CN107226998A - A kind of thermally curable polymer conductive material and preparation method thereof - Google Patents
A kind of thermally curable polymer conductive material and preparation method thereof Download PDFInfo
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- CN107226998A CN107226998A CN201710479801.4A CN201710479801A CN107226998A CN 107226998 A CN107226998 A CN 107226998A CN 201710479801 A CN201710479801 A CN 201710479801A CN 107226998 A CN107226998 A CN 107226998A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- C08K3/08—Metals
- C08K2003/0843—Cobalt
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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
- C08K2201/001—Conductive additives
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Manufacture Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses a kind of thermally curable polymer conductive material and preparation method thereof, include following components according to parts by weight:10 ~ 30 parts of epoxy resin, 10 ~ 20 parts of copper nano-wire, 5 ~ 10 parts of dicyanodiamine, 0.5 ~ 3.5 part of 2 ~ 8 parts of 0.5 ~ 7.5 part of 0.3 ~ 1.5 part of 1 ~ 5 part of 3 ~ 8 parts of 1 ~ 10 part of 5 ~ 14 parts of derivative, graphene, polyimides, melamine formaldehyde resin, polyurethane, phenolic resin, chopped carbon fiber, the adhesive of dimethyl urea.The preparation cost of the present invention is low, and copper nano-wire is cheap, can be mass-produced, and obtained conductive material intensity height, temperature tolerance, weather-resistant are good.
Description
Technical field
The invention belongs to electrician's electrical materials and appliances field, and in particular to a kind of thermally curable polymer conductive material and preparation method thereof.
Background technology
Epoxy resin is that a kind of physical-mechanical property is excellent, the outstanding engineering macromolecule chemical combination of production and application, manufacturability
Thing, for many years, has been widely used.
Wherein, the middle temperature of latency (120 DEG C) cured epoxy system using solidification-catalyst system and catalyzing as core is ground for many years
Sharpen, used in sqtructural adhesive, material prepreg engineering.
High polymer material, its electrical property generally belongs to dielectric substance or insulating materials.People are for utilization high polymer material
Some specialities, have begun to nonconducting high polymer material changing into conductive material, are nowadays widely used on electronic keyboard
Conductive rubber, conductive adhesive for many years etc. is used on electronic circuit;Also semi-conducting material is modified as, heating is used as
Body, electrode, resistance are used.This modification is mostly to add conductive material into nonconducting high polymer material to obtain.
The content of the invention
In view of the above-mentioned problems, the technical problem to be solved in the present invention is to provide a kind of thermally curable polymer conductive material and its
Preparation method, heat endurance is good, it is not easy to is influenceed by high temperature and changes electrical conductivity.
To achieve the above object, the technical scheme is that:A kind of thermally curable polymer conductive material, according to parts by weight
Including following components:10 ~ 30 parts of epoxy resin, 10 ~ 20 parts of copper nano-wire, 5 ~ 10 parts of dicyanodiamine, the derivative 5 of dimethyl urea
~ 14 parts, 1 ~ 10 part of graphene, 3 ~ 8 parts of polyimides, 1 ~ 5 part of melamine formaldehyde resin, 0.3 ~ 1.5 part of polyurethane, phenolic aldehyde tree
0.5 ~ 7.5 part of fat, 2 ~ 8 parts of chopped carbon fiber, 0.5 ~ 3.5 part of adhesive.
Further, the preparation method of the graphene is as follows:
Metallic copper, cobalt, nickel, ruthenium, the zinc sulphide of foam copper, foam cobalt, nickel foam or its combination and inert material support are provided
Grain or its combination are used as catalyst;
The catalyst is heated to after 600 ~ 1000 DEG C of reaction temperature and 30 ~ 60min of constant temperature, carbon source, hydrogen and protection is imported
Gas, carries out chemical vapour deposition reaction, 10 ~ 60min of reaction time;
It is 10 ~ 30 DEG C/min to control rate of temperature fall after completion of the reaction, is cooled to 20 ~ 25 DEG C;
Obtained product is removed into catalyst and supporter, the graphene is obtained.
