CN108084492A - A kind of production technology of the compound melamine resin of heat resistance graphene oxide - Google Patents
A kind of production technology of the compound melamine resin of heat resistance graphene oxide Download PDFInfo
- Publication number
- CN108084492A CN108084492A CN201711384493.3A CN201711384493A CN108084492A CN 108084492 A CN108084492 A CN 108084492A CN 201711384493 A CN201711384493 A CN 201711384493A CN 108084492 A CN108084492 A CN 108084492A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- melamine resin
- melamine
- resin
- compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
- C08G12/42—Chemically modified polycondensates by etherifying
- C08G12/428—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic and acyclic or carbocyclic compounds
-
- 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
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention discloses a kind of production technologies of the compound melamine resin of heat resistance graphene oxide, include the following steps：(1) preparation of modified graphene oxide, (2) preparation of compound melamine resin, (3) preparation of the melamine resin performed polymer containing graphene oxide, the preparation of (4) graphene oxide/melamine resin composite material.Resin of the present invention is with the addition of graphene oxide so that resin thermal conductivity factor improves 40% compared with the resin for being not added with graphene oxide, by adding titania nanotube, improves the resist chemical of resin and fast light corrosivity, improves the toughness of resin；Production technology of the present invention improves the toughness and anti-bending strength of melamine resin.
Description
Technical field
The present invention relates to melamine resin Material Field more particularly to a kind of compound melamine resins of heat resistance graphene oxide
Production technology.
Background technology
Graphene be by single layer of carbon atom it is tightly packed into the carbonaceous material with two dimensional surface honeycomb crystal lattice structure,
Its unique nanostructured determines it with a series of excellent performances, and theoretical specific surface area is up to 2600 ㎡/g；Thermal conductivity factor
Up to 5000W/ (m.K) is 5 times of diamond, and intensity is highest in known materials, is more than 100 times of steel up to 130GPa,
At present, graphene is considered having extensively in functional composite material, nano-device, energy storage material and catalyst carrier etc.
General application space.
Using the excellent properties of graphene, graphene/polymer composites are prepared, solution graphene is first had to and is polymerizeing
In object the problem of stable dispersion, surface of graphene oxide band is there are many oxygen-containing functional group, although oxidation is destroyed to a certain degree
The lattice structure of graphene, but these functional groups can form strong interaction with polymer, so as to improve composite wood
The performance of material.The method for preparing graphene oxide/polymer composites mainly has solution blended process, melt-blending process, original position
It polymerize graft process.
Melamine resin, that is, melamine formaldehyde resin is a kind of widely used thermosetting plastics.By using oxidation
Graphene carries out polymeric modification, can improve the thermal stability of resin, electric conductivity, thermal conductivity.But single graphene oxide
It is limited to the performance improvement of resin, it is also necessary to the performance of resin is further improved, can by improve technique and ingredient come
Improve the performance of resin；Such as it needs to improve intensity, water-resistant capacity, thermal stability, wearability, hardness, chemicals supported
The performances such as anti-ability, poor toughness are easily rupturable, Storage period is short so that the resin is more broadly useful for the side such as furniture, vehicle, building
Face.
The content of the invention
The present invention seeks to be intended to provide a kind of production technology of the compound melamine resin of heat resistance graphene oxide, the party
Resin thermal conductivity, resist chemical and fast light corrosivity, good toughness prepared by method.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
A kind of production technology of the compound melamine resin of heat resistance graphene oxide, includes the following steps,
(1) preparation of modified graphene oxide
Polyacrylonitrile is dissolved in dimethylformamide, is configured to the solution of 4wt%；Polyethylene glycol oxide is dissolved in dichloromethane
In alkane solvents, the solution of 4wt% is configured to, then above two solution is uniformly mixed, adds in titania nanotube, oxidation stone
Black alkene, stirs evenly, and adds trifluoroethyl methacrylate, tert-butyl hydroperoxide, is heated to 60-70 DEG C, is stirred to react
Filter cake with ethyl alcohol is cleaned 2-3 times, obtains modified graphene oxide by 1-2 hour, filtering；
(2) preparation of compound melamine resin
A, formalin, melamine, hexa are added in reaction kettle to react under agitation, three
The molar ratio of poly cyanamid and 37% formalin prepolymerization reaction, melamine and formaldehyde is 1:2-3, control ph 8-8.5, control
85-105 DEG C of pre-polymerization temperature processed, pre-polymerization time are 70-120min, and the quality of hexa is the 4- of melamine quality
12%；
B, add polyethylene glycol and carry out polycondensation reaction, control ph 5-6, the quality of polyethylene glycol is melamine quality
40-60%, wherein the molecular weight of polyethylene glycol be 800-1500；45-55 DEG C of condensation temperature is controlled, the polycondensation time is 80-
100min obtains compound melamine resin；
(3) preparation of the melamine resin performed polymer containing graphene oxide
Graphene oxide obtained in step (1) is added in the compound melamine resin in step (2), is stirred
It mixes 10-20 minutes, adds in alkaline pH adjuster, adjusting pH value is 8-9, when reaction 3-4 is small, is obtained containing graphene oxide
Melamine resin performed polymer；
(4) preparation of graphene oxide/melamine resin composite material
Performed polymer is placed in 30 DEG C of vacuum drying ovens, pH value is adjusted as 5-6 after removing water, it is small to cure 8-9 in 50 DEG C of baking ovens
When be molded, obtain graphene oxide/melamine resin composite material.
