CN108165198B - A kind of highly conductive epoxyn and preparation method thereof - Google Patents
A kind of highly conductive epoxyn and preparation method thereof Download PDFInfo
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- CN108165198B CN108165198B CN201810086853.XA CN201810086853A CN108165198B CN 108165198 B CN108165198 B CN 108165198B CN 201810086853 A CN201810086853 A CN 201810086853A CN 108165198 B CN108165198 B CN 108165198B
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- epoxyn
- conductive
- highly conductive
- carbon
- curing agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
-
- 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
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/53—Core-shell polymer
Abstract
The invention belongs to epoxide-resin glue technical fields, more particularly to a kind of highly conductive epoxyn and preparation method thereof, a kind of highly conductive epoxyn, including the following raw material: epoxy resin, toughener, curing agent, organometallic polymer, carbon conductive filler, wherein, the ratio of epoxy resin and toughener is 9:1-81, pass through the conductive synergistic effect of organometallic polymer and carbon conductive filler in the present invention, in the case where guaranteeing that adhesive easily disperses, storage stability is good and situation with good conductivity, the cost of adhesive is greatly reduced；A kind of preparation method of highly conductive epoxyn is also disclosed in the present invention, and this method process is convenient, operation is simple.
Description
Technical field
The invention belongs to epoxide-resin glue technical fields, and in particular to a kind of highly conductive epoxyn and its system
Preparation Method.
Background technique
The research of conductive polymer composite begin in the 1960s, its industrial applications be in the mid-1970s, this
The application study development of the material is very fast afterwards.Insulated type high molecular material has good electric conductivity because of incorporation conductive filler two
Can, and preparation method is simple and easy, is widely used in the industries such as electronics, communication, thermal control and the energy at present.Wherein epoxy
Resin thermoset conductive polymer material is Typical Representative, since it is easy to get with raw material, the processing is simple and heat resistance is preferable
The advantages that, therefore can be widely used for the fields such as optoelectronic device, electromagnetic shielding, anti-static material and conducting resinl.
It is different by the type of conducting particles in conducting resinl, metal system and carbon series conductive glue can be divided into.Metal system conducting resinl tool
There is good electric conductivity, but disadvantage is expensive, the disadvantages of conductive metal and resin are easily layered and working life is short.Carbon system leads
Electric glue is low in cost, has absolute price advantage, but there is conductive fillers to disperse the drawbacks such as difficult, electric conductivity is low.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of electric conductivity is good
Epoxyn good, high mechanical strength, storage stability are good；Another object of the present invention is to provide a kind of technique letters
The preparation method of epoxyn single, maneuverable one kind is highly conductive.
The purpose of the invention is achieved by the following technical solution: a kind of highly conductive epoxyn, including as follows
Raw material:
Wherein, epoxy resin be one or both of CTBN modified epoxy or core shell rubbers modified epoxy,
And the ratio of epoxy resin and toughener is 9:1-81.
By the conductive synergistic effect of organometallic polymer and carbon conductive filler in the present invention, guaranteeing that adhesive is easy
Under dispersion, storage stability be good and situation with good conductivity, the cost of adhesive is greatly reduced.
Further, the highly conductive epoxyn includes following raw material:
Wherein, the ratio of epoxy resin and toughener is 9:1-81.
Further, the curing agent is amine curing agent.
Further, the curing agent be dicyandiamide, m-phenylene diamine (MPD), m-xylene diamine, 4,4 '-two amido diphenyl-methanes,
One of 4,4 '-two amido diphenyl sulphone (DPS)s or more than one.
Further, the carbon conductive filler is carbon black or graphite.
Further, the carbon conductive filler is crystalloid graphite, crystalline flake graphite, graphite fibre, graphene, conductive charcoal
One of black, conductive carbon fibre or conductive carbon nanotube or more than one.
Further, the organometallic polymer end group contains the organometallic polymer of iron.
The preparation method of highly conductive epoxyn, includes the following steps: described in one
(1) after epoxy resin and toughener being mixed by the parts by weight preheat 20-30min under conditions of 60-70 DEG C,
Obtain mixture A；
(2) organometallic polymer, carbon conductive filler, curing agent of the parts by weight are added in mixture A, are stirred
60-120min is mixed, reactant B is obtained；
(3) after reactant B ultrasonic wave being dispersed 60-120min, then deaeration 20-60min obtains height and leads under vacuum conditions
The epoxyn of electricity.
