CN107418491A - A kind of conducting resinl and preparation method thereof - Google Patents
A kind of conducting resinl and preparation method thereof Download PDFInfo
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- CN107418491A CN107418491A CN201710857612.6A CN201710857612A CN107418491A CN 107418491 A CN107418491 A CN 107418491A CN 201710857612 A CN201710857612 A CN 201710857612A CN 107418491 A CN107418491 A CN 107418491A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated compounds
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- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
- C08G59/1455—Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
- C08G59/1461—Unsaturated monoacids
- C08G59/1466—Acrylic or methacrylic acids
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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
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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
- C08K2003/0806—Silver
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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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- Conductive Materials (AREA)
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Abstract
The invention discloses a kind of conducting resinl and preparation method thereof, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；Wherein component A includes：Acrylated epoxy, silver powder, titanate coupling agent, glycerine, acetone；B component includes the raw material of following parts by weight：Silver powder, abietyl epoxy hardener, glycerine, acetone, the conducting resinl are simple to manufacture, storage life limit for length, and intensity is high, and long lifespan is safe to use.
Description
Technical field
The present invention relates to conducting resinl technical field, more particularly to a kind of conducting resinl.The present invention also provides a kind of including above-mentioned
The preparation method of conducting resinl.
Background technology
Conducting resinl is a kind of adhesive for solidifying or having certain electric conductivity after drying, and it generally with matrix resin and leads
Electric filler is that conducting particles is main constituents, conducting particles is combined together by the bonding effect of matrix resin, shape
Into conductive path, being conductively connected for glued material is realized.
In the prior art, conducting resinl has that period of storage is short, storage requirement is harsh (needs closed, lucifuge and low temperature ring
Stored under border), because condition is harsh, under normal temperature the storage period of conducting resinl be no more than 3 months, be no more than 6 months under low temperature environment.
Furthermore the situation shunk greatly occurs after use, bonding strength reduces, and contraction seriously causes to cause electric conductivity to decline.Separately
Outside, in the curing process, the volatilization of curing accelerator, diluent etc. is more serious, and has necessarily in the gas to volatilize
Poisonous and harmful substance, operating environment is both influenceed, the health that infringement operating personnel again be present.
Therefore it provides a kind of conducting resinl and preparation method thereof, to be simple to manufacture, storage life limit for length, intensity is high, the life-span
It is long, it is safe to use, just turn into those skilled in the art's urgent problem to be solved.
The content of the invention
It is an object of the invention to provide a kind of conducting resinl and preparation method thereof, to be simple to manufacture, storage life limit for length, intensity
Height, long lifespan are safe to use.
To achieve these goals, the present invention provides a kind of conducting resinl, including component A and B component, the component A and institute
State B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：20~48 parts of acrylated epoxy, silver powder 45~70
Part, 1~5 part of titanate coupling agent, 1~5 part of glycerine, acetone is 5~30 parts；
The B component includes the raw material of following parts by weight：45~75 parts of silver powder, 10~24 parts of abietyl epoxy hardener,
1~5 part of glycerine, 5~20 parts of acetone.
Preferably, fine silver powder is nano powder, and diameter of particle is 50~70nm.
Preferably, 35~40 parts of acrylated epoxy in the component A, 60~65 parts of fine silver powder, titanate esters
3~4 parts of coupling agent, 2~4 parts of glycerine, acetone are 10~20 parts.
Preferably, the B component includes the raw material of following parts by weight：55~60 parts of fine silver powder, abietyl epoxy hardener
15~20 parts, 2~4 parts of glycerine, 10~15 parts of acetone.
The beneficial effects of the invention are as follows：
1) conductive adhesive performance of the invention is stable, is easy to store, and the sealing lucifuge shelf-life can reach more than 1 year.
2) conducting resinl of the invention is cold curing, is easy to construct, while high strength after curing, bonding tensile-sbear strength (steel/
Steel) >=20MPa, pulls apart elongation 13%.
3) conducting resinl ageing resistace of the invention is good, its aging life-span >=15 year.
4) electric conductivity of the present invention is excellent, its specific insulation ＜ 10-3Ω, it can effectively ensure that conductive effect.
5) conducting resinl use range of the invention is extensive, -45 DEG C~-150 DEG C of suitable environment, can be resistant to soda acid salt corrosion.
