CN104817671A - High-heat-conductive graphene oxide melamine resin and preparation method of same - Google Patents

High-heat-conductive graphene oxide melamine resin and preparation method of same Download PDF

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Publication number
CN104817671A
CN104817671A CN201510220723.7A CN201510220723A CN104817671A CN 104817671 A CN104817671 A CN 104817671A CN 201510220723 A CN201510220723 A CN 201510220723A CN 104817671 A CN104817671 A CN 104817671A
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China
Prior art keywords
graphene oxide
parts
melmac
appropriate
resin
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CN201510220723.7A
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Chinese (zh)
Inventor
张庆
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Wuhu Baoyi Amusement Equipment Co Ltd
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Wuhu Baoyi Amusement Equipment Co Ltd
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Priority to CN201510220723.7A priority Critical patent/CN104817671A/en
Publication of CN104817671A publication Critical patent/CN104817671A/en
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Abstract

A high-heat-conductive graphene oxide melamine resin is prepared from following raw materials, by weight: 0.3-0.5 parts of nano tin powder, 0.4-0.6 parts of silicon carbide nano fibers, 20-25 parts of melamine, 40-45 parts of 37% formalin, 1.8-2.1 parts of graphene oxide, 0.7-0.9 parts of trifluoroethyl methylacrylate, 0.7-0.9 parts of polyacrylonitrile, a proper amount of dimethylformamide, 0.2-0.3 parts of polyoxyethylene, a proper amount of a composite solvent composed of dimethylformamide and dichloromethane with the volume ratio of 1:1, 0.3-0.5 parts of tert-butyl hydrogen peroxide, a proper amount of citric acid, a proper amount of an alkaline pH regulator AMP-95, and a proper amount of ethanol. The resin is added with the nano tin powder, the silicon carbide nano fibers and the graphene oxide, so that the resin is greatly enhanced in heat conduction and abrasion resistance. In addition, the resin is low in thermo-expansion coefficient and is high in high-temperature strength.