Further, the gas flow of the carbon source, hydrogen and protective gas is 1 ~ 900sccm(Ml/min).
Further, the draw ratio of the copper nano-wire is 100 ~ 1000, the diameter dimension of the copper nano-wire for 20 ~
500nm;The graphene number of plies is 1 ~ 20, and graphene size is 1 ~ 2000 μm 2.
Further, described adhesive is selected from propane diols, Kynoar, polyvinylpyrrolidone, polyethylene glycol and gathered
One kind or their compositions in vinyl alcohol.
A kind of preparation method of thermally curable polymer conductive material, is mainly included the following steps that:
Step 1:Organic solution is prepared, adhesive is dissolved in the organic solvent that temperature is 40 ~ 50 DEG C;
Step 2:Copper nano-wire is prepared, the aqueous solution of divalent metal mantoquita is added into aliphatic alkylamine obtains mixed solution, and
And control the mol ratio of copper ion and alkylamine to be 1:1 ~ 20, then by mixed solution stirring sealing reaction, it is warming up to 100 ~ 200
60 ~ 90min of constant temperature after DEG C, is cooled back to normal temperature, and copper nano-wire is produced after carrying out centrifuge washing;
Step 3:Copper nano-wire, epoxy resin and remaining raw material are put into organic solution, under conditions of protective gas
Solidified after fully dispersed 2 ~ 24h, produce the thermally curable polymer electrically-conducting paint.
Further, the divalent metal mantoquita in the step 2 be copper chloride, copper sulphate and copper nitrate in one kind or
Their mixture.
Further, organic solvent described in the organic solvent in the step 1 is selected from styrene, perchloroethylene, three chloroethenes
One or more in alkene, ethylene glycol ether and triethanolamine.
The beneficial effects of the present invention are:The present invention provides a kind of thermally curable polymer conductive material, the ring mainly used
Oxygen tree fat and copper nano-wire are as raw material, and the curing agent of resin system, accelerator form the spy of latency intermediate temperature setting
Property, by adding the conductive material of graphene, epoxy resin resistivity is substantially reduced, the conductive pyrogenicity resin as semiconductor,
Epoxy resin and other resin systems can be by adding certain voltage, conductive pyrogenicity, being warming up to 120~150 DEG C of solidifications, no
External heat equipment construction is needed, production cost is reduced, no matter environment temperature is higher or lower can be solidified, not by environment
Condition is limited to.
The preparation cost of the present invention is low, and copper nano-wire is cheap, can be mass-produced, obtained conductive material intensity
Height, temperature tolerance, weather-resistant are good.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, do not limit
The fixed present invention.
Embodiment 1
A kind of thermally curable polymer conductive material, includes following components according to parts by weight:10 parts of epoxy resin, copper nano-wire 10
Part, 1 part of 3 parts of 1 part of 5 parts of derivative, graphene, polyimides, the melamine formaldehyde resin of 5 parts of dicyanodiamine, dimethyl urea,
0.3 part of polyurethane, 0.5 part of phenolic resin, 2 parts of chopped carbon fiber, 0.5 part of adhesive.
The preparation method of the graphene is as follows:
Metallic copper, cobalt, nickel, ruthenium, the zinc sulphide of foam copper, foam cobalt, nickel foam or its combination and inert material support are provided
Grain or its combination are used as catalyst;
The catalyst is heated to after 600 DEG C of reaction temperature and constant temperature 30min, carbon source, hydrogen and protective gas is imported, carried out
Chemical vapour deposition reaction, reaction time 10min;
It is 10 DEG C/min to control rate of temperature fall after completion of the reaction, is cooled to 20 DEG C;
Obtained product is removed into catalyst and supporter, the graphene is obtained.
The gas flow of the carbon source, hydrogen and protective gas is 1sccm(Ml/min).
The draw ratio of the copper nano-wire is 100, and the diameter dimension of the copper nano-wire is 20nm;The graphene number of plies
For 1, graphene size is 1 μm 2.