The present invention also provides a kind of preparation method of conducting resinl, it is characterised in that comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 50~70nm；
S52 is by 40~60 parts of epoxy resin, 30~60 parts of acrylic acid, 1~2 part of catalyst, 0.2 part of MEHQ,
0.1 part of hypophosphorous acid, put into equipped with agitator, thermometer reaction vessel in, stirring be warming up to 95~100 DEG C insulation 1.5~
2.5h, 105~110 DEG C of 1.5~2.5h of insulation are continuously heating to, until AV≤5mgKOH/g, obtains Acrylate Modified Epoxy
Resin；
S53 prepares component A：Take 20~48 parts of the acrylated epoxy of gained in step S52, step S51 silver
45~70 parts of powder, 1~5 part of titanate coupling agent, 1~5 part of glycerine, acetone are 5~30 parts；
S54 prepares B component：45~75 parts of step S51 silver powder, 10~24 parts of abietyl epoxy hardener, glycerine 1~5
Part, 5~20 parts of acetone；
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 10~30 minutes, obtain conducting resinl.
Preferably, catalyst described in step 2) is the mixture of triethylamine and organo-chromium compound.
Preferably, the ratio of the triethylamine and the organo-chromium compound is 60:1.
Preferably, component A described in step 3) carries out the scattered 35min of ultrasonic wave at room temperature, is vacuumized in vacuum tank
25min so that air entrapment is discharged.
Preferably, the step 3) B component carries out the scattered 35min of ultrasonic wave at room temperature, is vacuumized in vacuum tank
25min so that air entrapment is discharged.
The preparation method of the conducting resinl of the present invention has the beneficial effect that：
1) electric silica gel component of the invention is few, and raw material sources are extensive, and manufacturing process is simple and is easily achieved, can be effective
Reduce manufacturing cost.
2) conducting resinl of the invention is conducting particles using nano-silver powder particle, and nano level silver powder can reduce adjacent lead
Contact gap between charged particle, while increase the contact area between adjacent conductive particle, the contact point with matrix is reduced, from
And strengthen resistivity.
3) conducting resinl of the invention, can carry out curing reaction at ambient temperature in preparation process, and it is solid to improve heating
There is the problems such as hotlist heat ageing in conducting element caused by change.
4) conducting resinl of the invention significantly improves conducting resinl using acrylated epoxy as matrix resin
Impact capacity and anti-vibration ability.Even in the winter of cold, acrylated epoxy is not easy in conducting resinl
Crystallization.
Brief description of the drawings
Fig. 1 is conducting resinl preparation flow figure provided by the present invention.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
Fig. 1 is refer to, Fig. 1 is conducting resinl preparation flow figure provided by the present invention.
Embodiment 1：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：35 parts of acrylated epoxy, 60 parts of silver powder, titanate coupling agent 3
Part, 2 parts of glycerine, acetone is 10 parts；The B component includes the raw material of following parts by weight：55 parts of silver powder, abietyl curable epoxide
15 parts of agent, 2 parts of glycerine, 10 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 50nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 50nm；
S52 is by 40 parts of epoxy resin, 30 parts of acrylic acid, 1 part of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 95 insulation 1.5h, is continuously heating to 105 DEG C of insulations
1.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 35 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 60
Part, 3 parts of titanate coupling agent, 2 parts of glycerine, acetone is 10 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：55 parts of step S51 silver powder, 15 parts of abietyl epoxy hardener, 2 parts of glycerine, 10 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 10 minutes, obtain conducting resinl.
Embodiment 2：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：37 parts of acrylated epoxy, 62 parts of silver powder, titanate coupling agent 3
Part, 2 parts of glycerine, acetone is 15 parts；The B component includes the raw material of following parts by weight：55 parts of silver powder, abietyl curable epoxide
18 parts of agent, 3 parts of glycerine, 10 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 60nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 60nm；
S52 is by 45 parts of epoxy resin, 35 parts of acrylic acid, 1 part of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
To put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 95 insulation 2h, is continuously heating to 100 DEG C of insulations 2,
Until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and organo-chromium compound 60：
1 mixture.
