CN104804375A - High-tenacity oxidized graphene melamine resin and preparation method thereof - Google Patents

High-tenacity oxidized graphene melamine resin and preparation method thereof Download PDF

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Publication number
CN104804375A
CN104804375A CN201510220458.2A CN201510220458A CN104804375A CN 104804375 A CN104804375 A CN 104804375A CN 201510220458 A CN201510220458 A CN 201510220458A CN 104804375 A CN104804375 A CN 104804375A
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Prior art keywords
graphene oxide
resin
melmac
appropriate
oxidized graphene
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CN201510220458.2A
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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 CN201510220458.2A priority Critical patent/CN104804375A/en
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Abstract

The invention discloses a high-tenacity oxidized graphene melamine resin. The high-tenacity oxidized graphene melamine resin is prepared from the following raw materials in parts by weight: 1.6-2.1 parts of nano-crystalline cellulose, 0.2-0.3 part of rare earth cerium fluoride, 20-25 parts of melamine, 40-45 parts of 37% formaldehyde solution, 1.8-2.1 parts of oxidized graphene, 0.7-0.9 part of trifluoroethyl methacrylate, 0.7-0.9 part of polyacrylonitrile, a proper amount of dimethyl formamide, 0.2-0.3 part of polyoxyethylene, a proper amount of composite solvent comprising dimethyl formamide and dichloromethane of which the volume ratio is 1: 1, 0.3-0.5 part of tert-butyl hydroperoxide, a proper amount of citric acid, a proper amount of alkaline pH value modifier AMP-95 and a proper amount of ethyl alcohol. The resin disclosed by the invention is added with the oxidized graphene, so that the heat conductivity coefficient of the resin is improved by 41% compared with that of resin without adding oxidized graphene; by adding the nano-crystalline cellulose, the tenacity of the resin is improved, and the resin is prevented from cracking; by adding the rare earth cerium fluoride, the resin has a fluorescent effect.

Description

A kind of high tenacity graphene oxide melmac and preparation method thereof
Technical field
The present invention relates to melmac Material Field, particularly relate to a kind of high tenacity 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 tenacity graphene oxide melmac, this resin thermal conductivity is good, and good toughness, has fluorescent effect.
Technical scheme of the present invention is as follows:
A kind of high tenacity graphene oxide melmac, it is characterized in that being made up of the raw material of following weight part: nano cellulose crystal 1.6-2.1, rare earth cerium fluoride 0.2-0.3, 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 tenacity 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 nano cellulose crystal, rare earth cerium fluoride, 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 graphene oxide, and the resin making resin thermal conductivity not add graphene oxide improves 41%, by adding nano cellulose crystal, improves the toughness of resin, prevents cracking; By adding rare earth cerium fluoride, resin is made to have fluorescent effect; 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 tenacity graphene oxide melmac, is made up of the raw material of following weight part (kilogram): nano cellulose crystal 1.9, rare earth cerium fluoride 0.2, 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 tenacity 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 nano cellulose crystal, rare earth cerium fluoride, 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 0.40W/ (m ﹒ K), flexural strength 102MPa, water-intake rate < 0.1%.

Claims (2)

1. a high tenacity graphene oxide melmac, it is characterized in that being made up of the raw material of following weight part: nano cellulose crystal 1.6-2.1, rare earth cerium fluoride 0.2-0.3, 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 tenacity 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 nano cellulose crystal, rare earth cerium fluoride, 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.
CN201510220458.2A 2015-05-04 2015-05-04 High-tenacity oxidized graphene melamine resin and preparation method thereof Pending CN104804375A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107759972A (en) * 2017-12-07 2018-03-06 郑州峰泰纳米材料有限公司 A kind of high heat-resisting graphene oxide melamine resin and preparation method thereof
CN107857971A (en) * 2017-12-07 2018-03-30 郑州峰泰纳米材料有限公司 A kind of flame retardant type graphene oxide melamine resin and preparation method thereof
CN107903580A (en) * 2017-12-07 2018-04-13 郑州峰泰纳米材料有限公司 A kind of high tenacity graphene oxide melamine resin and preparation method thereof
CN108070209A (en) * 2017-12-21 2018-05-25 贺州宝兴新材料有限公司 A kind of preparation method of high tenacity melamine resin
CN108192148A (en) * 2018-01-31 2018-06-22 厦门大学 A kind of preparation method for the cellulose acetate composite film for adulterating graphene oxide and rare earth compounding
CN108822549A (en) * 2018-06-28 2018-11-16 宁波蒙曼生物科技有限公司 A kind of bicomponent condensed type room temperature sulfidization silicon rubber and its preparation
CN113429740A (en) * 2021-07-21 2021-09-24 开化瑞达塑胶科技有限公司 Preparation method of cellulose nanowhisker reinforced modified melamine molding compound
CN113604113A (en) * 2021-07-22 2021-11-05 广州大学 Hydrophobic melamine resin nano soil/polyethylene anticorrosive composite coating for carbon steel surface and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
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CN103855320A (en) * 2012-11-30 2014-06-11 海洋王照明科技股份有限公司 Organic light-emitting device and preparation method thereof
CN103881523A (en) * 2014-02-14 2014-06-25 程实 LED (Light-Emitting Diode) radiating coating capable of absorbing electromagnetic wave and preparation method thereof

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CN103855320A (en) * 2012-11-30 2014-06-11 海洋王照明科技股份有限公司 Organic light-emitting device and preparation method thereof
CN103881523A (en) * 2014-02-14 2014-06-25 程实 LED (Light-Emitting Diode) radiating coating capable of absorbing electromagnetic wave and preparation method thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107759972A (en) * 2017-12-07 2018-03-06 郑州峰泰纳米材料有限公司 A kind of high heat-resisting graphene oxide melamine resin and preparation method thereof
CN107857971A (en) * 2017-12-07 2018-03-30 郑州峰泰纳米材料有限公司 A kind of flame retardant type graphene oxide melamine resin and preparation method thereof
CN107903580A (en) * 2017-12-07 2018-04-13 郑州峰泰纳米材料有限公司 A kind of high tenacity graphene oxide melamine resin and preparation method thereof
CN108070209A (en) * 2017-12-21 2018-05-25 贺州宝兴新材料有限公司 A kind of preparation method of high tenacity melamine resin
CN108192148A (en) * 2018-01-31 2018-06-22 厦门大学 A kind of preparation method for the cellulose acetate composite film for adulterating graphene oxide and rare earth compounding
CN108822549A (en) * 2018-06-28 2018-11-16 宁波蒙曼生物科技有限公司 A kind of bicomponent condensed type room temperature sulfidization silicon rubber and its preparation
CN113429740A (en) * 2021-07-21 2021-09-24 开化瑞达塑胶科技有限公司 Preparation method of cellulose nanowhisker reinforced modified melamine molding compound
CN113604113A (en) * 2021-07-22 2021-11-05 广州大学 Hydrophobic melamine resin nano soil/polyethylene anticorrosive composite coating for carbon steel surface and preparation method and application thereof

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Application publication date: 20150729