It further limits, the rate of charge of modified graphene oxide and compound melamine resin is 1:1.6-1:
2.8。
It further limits, the pH adjusting agent in step (3) is sodium hydroxide.
Claims (3)
1. a kind of production technology of the compound melamine resin of heat resistance graphene oxide, it is characterised in that：Include the following steps,
(1) preparation of modified graphene oxide
Polyacrylonitrile is dissolved in dimethylformamide, is configured to the solution of 4wt%；It is molten that polyethylene glycol oxide is dissolved in dichloromethane
In agent, the solution of 4wt% is configured to, then above two solution is uniformly mixed, adds in titania nanotube, graphite oxide
Alkene stirs evenly, and adds trifluoroethyl methacrylate, tert-butyl hydroperoxide, is heated to 60-70 DEG C, is stirred to react 1-2
Filter cake with ethyl alcohol is cleaned 2-3 times, obtains modified graphene oxide by a hour, filtering；
(2) preparation of compound melamine resin
A, formalin, melamine, hexa are added in reaction kettle to react under agitation, melamine
The molar ratio of amine and 37% formalin prepolymerization reaction, melamine and formaldehyde is 1:2-3, control ph 8-8.5, control are pre-
Poly- 85-105 DEG C of temperature, pre-polymerization time are 70-120min, and the quality of hexa is the 4-12% of melamine quality；
B, add polyethylene glycol and carry out polycondensation reaction, control ph 5-6, the quality of polyethylene glycol is melamine quality
The molecular weight of 40-60%, wherein polyethylene glycol are 800-1500；45-55 DEG C of condensation temperature is controlled, the polycondensation time is 80-
100min obtains compound melamine resin；
(3) preparation of the melamine resin performed polymer containing graphene oxide
Graphene oxide obtained in step (1) is added in the compound melamine resin in step (2), is stirred
10-20 minutes, alkaline pH adjuster is added in, adjusting pH value is 8-9, when reaction 3-4 is small, obtains the melamine containing graphene oxide
Resin prepolymer；
(4) preparation of graphene oxide/melamine resin composite material
Performed polymer is placed in 30 DEG C of vacuum drying ovens, it is 5-6 to remove and adjust pH value after water, cure in 50 DEG C of baking ovens 8-9 it is small when into
Type obtains graphene oxide/melamine resin composite material.
2. a kind of production technology of the compound melamine resin of environmentally friendly graphene oxide according to claim 1, it is characterised in that：
The rate of charge of modified graphene oxide and compound melamine resin is 1:1.6-1:2.8.