S53 prepares component A：Take 37 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 62
Part, 3 parts of titanate coupling agent, 2 parts of glycerine, acetone is 15 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：55 parts of step S51 silver powder, 18 parts of abietyl epoxy hardener, 3 parts of glycerine, 3 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 10 minutes, obtain conducting resinl.
Embodiment 3：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：40 parts of acrylated epoxy, 60 parts of silver powder, titanate coupling agent 4
Part, 3 parts of glycerine, acetone is 15 parts；The B component includes the raw material of following parts by weight：58 parts of silver powder, abietyl curable epoxide
18 parts of agent, 3 parts of glycerine, 15 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 55nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 55nm；
S52 is by 40 parts of epoxy resin, 30 parts of acrylic acid, 1 part of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 95 insulation 1.5h, is continuously heating to 105 DEG C of insulations
1.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 40 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 60
Part, 4 parts of titanate coupling agent, 3 parts of glycerine, acetone is 15 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：58 parts of step S51 silver powder, 18 parts of abietyl epoxy hardener, 3 parts of glycerine, 15 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 15 minutes, obtain conducting resinl.
Embodiment 4：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：40 parts of acrylated epoxy, 65 parts of silver powder, titanate coupling agent 4
Part, 4 parts of glycerine, acetone is 20 parts；The B component includes the raw material of following parts by weight：60 parts of silver powder, abietyl curable epoxide
20 parts of agent, 4 parts of glycerine, 15 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 55nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 60nm；
S52 is by 50 parts of epoxy resin, 40 parts of acrylic acid, 2 parts of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 100 insulation 2h, is continuously heating to 110 DEG C of insulations
2.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 40 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 65
Part, 4 parts of titanate coupling agent, 4 parts of glycerine, acetone is 20 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：60 parts of step S51 silver powder, 20 parts of abietyl epoxy hardener, 4 parts of glycerine, 15 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 20 minutes, obtain conducting resinl.
Embodiment 5：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：40 parts of acrylated epoxy, 65 parts of silver powder, titanate coupling agent 4
Part, 4 parts of glycerine, acetone is 20 parts；The B component includes the raw material of following parts by weight：60 parts of silver powder, abietyl curable epoxide
20 parts of agent, 4 parts of glycerine, 15 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 60nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 60nm；
S52 is by 50 parts of epoxy resin, 40 parts of acrylic acid, 2 parts of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 100 insulation 2h, is continuously heating to 110 DEG C of insulations
2.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 40 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 65
Part, 4 parts of titanate coupling agent, 4 parts of glycerine, acetone is 20 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：60 parts of step S51 silver powder, 20 parts of abietyl epoxy hardener, 4 parts of glycerine, 15 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 25 minutes, obtain conducting resinl.
Comparative examples 1：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：40 parts of acrylated epoxy, 65 parts of silver powder, titanate coupling agent 4
Part, acetone is 20 parts；The B component includes the raw material of following parts by weight：60 parts of silver powder, 20 parts of abietyl epoxy hardener, third
15 parts of ketone, wherein, fine silver powder is nano powder, diameter of particle 60nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 60nm；
S52 is by 50 parts of epoxy resin, 40 parts of acrylic acid, 2 parts of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 100 insulation 2h, is continuously heating to 110 DEG C of insulations
2.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 40 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 65
Part, 4 parts of titanate coupling agent, acetone is 20 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min, is taken out in vacuum tank
Vacuum 25min so that air entrapment is discharged.
S54 prepares B component：60 parts of step S51 silver powder, 20 parts of abietyl epoxy hardener, 15 parts of acetone；B component is existed
Ultrasonic wave is carried out at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 25 minutes, obtain conducting resinl.
Comparative examples 2：
A kind of conducting resinl, including component A and B component, the component A and the B component in mass ratio 1：1 mixes；
The component A includes the raw material of following parts by weight：40 parts of acrylated epoxy, 65 parts of silver powder, titanate coupling agent 4
Part, 4 parts of glycerine, acetone is 20 parts；The B component includes the raw material of following parts by weight：60 parts of silver powder, abietyl curable epoxide
20 parts of agent, 4 parts of glycerine, 15 parts of acetone, wherein, fine silver powder is nano powder, diameter of particle 50nm.