Preparation method process of the invention is convenient, operation is simple, and the highly conductive epoxyn of preparation exists
The phenomenon that storage stability is good under room temperature, is not in layering or precipitating.
The beneficial effects of the present invention are: highly conductive epoxyn prepared by the present invention easily disperses, stores
Under stability is good and situation with good conductivity, the cost of adhesive is greatly reduced；Highly conductive ring is prepared in the present invention
The method flow of oxygen resin adhesive is convenient, operation is simple.
Specific embodiment
For the ease of the understanding of those skilled in the art, below with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1,
A kind of highly conductive epoxyn, including following raw material:
Wherein, epoxy resin is core shell rubbers modified epoxy；Curing agent is dicyandiamide；The carbon conductive filler is
Conductive black, organometallic polymer end group contain the organometallic polymer of iron.
A kind of preparation method of highly conductive epoxyn, includes the following steps:
(1) 20min is preheated under conditions of 60 DEG C after mixing epoxy resin and toughener by the parts by weight, is mixed
Close object A；
(2) organometallic polymer, carbon conductive filler, curing agent of the parts by weight are added in mixture A, are stirred
60min is mixed, reactant B is obtained；
(3) after reactant B ultrasonic wave being dispersed 60min, then deaeration 20min obtains highly conductive epoxy under vacuum conditions
Resin adhesive.
Embodiment 2,
Embodiment 2 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Embodiment 3
Embodiment 3 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Embodiment 4,
Embodiment 4 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Embodiment 5,
Embodiment 5 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Embodiment 6,
Embodiment 6 the difference from embodiment 1 is that: the epoxy resin is E44 and bisphenol F epoxy resin mass ratio is 1:
1 mixture.
Embodiment 7,
Embodiment 7 the difference from embodiment 1 is that: the curing agent be m-phenylene diamine (MPD).
Embodiment 8,
Embodiment 8 the difference from embodiment 1 is that: the curing agent be m-xylene diamine.
Embodiment 9,
Embodiment 9 the difference from embodiment 1 is that: the curing agent be 4,4 '-two amido diphenyl-methanes.
Embodiment 10,
Embodiment 10 the difference from embodiment 1 is that: the curing agent be 4,4 '-two amido diphenyl sulphone (DPS)s.
Embodiment 11
Embodiment 11 the difference from embodiment 1 is that: the curing agent is 4,4 '-two amido hexichol that molar ratio is 1:1
The mixture of methane and 4,4 '-two amido diphenyl sulphone (DPS)s.
Embodiment 12
Embodiment 12 the difference from embodiment 1 is that: the carbon conductive filler be crystalloid graphite.
Embodiment 13
Embodiment 13 the difference from embodiment 1 is that: the carbon conductive filler be conductive carbon nanotube.
Embodiment 14
Embodiment 14 the difference from embodiment 1 is that:
A kind of preparation method of highly conductive epoxyn, includes the following steps:
(1) 30min is preheated under conditions of 70 DEG C after mixing epoxy resin and toughener by the parts by weight, is mixed
Close object A；
(2) organometallic polymer, carbon conductive filler, curing agent of the parts by weight are added in mixture A, are stirred
120min is mixed, reactant B is obtained；
(3) after reactant B ultrasonic wave being dispersed 120min, then deaeration 60min obtains highly conductive ring under vacuum conditions
Oxygen resin adhesive.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Comparative example 3
Comparative example 3 the difference from embodiment 1 is that: a kind of highly conductive epoxyn, including following parts by weight
Raw material:
Highly conductive epoxyn prepared in above embodiments and comparative example is tested, test data is such as
Table 1:
Instrument and equipment
RGT-30 type microcomputer controlled electronic universal testing machine, Shenzhen Rui Geer Co., Ltd；ZC36 megger: Shanghai
Precision instrumentation Co., Ltd.Test index electrical property
Test index
Electrical property
Referring to national standard, the volume resistivity of casting resin sample is tested.
Mechanical property
By relevant national standard, the bending property and compressive strength, aluminium/aluminium adhesive strength of resin composite materials are tested.
Glue room temperature storage stability is investigated
Uncured composition epoxy resin at 25 DEG C it is closed save one week, then observe composition with the presence or absence of be layered or
Deposited phenomenon.