Described adhesive is in propane diols, Kynoar, polyvinylpyrrolidone, polyethylene glycol and polyvinyl alcohol
A kind of or their compositions.
A kind of preparation method of thermally curable polymer conductive material, is mainly included the following steps that:
Step 1:Organic solution is prepared, adhesive is dissolved in the organic solvent that temperature is 40 DEG C;
Step 2:Copper nano-wire is prepared, the aqueous solution of divalent metal mantoquita is added into aliphatic alkylamine obtains mixed solution, and
And control the mol ratio of copper ion and alkylamine to be 1:1, then by mixed solution stirring sealing reaction, it is warming up to after 100 DEG C permanent
Warm 60min, is cooled back to normal temperature, and copper nano-wire is produced after carrying out centrifuge washing;
Step 3:Copper nano-wire, epoxy resin and remaining raw material are put into organic solution, under conditions of protective gas
Solidified after fully dispersed 2h, produce the thermally curable polymer electrically-conducting paint.
Divalent metal mantoquita in the step 2 is a kind of in copper chloride, copper sulphate and copper nitrate or theirs is mixed
Compound.
Organic solvent described in organic solvent in the step 1 is selected from styrene, perchloroethylene, trichloro ethylene, ethene second
One or more in glycol ethers and triethanolamine.
Embodiment 2
A kind of thermally curable polymer conductive material, includes following components according to parts by weight:20 parts of epoxy resin, copper nano-wire 15
Part, 5 parts of 5 parts of 10 parts of derivative, graphene, polyimides, the melamine formaldehyde resin 3 of 8 parts of dicyanodiamine, dimethyl urea
Part, 1.2 parts of polyurethane, 5.5 parts of phenolic resin, 5 parts of chopped carbon fiber, 2.5 parts of adhesive.
The preparation method of the graphene is as follows:
Metallic copper, cobalt, nickel, ruthenium, the zinc sulphide of foam copper, foam cobalt, nickel foam or its combination and inert material support are provided
Grain or its combination are used as catalyst;
The catalyst is heated to after 800 DEG C of reaction temperature and constant temperature 40min, carbon source, hydrogen and protective gas is imported, carried out
Chemical vapour deposition reaction, reaction time 30min;
It is 20 DEG C/min to control rate of temperature fall after completion of the reaction, is cooled to 23 DEG C;
Obtained product is removed into catalyst and supporter, the graphene is obtained.
The gas flow of the carbon source, hydrogen and protective gas is 400sccm(Ml/min).
The draw ratio of the copper nano-wire is 500, and the diameter dimension of the copper nano-wire is 300nm;The graphene layer
Number is 15, and graphene size is 1000 μm 2.
Described adhesive is in propane diols, Kynoar, polyvinylpyrrolidone, polyethylene glycol and polyvinyl alcohol
A kind of or their compositions.
A kind of preparation method of thermally curable polymer conductive material, is mainly included the following steps that:
Step 1:Organic solution is prepared, adhesive is dissolved in the organic solvent that temperature is 45 DEG C;
Step 2:Copper nano-wire is prepared, the aqueous solution of divalent metal mantoquita is added into aliphatic alkylamine obtains mixed solution, and
And control the mol ratio of copper ion and alkylamine to be 1:10, then by mixed solution stirring sealing reaction, it is warming up to after 120 DEG C permanent
Warm 70min, is cooled back to normal temperature, and copper nano-wire is produced after carrying out centrifuge washing;
Step 3:Copper nano-wire, epoxy resin and remaining raw material are put into organic solution, under conditions of protective gas
Solidified after fully dispersed 12h, produce the thermally curable polymer electrically-conducting paint.
Divalent metal mantoquita in the step 2 is a kind of in copper chloride, copper sulphate and copper nitrate or theirs is mixed
Compound.
Organic solvent described in organic solvent in the step 1 is selected from styrene, perchloroethylene, trichloro ethylene, ethene second
One or more in glycol ethers and triethanolamine.
