CN104817673A - Heat-resistant graphene oxide melamine resin and preparation method of same - Google Patents
Heat-resistant graphene oxide melamine resin and preparation method of same Download PDFInfo
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- CN104817673A CN104817673A CN201510220740.0A CN201510220740A CN104817673A CN 104817673 A CN104817673 A CN 104817673A CN 201510220740 A CN201510220740 A CN 201510220740A CN 104817673 A CN104817673 A CN 104817673A
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Abstract
A heat-resistant graphene oxide melamine resin is prepared from following raw materials, by weight: 0.5-0.8 parts of titanium dioxide nano tube, 20-25 parts of melamine, 40-45 parts of 37% formalin, 1.8-2.1 parts of graphene oxide, 1-1.5 parts of trifluoroethyl methylacrylate, 1-1.5 parts of polyacrylonitrile, a proper amount of dimethylformamide, 0.3-0.5 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 graphene oxide so that the resin is increased in heat conduction coefficient by 40% than that of resin without the graphene oxide. By means of addition of the titanium dioxide nano tube, the resin is enhanced in resistances on chemical corrosion and photo corrosion and is enhanced in toughness. A preparation method can improve the toughness and flexural behavior of the melamine resin.
Description
Technical field
The present invention relates to melmac Material Field, particularly relate to a kind of thermotolerance 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 thermotolerance graphene oxide melmac, this resin thermal conductivity, resist chemical and fast light corrodibility, good toughness.
Technical scheme of the present invention is as follows:
A kind of thermotolerance graphene oxide melmac, is characterized in that being made up of the raw material of following weight part: titania nanotube 0.5-0.8, trimeric cyanamide 20-25,37% formalin 40-45, graphene oxide 1.8-2.1, trifluoroethyl methacrylate 1-1.5, polyacrylonitrile 1-1.5, dimethyl formamide are appropriate, polyoxyethylene 0.3-0.5, dimethylformamide/dichloromethane volume ratio are that 1:1 double solvents is appropriate, appropriate, the alkaline pH value regulator AMP-95 of tertbutyl peroxide 0.3-0.5, citric acid is appropriate, appropriate amount of ethanol.
The production method of described thermotolerance 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 titania nanotube, 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.
Beneficial effect of the present invention
Resin of the present invention with the addition of graphene oxide, the resin making resin thermal conductivity not add graphene oxide improves 40%, by adding titania nanotube, improves the resist chemical of resin and fast light corrodibility, improve the toughness of resin, prevent cracking; The melmac structure of this modification is more stable, and thermostability improves a lot; Production technique of the present invention can improve the dispersing uniformity of titania nanotube, graphene oxide, improves bonding strength, improves toughness and the anti-bending strength of melmac.
Embodiment
A kind of thermotolerance graphene oxide melmac, is made up of the raw material of following weight part (kilogram): titania nanotube 0.6, trimeric cyanamide 23,37% formalin 43, graphene oxide 2.5, trifluoroethyl methacrylate .3, polyacrylonitrile 1.3, dimethyl formamide are appropriate, polyoxyethylene 0.4, 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 thermotolerance 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 titania nanotube, 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, 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 after anhydrating with citric acid adjust ph be solidify in 5,50 DEG C of baking ovens 8 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 0.49W/ (m ﹒ K), flexural strength 110MPa, water-intake rate < 0.1%.
Claims (2)
1. a thermotolerance graphene oxide melmac, is characterized in that being made up of the raw material of following weight part: titania nanotube 0.5-0.8, trimeric cyanamide 20-25,37% formalin 40-45, graphene oxide 1.8-2.1, trifluoroethyl methacrylate 1-1.5, polyacrylonitrile 1-1.5, dimethyl formamide are appropriate, polyoxyethylene 0.3-0.5, dimethylformamide/dichloromethane volume ratio are that 1:1 double solvents is appropriate, appropriate, the alkaline pH value regulator AMP-95 of tertbutyl peroxide 0.3-0.5, citric acid is appropriate, appropriate amount of ethanol.
2. the production method of thermotolerance 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 titania nanotube, 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.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107987470A (en) * | 2017-12-20 | 2018-05-04 | 贺州宝兴新材料有限公司 | A kind of production technology of the compound melamine resin of antibacterial graphene oxide |
CN108084644A (en) * | 2017-12-20 | 2018-05-29 | 贺州宝兴新材料有限公司 | A kind of preparation method of the compound melamine resin of heat resistance graphene oxide |
CN108084492A (en) * | 2017-12-20 | 2018-05-29 | 贺州宝兴新材料有限公司 | A kind of production technology of the compound melamine resin of heat resistance graphene oxide |
CN109135017A (en) * | 2018-08-29 | 2019-01-04 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of thermo oxidative aging high-strength thermoplastic plastics |
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CN103304777A (en) * | 2013-07-04 | 2013-09-18 | 苏州瀚海高分子有限公司 | Titanium dioxide nanotube-epoxy resin composite flame retardant material and preparation method thereof |
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2015
- 2015-05-04 CN CN201510220740.0A patent/CN104817673A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103304777A (en) * | 2013-07-04 | 2013-09-18 | 苏州瀚海高分子有限公司 | Titanium dioxide nanotube-epoxy resin composite flame retardant material and preparation method thereof |
Non-Patent Citations (2)
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伍昱: "二氧化钛纳米管的掺杂与表面功能化及其聚合物复合材料热稳定性与阻燃性能的研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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 (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107987470A (en) * | 2017-12-20 | 2018-05-04 | 贺州宝兴新材料有限公司 | A kind of production technology of the compound melamine resin of antibacterial graphene oxide |
CN108084644A (en) * | 2017-12-20 | 2018-05-29 | 贺州宝兴新材料有限公司 | A kind of preparation method of the compound melamine resin of heat resistance graphene oxide |
CN108084492A (en) * | 2017-12-20 | 2018-05-29 | 贺州宝兴新材料有限公司 | A kind of production technology of the compound melamine resin of heat resistance graphene oxide |
CN109135017A (en) * | 2018-08-29 | 2019-01-04 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of thermo oxidative aging high-strength thermoplastic plastics |
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Application publication date: 20150805 |