Table 1:
It can be obtained from the data of table 1, the adhesive of preparation of the invention conducts electricity very well, stable storage, is not easy to be layered.
Above-described embodiment is the preferable implementation of the present invention, but the present invention is not limited to above-mentioned detailed raw material proportioning and tool
Body operating method, without departing from the inventive concept of the premise it is any it is obvious replacement protection scope of the present invention it
It is interior.
Claims (5)
1. a kind of highly conductive epoxyn, it is characterised in that: including following raw material:
Wherein, epoxy resin is one or both of CTBN modified epoxy or core shell rubbers modified epoxy, and ring
The ratio of oxygen resin and toughener is 9:(1-81)；
The organometallic polymer is the organometallic polymer that end group contains iron；
The carbon conductive filler is crystalloid graphite, crystalline flake graphite, graphite fibre, graphene, conductive black, conductive carbon fibre
One of conductive carbon nanotube or more than one.
2. highly conductive epoxyn as described in claim 1, it is characterised in that: including following raw material:
3. highly conductive epoxyn as described in claim 1, it is characterised in that: the curing agent is amine-type cure
Agent.
4. highly conductive epoxyn as claimed in claim 3, it is characterised in that: the curing agent be dicyandiamide,
M-phenylene diamine (MPD), m-xylene diamine, 4,4 '-diaminodiphenylmethane, the one or more of 4,4 '-two amido diphenyl sulphone (DPS)s.
5. the preparation method of the highly conductive epoxyn as described in claim 1-4 is any, it is characterised in that: including
Following steps:
(1) 20-30min is preheated under conditions of 60-70 DEG C after mixing epoxy resin and toughener by the parts by weight, is obtained
Mixture A；
(2) organometallic polymer, carbon conductive filler, curing agent of the parts by weight are added in mixture A, are stirred
60-120min obtains reactant B；
(3) by reactant B ultrasonic wave disperse 60-120min after, then under vacuum conditions deaeration 20-60min obtain it is highly conductive
Epoxyn.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810086853.XA CN108165198B (en) | 2018-01-30 | 2018-01-30 | A kind of highly conductive epoxyn and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810086853.XA CN108165198B (en) | 2018-01-30 | 2018-01-30 | A kind of highly conductive epoxyn and preparation method thereof |
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| CN108165198B true CN108165198B (en) | 2019-07-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110684494A (en) * | 2019-10-12 | 2020-01-14 | 宇石能源(南通)有限公司 | Conductive adhesive for bonding bipolar plate of fuel cell and preparation method thereof |
| CN111334232A (en) * | 2020-04-28 | 2020-06-26 | 东莞市恒尔朗实业有限公司 | Weather-resistant intermediate-temperature curing epoxy resin adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128040A (en) * | 1993-06-16 | 1996-07-31 | 美国3M公司 | Electrically conductive adhesive compositions |
| CN101654605A (en) * | 2008-08-21 | 2010-02-24 | 中山市东溢新材料有限公司 | Modified epoxy resin adhesive and preparation method thereof |
| CN104099051A (en) * | 2014-07-04 | 2014-10-15 | 中国西电电气股份有限公司 | Epoxy resin adhesive |
-
2018
- 2018-01-30 CN CN201810086853.XA patent/CN108165198B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128040A (en) * | 1993-06-16 | 1996-07-31 | 美国3M公司 | Electrically conductive adhesive compositions |
| CN101654605A (en) * | 2008-08-21 | 2010-02-24 | 中山市东溢新材料有限公司 | Modified epoxy resin adhesive and preparation method thereof |
| CN104099051A (en) * | 2014-07-04 | 2014-10-15 | 中国西电电气股份有限公司 | Epoxy resin adhesive |
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| CN108165198A (en) | 2018-06-15 |
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Address after: Room 101, 201, Building 2, No. 178 Dingxing Road, Tangjiawan Town, High tech Zone, Zhuhai City, Guangdong Province, 519085 Patentee after: Dongguan City Heng Erlang Industrial Co.,Ltd. Address before: 523000 No.10, Lane 5, Shangnan Road, nanzha No.5 Industrial Zone, Humen Town, Dongguan City, Guangdong Province Patentee before: DONGGUAN HENGERLANG INDUSTRIAL CO.,LTD. |