3. a kind of production technology of the compound melamine resin of environmentally friendly graphene oxide according to claim 2, it is characterised in that：
PH adjusting agent in step (3) is sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711384493.3A CN108084492A (en) | 2017-12-20 | 2017-12-20 | A kind of production technology of the compound melamine resin of heat resistance graphene oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711384493.3A CN108084492A (en) | 2017-12-20 | 2017-12-20 | A kind of production technology of the compound melamine resin of heat resistance graphene oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108084492A true CN108084492A (en) | 2018-05-29 |
Family
ID=62177490
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711384493.3A Withdrawn CN108084492A (en) | 2017-12-20 | 2017-12-20 | A kind of production technology of the compound melamine resin of heat resistance graphene oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108084492A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705816A (en) * | 2019-02-18 | 2019-05-03 | 西南交通大学 | Multifunction flexible phase-change material, preparation method and construction material |
| CN113948691A (en) * | 2021-10-15 | 2022-01-18 | 佛山科学技术学院 | Titanium dioxide composite material and application thereof as energy storage material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN104817674A (en) * | 2015-05-04 | 2015-08-05 | 芜湖市宝艺游乐科技设备有限公司 | Flame-retarding and heat-resistant graphene oxide melamine resin and preparation method of same |
| CN104817673A (en) * | 2015-05-04 | 2015-08-05 | 芜湖市宝艺游乐科技设备有限公司 | Heat-resistant graphene oxide melamine resin and preparation method of same |
| CN104945584A (en) * | 2015-05-04 | 2015-09-30 | 芜湖市宝艺游乐科技设备有限公司 | Photoaging-resistant graphene oxide melamine resin and preparation method thereof |
| CN105218771A (en) * | 2015-10-29 | 2016-01-06 | 江苏润钰新材料科技有限公司 | A kind of preparation method of melmac |
-
2017
- 2017-12-20 CN CN201711384493.3A patent/CN108084492A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN104817674A (en) * | 2015-05-04 | 2015-08-05 | 芜湖市宝艺游乐科技设备有限公司 | Flame-retarding and heat-resistant graphene oxide melamine resin and preparation method of same |
| CN104817673A (en) * | 2015-05-04 | 2015-08-05 | 芜湖市宝艺游乐科技设备有限公司 | Heat-resistant graphene oxide melamine resin and preparation method of same |
| CN104945584A (en) * | 2015-05-04 | 2015-09-30 | 芜湖市宝艺游乐科技设备有限公司 | Photoaging-resistant graphene oxide melamine resin and preparation method thereof |
| CN105218771A (en) * | 2015-10-29 | 2016-01-06 | 江苏润钰新材料科技有限公司 | A kind of preparation method of melmac |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705816A (en) * | 2019-02-18 | 2019-05-03 | 西南交通大学 | Multifunction flexible phase-change material, preparation method and construction material |
| CN113948691A (en) * | 2021-10-15 | 2022-01-18 | 佛山科学技术学院 | Titanium dioxide composite material and application thereof as energy storage material |
| CN113948691B (en) * | 2021-10-15 | 2023-03-10 | 佛山科学技术学院 | Titanium dioxide composite material and application thereof as energy storage material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110461814B (en) | Resin blends, prepregs and articles containing a phthalonitrile reactive diluent and a bisphthalonitrile resin | |
| CN104804159A (en) | Graphene oxide melamine resin and preparation method thereof | |
| JP2006183032A5 (en) | ||
| CN107108827B (en) | Benzoxazine and composition containing benzoxazine | |
| CN101700705A (en) | Thermosetting resin glass fiber laminating composite material and preparation method thereof | |
| CN108084492A (en) | A kind of production technology of the compound melamine resin of heat resistance graphene oxide | |
| JPS5865716A (en) | Heterocyclic polyfunctional amine adduct | |
| CN103850124A (en) | Interface modified carbon fiber/resin matrix composite material and preparation method thereof | |
| CN107987469A (en) | A kind of production technology of the compound melamine resin of environmental protection graphene oxide | |
| CN104177696A (en) | Filling material master batch used for non-woven fabrics and preparing process thereof | |
| Kiskan et al. | Benzoxazine resins as smart materials and future perspectives | |
| CN104817674A (en) | Flame-retarding and heat-resistant graphene oxide melamine resin and preparation method of same | |
| CN102199265B (en) | Long carbon chain nylon modified phenolic resin and preparation method thereof | |
| CN104817673A (en) | Heat-resistant graphene oxide melamine resin and preparation method of same | |
| CN104804160A (en) | Environment-friendly oxidized graphene melamine resin and preparation method thereof | |
| CN104804161A (en) | Antibacterial graphene oxide composite melamine resin and preparation method thereof | |
| JP2019513156A (en) | Novel heterodiels alder crosslinker and its use in a reversible crosslinkable polymer system | |
| CN107987468A (en) | A kind of production technology of the compound melamine resin of high dielectric property graphene oxide | |
| TW201823319A (en) | Novel crosslinker unit for use in reversibly crosslinking polymer systems | |
| JP2009030052A (en) | Method for creating preceramic silazane polymer, and preceramic polymer composition | |
| CN108329836A (en) | A kind of organic siliconresin that rosin resin is modified | |
| CN104804157A (en) | Anti-abrasion graphene oxide composite melamine resin and preparation method thereof | |
| CN104910583A (en) | High-dielectric graphene oxide melamine resin and preparation method thereof | |
| CN107987470A (en) | A kind of production technology of the compound melamine resin of antibacterial graphene oxide | |
| CN107987464A (en) | A kind of preparation method of the compound melamine resin of environmental protection graphene oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180529 |
|
| WW01 | Invention patent application withdrawn after publication |