Embodiment 3
A kind of thermally curable polymer conductive material, includes following components according to parts by weight:30 parts of epoxy resin, copper nano-wire 20
Part, 8 parts of 10 parts of 14 parts of derivative, graphene, polyimides, the melamine formaldehyde resin 5 of 10 parts of dicyanodiamine, dimethyl urea
Part, 1.5 parts of polyurethane, 7.5 parts of phenolic resin, 8 parts of chopped carbon fiber, 3.5 parts of adhesive.
The preparation method of the graphene is as follows:
Metallic copper, cobalt, nickel, ruthenium, the zinc sulphide of foam copper, foam cobalt, nickel foam or its combination and inert material support are provided
Grain or its combination are used as catalyst;
The catalyst is heated to after 1000 DEG C of reaction temperature and constant temperature 60min, carbon source, hydrogen and protective gas is imported, enters
Row chemical vapour deposition reaction, reaction time 60min;
It is 30 DEG C/min to control rate of temperature fall after completion of the reaction, is cooled to 25 DEG C;
Obtained product is removed into catalyst and supporter, the graphene is obtained.
The gas flow of the carbon source, hydrogen and protective gas is 900sccm(Ml/min).
The draw ratio of the copper nano-wire is 1000, and the diameter dimension of the copper nano-wire is 500nm;The graphene layer
Number is 20, and graphene size is 2000 μm 2.
Described adhesive is in propane diols, Kynoar, polyvinylpyrrolidone, polyethylene glycol and polyvinyl alcohol
A kind of or their compositions.
A kind of preparation method of thermally curable polymer conductive material, is mainly included the following steps that:
Step 1:Organic solution is prepared, adhesive is dissolved in the organic solvent that temperature is 50 DEG C;
Step 2:Copper nano-wire is prepared, the aqueous solution of divalent metal mantoquita is added into aliphatic alkylamine obtains mixed solution, and
And control the mol ratio of copper ion and alkylamine to be 1:20, then by mixed solution stirring sealing reaction, it is warming up to after 200 DEG C permanent
Warm 90min, is cooled back to normal temperature, and copper nano-wire is produced after carrying out centrifuge washing;
Step 3:Copper nano-wire, epoxy resin and remaining raw material are put into organic solution, under conditions of protective gas
Solidified after fully dispersed 24h, produce the thermally curable polymer electrically-conducting paint.
Divalent metal mantoquita in the step 2 is a kind of in copper chloride, copper sulphate and copper nitrate or theirs is mixed
Compound.
Organic solvent described in organic solvent in the step 1 is selected from styrene, perchloroethylene, trichloro ethylene, ethene second
One or more in glycol ethers and triethanolamine.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (8)
1. a kind of thermally curable polymer conductive material, it is characterised in that include following components according to parts by weight:Epoxy resin 10 ~
30 parts, 10 ~ 20 parts of copper nano-wire, 5 ~ 10 parts of dicyanodiamine, 1 ~ 10 part of 5 ~ 14 parts of derivative, graphene, the polyamides of dimethyl urea
3 ~ 8 parts of imines, 1 ~ 5 part of melamine formaldehyde resin, 0.3 ~ 1.5 part of polyurethane, 0.5 ~ 7.5 part of phenolic resin, chopped carbon fiber 2
~ 8 parts, 0.5 ~ 3.5 part of adhesive.
2. a kind of thermally curable polymer conductive material according to claim 1, it is characterised in that the preparation of the graphene
Method is as follows:
Metallic copper, cobalt, nickel, ruthenium, the zinc sulphide of foam copper, foam cobalt, nickel foam or its combination and inert material support are provided
Grain or its combination are used as catalyst;
The catalyst is heated to after 600 ~ 1000 DEG C of reaction temperature and 30 ~ 60min of constant temperature, carbon source, hydrogen and protection is imported
Gas, carries out chemical vapour deposition reaction, 10 ~ 60min of reaction time;
It is 10 ~ 30 DEG C/min to control rate of temperature fall after completion of the reaction, is cooled to 20 ~ 25 DEG C;
Obtained product is removed into catalyst and supporter, the graphene is obtained.