Description

A kind of high thermal conductivity graphene oxide melmac and preparation method thereof
Technical field
The present invention relates to melmac Material Field, particularly relate to a kind of high thermal conductivity graphene oxide melmac and preparation method thereof.
Background technology
Graphene is by the carbonaceous material with the cellular crystalline network of two dimensional surface of the tightly packed one-tenth of monolayer carbon atom, and the nanostructure of its uniqueness determines that it has the performance of a series of excellence, and theoretical specific surface area is up to 2600 ㎡/g; Thermal conductivity is up to 5000W/ (m.K), for adamantine 5 times, intensity is the highest in known materials, reach 130GPa, it is more than 100 times of steel, at present, Graphene is considered to have a wide range of applications space in functional composite material, nano-device, energy storage material and support of the catalyst etc.
Utilize the excellent properties of Graphene, prepare Graphene/polymer composites, first the problem of Graphene stable dispersion in the polymer will be solved, surface of graphene oxide is with many oxygen-containing functional groups, although oxygenizement to a certain degree destroys the crystalline network of Graphene, but the interaction that these functional groups can be strong with polymer formation, thus improve the performance of matrix material.The method preparing graphene oxide/polymer composites mainly contains solution blended process, melt-blending process, in-situ polymerization intercalated method.
Melmac and melamine formaldehyde resin are a kind of widely used thermosetting resines.By using graphene oxide to carry out polymeric modification, the thermostability of resin can be improved, electroconductibility, thermal conductivity.But the improvement in performance of single graphene oxide to resin is limited, also need the performance further improving resin, can by improving technique and the performance becoming to assign to improve resin; Such as need to improve intensity, water-resistant capacity, thermostability, wear resistance, hardness, to the resistivity of chemicals, the performance such as poor toughness is easily broken, the shelf lives is short, make this resin widely for aspects such as furniture, vehicle, buildings.
Summary of the invention
The object of the present invention is to provide a kind of high thermal conductivity graphene oxide melmac, this resin thermal conductivity, wear resistance are good, and thermal expansivity is low, and hot strength is large.
Technical scheme of the present invention is as follows:
A kind of high thermal conductivity graphene oxide melmac, it is characterized in that being made up of the raw material of following weight part: nanometer glass putty 0.3-0.5, SiC nano fiber 0.4-0.6, trimeric cyanamide 20-25, 37% formalin 40-45, graphene oxide 1.8-2.1, trifluoroethyl methacrylate 0.7-0.9, polyacrylonitrile 0.7-0.9, dimethyl formamide is appropriate, polyoxyethylene 0.2-0.3, dimethylformamide/dichloromethane volume ratio is that 1:1 double solvents is appropriate, tertbutyl peroxide 0.3-0.5, citric acid is appropriate, pH value regulator AMP-95 is appropriate for alkalescence, appropriate amount of ethanol.
The production method of described high thermal conductivity graphene oxide melmac, is characterized in that:
(1) polyacrylonitrile is dissolved in dimethyl formamide, is mixed with the solution of 4wt%; Polyoxyethylene being dissolved in dimethylformamide/dichloromethane volume ratio is 1:1 double solvents, be mixed with the solution of 4wt%, again above-mentioned two kinds of solution are mixed, add nanometer glass putty, SiC nano fiber, graphene oxide, stir, add trifluoroethyl methacrylate, tertbutyl peroxide again, be heated to 60-70 DEG C, stirring reaction 1-2 hour, filter, by filter cake ethanol purge 2-3 time, obtain the graphene oxide of modification.
(2) by trimeric cyanamide, 37% formalin mixing, be heated to 70-75 DEG C, stir until all dissolve, add the graphene oxide of the modification that (1) step obtains again, stir 10-20 minute, add alkaline pH value regulator AMP-95, regulate pH value to be 8-9, reaction 3-4 hour, obtains the melmac performed polymer containing graphene oxide;
(3) performed polymer is placed in 30 DEG C of vacuum drying ovens, except being 5-6 by citric acid adjust ph after anhydrating, solidify in 50 DEG C of baking ovens 8-9 hour shaping, obtain graphene oxide/melmac matrix material.
Beneficial effect of the present invention
Resin of the present invention with the addition of nanometer glass putty, SiC nano fiber, graphene oxide, and substantially increase the thermal conductivity of resin, wear resistance, and thermal expansivity is low, hot strength is large; Production technique of the present invention can improve the dispersing uniformity of graphene oxide, improves bonding strength, improves toughness and the anti-bending strength of melmac.
Embodiment
A kind of high thermal conductivity graphene oxide melmac, is made up of the raw material of following weight part (kilogram): nanometer glass putty 0.4, SiC nano fiber 0.5, trimeric cyanamide 23,37% formalin 43, graphene oxide 2, trifluoroethyl methacrylate 0.7-0.9, polyacrylonitrile 0.8, dimethyl formamide are appropriate, polyoxyethylene 0.2, dimethylformamide/dichloromethane volume ratio are that 1:1 double solvents is appropriate, appropriate, the alkaline pH value regulator AMP-95 of tertbutyl peroxide 0.4, citric acid is appropriate, appropriate amount of ethanol.
The production method of described high thermal conductivity graphene oxide melmac, is characterized in that:
(1) polyacrylonitrile is dissolved in dimethyl formamide, is mixed with the solution of 4wt%; Polyoxyethylene being dissolved in dimethylformamide/dichloromethane volume ratio is 1:1 double solvents, be mixed with the solution of 4wt%, again above-mentioned two kinds of solution are mixed, add nanometer glass putty, SiC nano fiber, graphene oxide, stir, add trifluoroethyl methacrylate, tertbutyl peroxide again, be heated to 65 DEG C, stirring reaction 1.5 hours, filter, by filter cake ethanol purge 2 times, obtain the graphene oxide of modification.
(2) by trimeric cyanamide, 37% formalin mixing, be heated to 73 DEG C, stir until all dissolve, add the graphene oxide of the modification that (1) step obtains again, stir 15 minutes, add alkaline pH value regulator AMP-95, regulate pH value to be 8.6, react 3.5 hours, obtain the melmac performed polymer containing graphene oxide;
(3) performed polymer is placed in 30 DEG C of vacuum drying ovens, except being 6 by citric acid adjust ph after anhydrating, solidify in 50 DEG C of baking ovens 8.6 hours shaping, obtain graphene oxide/melmac matrix material.
Experimental data:
The polypropylene of this embodiment is through extrusion moulding, and after tested, thermal conductivity is 0.55W/ (m ﹒ K), flexural strength 111MPa, water-intake rate < 0.1%.

