or graphene oxide 10 - 50% Silane coupling agent 0.1 - 2% Curing agent 5 - 20% 。 - 2. graphene/phenolic resin high heat conducting nano composite material according to claim 1, it is characterised in that described Phenolic resin is formed using phenol, cresols, xylenol, resorcinol one of which as prepared by principal component.
- 3. graphene/phenolic resin high heat conducting nano composite material according to claim 1, it is characterised in that described Graphene or graphene oxide are the modified graphene of size 50nm -100nm or modified graphene oxide microplate powder.
- 4. graphene/phenolic resin high heat conducting nano composite material according to claim 1, it is characterised in that described Silane coupling agent is the amido functional group silane of γ-aminopropyl triethoxysilane or γ-(the third oxygen of 2,3- epoxies) third The epoxy functionality silane of base trimethoxy silane.
- 5. graphene/phenolic resin high heat conducting nano composite material according to claim 1, it is characterised in that described Curing agent is hexamethylenetetramine.
- 6. graphene/phenolic resin high heat conducting nano composite material according to claim 1, it is characterised in that described Preparation method comprises the following steps：(1) obtain the provided phenolic resin of formula described in claim 1 into dew point drying equipment with temperature-20-- Water removal operation is dried when small in 40 DEG C of times 4-12；(2) silane coupling agent, graphene or the graphene oxide that formula is provided described in claim 1 are obtained and inserts nitrogen charging guarantor It protects in homogenizer, stone is carried out with 800-2200 rpm of rotating speed, 80-120 DEG C of temperature, 5-15 minutes time Black alkene or graphene oxide are modified grafting processing procedure；(3) the provided curing agent of formula described in claim 1 and the phenolic resin described in (1) step and the are provided (2) modified graphene of step or modified graphene oxide are inserted in nitrogen filled protection high speed grinding dispersion machine with temperature 50 - 110 DEG C, 5-15 minutes time carry out being kneaded primary solidification processing procedure, graphene/phenolic resin blending master batch is made；(4) graphene/phenolic resin blending master batch of (3) step is obtained；Insert injection-type compacting shape machine or injection molding machine In with 150-180 DEG C of temperature, 1-15 minute time curing molding to get graphene/phenolic resin high heat conducting nano Composite products.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611060274.5A CN108117717A (en) | 2016-11-28 | 2016-11-28 | A kind of graphene/phenolic resin high heat conducting nano composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611060274.5A CN108117717A (en) | 2016-11-28 | 2016-11-28 | A kind of graphene/phenolic resin high heat conducting nano composite material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003612A (en) * | 2019-05-13 | 2019-07-12 | 深圳市烯华先进材料科技有限公司 | LED light shell and preparation method thereof |
| CN112795135A (en) * | 2021-01-18 | 2021-05-14 | 浙江南塑合成材料有限公司 | Method for manufacturing high-performance heat-conducting plastic composite material |
| CN115197532A (en) * | 2022-07-22 | 2022-10-18 | 深圳市烯华先进材料科技有限公司 | Phenolic resin material, preparation method thereof and heat dissipation device |
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| CN104448174A (en) * | 2014-12-11 | 2015-03-25 | 山东圣泉新材料股份有限公司 | Graphene phenolic resin composite material |
| KR20150074481A (en) * | 2013-12-24 | 2015-07-02 | 현대자동차주식회사 | nylon composite And Method of nylon composite |
| CN105385100A (en) * | 2015-12-23 | 2016-03-09 | 江南大学 | Graphene-modified phenolic molding material and preparation method thereof |
| CN108084635A (en) * | 2016-11-22 | 2018-05-29 | 厦门泰启力飞电子科技有限公司 | A kind of graphene nano Combined Electrostatic shielding material and preparation method thereof |
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2016
- 2016-11-28 CN CN201611060274.5A patent/CN108117717A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20150074481A (en) * | 2013-12-24 | 2015-07-02 | 현대자동차주식회사 | nylon composite And Method of nylon composite |
| CN104448174A (en) * | 2014-12-11 | 2015-03-25 | 山东圣泉新材料股份有限公司 | Graphene phenolic resin composite material |
| CN105385100A (en) * | 2015-12-23 | 2016-03-09 | 江南大学 | Graphene-modified phenolic molding material and preparation method thereof |
| CN108084635A (en) * | 2016-11-22 | 2018-05-29 | 厦门泰启力飞电子科技有限公司 | A kind of graphene nano Combined Electrostatic shielding material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003612A (en) * | 2019-05-13 | 2019-07-12 | 深圳市烯华先进材料科技有限公司 | LED light shell and preparation method thereof |
| CN112795135A (en) * | 2021-01-18 | 2021-05-14 | 浙江南塑合成材料有限公司 | Method for manufacturing high-performance heat-conducting plastic composite material |
| CN115197532A (en) * | 2022-07-22 | 2022-10-18 | 深圳市烯华先进材料科技有限公司 | Phenolic resin material, preparation method thereof and heat dissipation device |
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Address after: Room 303b, Xinye building, Pioneer Park, torch hi tech Zone, Xiamen, Fujian, 361000 Applicant after: XIAMEN TEKILIFI ELECTRONIC TECHNOLOGY Co.,Ltd. Address before: 361000 6B, No.2 workshop, no.145-1, Yuehua Road, Huli District, Xiamen City, Fujian Province Applicant before: XIAMEN TAIQILIFEI ELECTRONIC TECHNOLOGY Co.,Ltd. |
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Application publication date: 20180605 |