3. a kind of thermally curable polymer conductive material according to claim 2, it is characterised in that the carbon source, hydrogen and
The gas flow of protective gas is 1 ~ 900sccm(Ml/min).
4. a kind of thermally curable polymer conductive material according to claim 1, it is characterised in that the length of the copper nano-wire
Footpath ratio is 100 ~ 1000, and the diameter dimension of the copper nano-wire is 20 ~ 500nm;The graphene number of plies is 1 ~ 20, graphene face
Product size is 1 ~ 2000 μm 2.
5. a kind of thermally curable polymer conductive material according to claim 1, it is characterised in that described adhesive is selected from third
One kind or their compositions in glycol, Kynoar, polyvinylpyrrolidone, polyethylene glycol and polyvinyl alcohol.
6. a kind of preparation method of thermally curable polymer conductive material, it is characterised in that mainly include the following steps that:
Step 1:Organic solution is prepared, adhesive is dissolved in the organic solvent that temperature is 40 ~ 50 DEG C;
Step 2:Copper nano-wire is prepared, the aqueous solution of divalent metal mantoquita is added into aliphatic alkylamine obtains mixed solution, and
And control the mol ratio of copper ion and alkylamine to be 1:1 ~ 20, then by mixed solution stirring sealing reaction, it is warming up to 100 ~ 200
60 ~ 90min of constant temperature after DEG C, is cooled back to normal temperature, and copper nano-wire is produced after carrying out centrifuge washing;
Step 3:Copper nano-wire, epoxy resin and remaining raw material are put into organic solution, under conditions of protective gas
Solidified after fully dispersed 2 ~ 24h, produce the thermally curable polymer electrically-conducting paint.
7. a kind of preparation method of thermally curable polymer conductive material according to claim 6, it is characterised in that the step
Divalent metal mantoquita in rapid 2 is a kind of or their mixture in copper chloride, copper sulphate and copper nitrate.
8. a kind of preparation method of thermally curable polymer conductive material according to claim 6, it is characterised in that the step
Organic solvent described in organic solvent in rapid 1 is selected from styrene, perchloroethylene, trichloro ethylene, ethylene glycol ether and three ethanol
One or more in amine.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108410314A (en) * | 2018-02-05 | 2018-08-17 | 东莞市大兴化工有限公司 | Antirusting paint, preparation method and applications |
Citations (4)
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CN102176338A (en) * | 2011-03-10 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Graphene/copper nanowire composite electric-conducting material and preparation method thereof |
CN102516708A (en) * | 2011-11-25 | 2012-06-27 | 中国电力科学研究院 | Composite core for power grid transmission line wire and preparation method thereof |
CN103525013A (en) * | 2013-10-17 | 2014-01-22 | 嘉兴市隆鑫碳纤维制品有限公司 | Conducting carbon fiber composite material as well as preparation method thereof |
CN103694640A (en) * | 2013-12-20 | 2014-04-02 | 北京郁懋科技有限责任公司 | Preparation method of conductive thermo-cured epoxy resin system |
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2017
- 2017-06-22 CN CN201710479801.4A patent/CN107226998A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102176338A (en) * | 2011-03-10 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Graphene/copper nanowire composite electric-conducting material and preparation method thereof |
CN102516708A (en) * | 2011-11-25 | 2012-06-27 | 中国电力科学研究院 | Composite core for power grid transmission line wire and preparation method thereof |
CN103525013A (en) * | 2013-10-17 | 2014-01-22 | 嘉兴市隆鑫碳纤维制品有限公司 | Conducting carbon fiber composite material as well as preparation method thereof |
CN103694640A (en) * | 2013-12-20 | 2014-04-02 | 北京郁懋科技有限责任公司 | Preparation method of conductive thermo-cured epoxy resin system |
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CN108410314A (en) * | 2018-02-05 | 2018-08-17 | 东莞市大兴化工有限公司 | Antirusting paint, preparation method and applications |
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Application publication date: 20171003 |