The preparation method of above-mentioned conducting resinl, comprises the following steps：
S51 takes 0.18mol/L silver nitrate solution, and polyoxamide is slowly dropped in the solution of silver nitrate, 55
Reacted under DEG C water bath condition, stirring during the course of the reaction make it that reaction is abundant, product is centrifuged, using ethanol to product
Washed repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 50nm；
S52 is by 50 parts of epoxy resin, 40 parts of acrylic acid, 2 parts of catalyst, 0.2 part of MEHQ, 0.1 part of hypophosphorous acid,
Put into and be equipped with the reaction vessel of agitator, thermometer, stirring is warming up to 100 insulation 2h, is continuously heating to 110 DEG C of insulations
2.5, until AV≤5mgKOH/g, obtains acrylated epoxy；The catalyst is triethylamine and Organic Chromium chemical combination
Thing 60：1 mixture.
S53 prepares component A：Take 40 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 65
Part, 4 parts of titanate coupling agent, 4 parts of glycerine, acetone is 20 parts；Component A is carried out to ultrasonic wave at room temperature and disperses 35min,
25min is vacuumized in vacuum tank so that air entrapment is discharged.
S54 prepares B component：60 parts of step S51 silver powder, 20 parts of abietyl epoxy hardener, 4 parts of glycerine, 15 parts of acetone；
B component is carried out to ultrasonic wave at room temperature and disperses 35min, 25min is vacuumized in vacuum tank so that air entrapment is discharged.
S55 is mixed：By component A and B component in mass ratio 1：After 1 is well mixed, it is placed under conditions of pressure ﹤ 0.02Mpa
Deaeration 25 minutes, obtain conducting resinl.
To verify the performance of product of the present invention, We conducted following test：
(1) specific insulation is tested
It is 5mm that the electrode of two of resistance instrument is pressed onto into thickness, and long and width is on 30mm molded tablet, and test obtains electricity
Resistance, Gu specific insulation is the resistance value that test obtains and the product of thickness, unit is Ω cm.It the results are shown in Table shown in 1, it is obtained
Conductive glue has good electric conductivity.
(2) adhesion strength is tested
Embodiment 1~5 and obtained product adhesive dispensing device will be prepared, the glue of 30mm length high into 1.5mm is put on aluminium base
Bar, after 160 DEG C, 1h solidifications, its adhesive force is surveyed using standard test weight and tool, and calculates its adhesion strength with aluminium base,
1 is the results are shown in Table, the conducting resinl and aluminium sheet for showing the present invention have good caking property.
(3) tear strength properties are tested
It is 3mm prints that thickness, which is made, in product made from embodiment 1~5 being prepared, after baking 1h at a temperature of 160 DEG C,
Be punched into crescent print, then on stretching-machine test sample tearing strength.1 is the results are shown in Table, shows the solidification of the present invention
Conductive glue afterwards has good tearing strength.
(4) elongation at break
It is 3mm prints that product made from implementing 1~5 will be prepared thickness is made, after baking 1h at a temperature of 160 DEG C, punching
Be cut into the print of dumbbell shape, then on stretching-machine test sample elongation at break.Fracture elongation is at breakaway poing
The percentage of print elongation.
It can be seen from the data result of table 1, electric silica gel prepared by the present invention has good electric conductivity, caking property, tear
Intensity and elongation at break, wherein comparative example 1 and 2 are contrasted with embodiment 5.
The beneficial effects of the invention are as follows：
1) conductive adhesive performance of the invention is stable, is easy to store, and the sealing lucifuge shelf-life can reach more than 1 year.
2) conducting resinl of the invention is cold curing, is easy to construct, while high strength after curing, bonding tensile-sbear strength (steel/
Steel) >=20MPa, pulls apart elongation 13%.
3) conducting resinl ageing resistace of the invention is good, its aging life-span >=15 year.
4) electric conductivity of the present invention is excellent, its specific insulation ＜ 10-3Ω, it can effectively ensure that conductive effect.
5) conducting resinl use range of the invention is extensive, -45 DEG C~-150 DEG C of suitable environment, can be resistant to soda acid salt corrosion.
The preparation method of the conducting resinl of the present invention has the beneficial effect that：
1) electric silica gel component of the invention is few, and raw material sources are extensive, and manufacturing process is simple and is easily achieved, can be effective
Reduce manufacturing cost.