Claims (2)

1. a high thermal conductivity graphene oxide melmac, it is characterized in that being made up of the raw material of following weight part: nanometer glass putty 0.3-0.5, SiC nano fiber 0.4-0.6, trimeric cyanamide 20-25, 37% formalin 40-45, graphene oxide 1.8-2.1, trifluoroethyl methacrylate 0.7-0.9, polyacrylonitrile 0.7-0.9, dimethyl formamide is appropriate, polyoxyethylene 0.2-0.3, dimethylformamide/dichloromethane volume ratio is that 1:1 double solvents is appropriate, tertbutyl peroxide 0.3-0.5, citric acid is appropriate, pH value regulator AMP-95 is appropriate for alkalescence, appropriate amount of ethanol.
2. the production method of high thermal conductivity graphene oxide melmac according to claim 1, is characterized in that:
(1) polyacrylonitrile is dissolved in dimethyl formamide, is mixed with the solution of 4wt%; Polyoxyethylene being dissolved in dimethylformamide/dichloromethane volume ratio is 1:1 double solvents, be mixed with the solution of 4wt%, again above-mentioned two kinds of solution are mixed, add nanometer glass putty, SiC nano fiber, graphene oxide, stir, add trifluoroethyl methacrylate, tertbutyl peroxide again, be heated to 60-70 DEG C, stirring reaction 1-2 hour, filter, by filter cake ethanol purge 2-3 time, obtain the graphene oxide of modification;
(2) by trimeric cyanamide, 37% formalin mixing, be heated to 70-75 DEG C, stir until all dissolve, add the graphene oxide of the modification that (1) step obtains again, stir 10-20 minute, add alkaline pH value regulator AMP-95, regulate pH value to be 8-9, reaction 3-4 hour, obtains the melmac performed polymer containing graphene oxide;
(3) performed polymer is placed in 30 DEG C of vacuum drying ovens, except being 5-6 by citric acid adjust ph after anhydrating, solidify in 50 DEG C of baking ovens 8-9 hour shaping, obtain graphene oxide/melmac matrix material.
CN201510220723.7A 2015-05-04 2015-05-04 High-heat-conductive graphene oxide melamine resin and preparation method of same Pending CN104817671A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108109317A (en) * 2017-11-13 2018-06-01 杭州师范大学 A kind of resistor-type detection/early warning sensor and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102174254A (en) * 2010-12-27 2011-09-07 东莞劲胜精密组件股份有限公司 Highly heat-conducting insulation engineering plastic and preparation method thereof
CN102719210A (en) * 2011-03-30 2012-10-10 中国科学院理化技术研究所 Adhesive with insulating and heat-conducting properties used at ultralow temperature
CN104292817A (en) * 2014-01-08 2015-01-21 上海智高贸易有限公司 Continuous fiber composite high thermal conductive material and processing technology thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102174254A (en) * 2010-12-27 2011-09-07 东莞劲胜精密组件股份有限公司 Highly heat-conducting insulation engineering plastic and preparation method thereof
CN102719210A (en) * 2011-03-30 2012-10-10 中国科学院理化技术研究所 Adhesive with insulating and heat-conducting properties used at ultralow temperature
CN104292817A (en) * 2014-01-08 2015-01-21 上海智高贸易有限公司 Continuous fiber composite high thermal conductive material and processing technology thereof

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Title
陈中华等: "氧化石墨烯/密胺树脂复合材料的制备及其热性能研究", 《功能材料》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108109317A (en) * 2017-11-13 2018-06-01 杭州师范大学 A kind of resistor-type detection/early warning sensor and application
CN108109317B (en) * 2017-11-13 2019-10-29 杭州师范大学 A kind of resistor-type fire detection/early warning sensor and application

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Application publication date: 20150805