2) conducting resinl of the invention is conducting particles using nano-silver powder particle, and nano level silver powder can reduce adjacent lead
Contact gap between charged particle, while increase the contact area between adjacent conductive particle, the contact point with matrix is reduced, from
And strengthen resistivity.
3) conducting resinl of the invention, can carry out curing reaction at ambient temperature in preparation process, and it is solid to improve heating
There is the problems such as hotlist heat ageing in conducting element caused by change.
4) conducting resinl of the invention significantly improves conducting resinl using acrylated epoxy as matrix resin
Impact capacity and anti-vibration ability.Even in the winter of cold, acrylated epoxy is not easy in conducting resinl
Crystallization.
The various embodiments described above are only the preferred embodiment of the present invention, in the art, every to be based on skill of the present invention
Changes and improvements in art scheme, it should not exclude outside protection scope of the present invention.
Claims (9)
- A kind of 1. conducting resinl, it is characterised in that including component A and B component, the component A and the B component in mass ratio 1：1 Mix；The component A includes the raw material of following parts by weight：20~48 parts of acrylated epoxy, 45~70 parts of silver powder, 1~5 part of titanate coupling agent, 1~5 part of glycerine, acetone are 5~30 parts；The B component includes the raw material of following parts by weight：45~75 parts of silver powder, 10~24 parts of abietyl epoxy hardener, the third three 1~5 part of alcohol, 5~20 parts of acetone.
- 2. conducting resinl according to claim 1, it is characterised in that fine silver powder is nano powder, and diameter of particle is 50~70nm.
- 3. conducting resinl according to claim 1, it is characterised in that acrylated epoxy 35 in the component A ~40 parts, 60~65 parts of fine silver powder, 3~4 parts of titanate coupling agent, 2~4 parts of glycerine, acetone is 10~20 parts.
- 4. conducting resinl according to claim 1, it is characterised in that the B component includes the raw material of following parts by weight：Fine silver 55~60 parts of powder, 15~20 parts of abietyl epoxy hardener, 2~4 parts of glycerine, 10~15 parts of acetone.
- 5. a kind of preparation method of conducting resinl, it is characterised in that comprise the following steps：S51:0.18mol/L silver nitrate solution is taken, polyoxamide is slowly dropped in the solution of silver nitrate, in 55 DEG C of water Reacted under the conditions of bath, stirring during the course of the reaction make it that reaction is abundant, centrifuges product, and product is carried out using ethanol Wash repeatedly, the product after washing is dried to obtain the silver powder that pure Size Distribution is 50~70nm；S52:By 40~60 parts of epoxy resin, 30~60 parts of acrylic acid, 1~2 part of catalyst, 0.2 part of MEHQ, secondary phosphorus Acid 0.1 part, put into equipped with agitator, thermometer reaction vessel in, stirring be warming up to 95~100 DEG C insulation 1.5~2.5h, 105~110 DEG C of 1.5~2.5h of insulation are continuously heating to, until AV≤5mgKOH/g, obtains acrylated epoxy；S53:Prepare component A：Take 20~48 parts of the acrylated epoxy of gained in step S52, step S51 silver powder 45 ~70 parts, 1~5 part of titanate coupling agent, 1~5 part of glycerine, acetone is 5~30 parts；S54：Prepare B component：45~75 parts of step S51 silver powder, 10~24 parts of abietyl epoxy hardener, 1~5 part of glycerine, 5~20 parts of acetone；S55：Mixing：By component A and B component in mass ratio 1：After 1 is well mixed, deaeration under conditions of pressure ﹤ 0.02Mpa is placed in 10~30 minutes, obtain conducting resinl.
- 6. preparation method according to claim 5, it is characterised in that catalyst described in step 2) is triethylamine and organic The mixture of chromium compound.
- 7. preparation method according to claim 6, it is characterised in that the ratio of the triethylamine and the organo-chromium compound Example is 60:1.
- 8. preparation method according to claim 5, it is characterised in that component A is surpassed at room temperature described in step 3) Sound wave disperses 35min, and 25min is vacuumized in vacuum tank so that air entrapment is discharged.
- 9. preparation method according to claim 5, it is characterised in that the step 3) B component carries out ultrasound at room temperature Wavelength-division dissipates 35min, and 25min is vacuumized in vacuum tank so that air entrapment is discharged.
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