CN103450830A - Preparation of high-performance magnetic conductive pressure-sensitive adhesive - Google Patents

Preparation of high-performance magnetic conductive pressure-sensitive adhesive Download PDF

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Publication number
CN103450830A
CN103450830A CN2013103932412A CN201310393241A CN103450830A CN 103450830 A CN103450830 A CN 103450830A CN 2013103932412 A CN2013103932412 A CN 2013103932412A CN 201310393241 A CN201310393241 A CN 201310393241A CN 103450830 A CN103450830 A CN 103450830A
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China
Prior art keywords
magnetic conductive
graphene oxide
sensitive adhesive
preparation
conductive pressure
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CN2013103932412A
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CN103450830B (en
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齐暑华
张帆
史金玲
张翼
马缓
黄英
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention relates to preparation of a high-performance magnetic conductive pressure-sensitive adhesive. In the pressure-sensitive adhesive, solvent type polyacrylate is used as a resin matrix, and modified graphene oxide is used as a magnetic conductive material. The graphene oxide is an insulator but has a large surface area and is stable and dispersed and is not easily agglomerated and also has oil-water amphipathy and excellent mechanical properties and can be used as a good carrier and a modification matrix; the polyacrylate has good affinity and is suitable for splicing many metals and nonmetal materials. By adopting the method, the related preparation process is simplified, and the research range of functional pressure-sensitive adhesive is widened, thus the method has positive significance.

Description

A kind of preparation of high performance magnetic conductive pressure sensitive adhesive
Technical field
The present invention relates to a kind of method of preparation and use of high performance magnetic conductive pressure sensitive adhesive, the invisible coating that can be naval vessels provides material, also can need for large-scale power station facility etc. the occasion of electromagnetic shielding.
Background technology
Along with the development of new and high technology with to the increasing input of leading-edge field, the development of developed countries electromagnetic shielding material is very fast, and particularly the U.S., West Europe, Japan etc. have formed the shielding material industry of the various classifications of production and series specification.And the appearance of the shielding material product of varied excellent performance has greatly promoted the military strength of these countries and regions.
In addition, the electromagnetic interference that hertzian wave causes (EMI) is day by day serious with electromagnetic compatibility (EMC) problem, and after noise pollution, atmospheric pollution, water pollute, Contamination of Electromagnetic Wave becomes the fourth-largest public hazards that threaten human health.Explore efficient electromagnetic shielding material, prevent that electromagenetic wave radiation from polluting with protection of the environment and HUMAN HEALTH, prevent that electromagnetic-wave leakage is to ensure information safety, become current problem in the urgent need to address in the world.
Existing magnetic conductive glue on domestic market, great majority are directly mixed by thermosetting resin and metal-powder (as nickel powder, silver powder etc.).The characteristics of this class tackiness agent are, application surface is narrow, can't repair after solidifying and internal stress great Yi causes fatigue of materials.Part scientific research institution and unit have also prepared thermoplastic magnetic conductive glue, but the magnetic conductive material selection is unreasonable, and technique trouble and cost are too high, can't meet the demand of Defence business and people's daily life.
Summary of the invention
For overcoming the above problems, the present invention aims to provide a kind of preparation method that can meet electromagnetic shielding requirement and the simple magnetic conductive pressure sensitive adhesive of preparation method.
Technical scheme
A kind of preparation method of high performance magnetic conductive pressure sensitive adhesive is characterized in that step is as follows:
Step 1: graphene oxide is mixed with deionized water, under ultrasound condition, graphene oxide is joined in deionized water, ultrasonic time is 12 hours, makes graphene oxide/aqueous suspension after dispersion; Described M graphene oxide: M go ionized water=1: 99;
Step 2: the PdCl that is 0.3% by massfraction 2solution mixes with the hydrochloric acid soln of 1mol/L, is made into activation solution; Described volume ratio is V palladium chloride solution: V hydrochloric acid soln=4: 1;
Step 3: the graphene oxide/aqueous suspension of step 1 is mixed with the activation solution of step 2, add boric acid postactivated, then give its plated surface one deck nickel, washing and drying, make the magnetic conductive material; The blending ratio of described graphene oxide/aqeous suspension and activation solution is V graphene oxide/water: V activation solution=1: 1;
Step 4: the polyacrylic ester by 40% mixes in solvent with 10%~30% magnetic conductive material, 0.6% coupling agent, after stirring, makes each component be uniformly dispersed, and makes the high performance magnetic conductive pressure sensitive adhesive; Described polyacrylic ester is solvent type polyacrylate; Described coupling agent is γ-methacryloxypropyl trimethoxy silane KH570; Described solvent is butanone.
Described nickel plating process is electroless plating.
The washing and drying of described step 3 is: with washed with de-ionized water, after suction filtration, 70 ℃ of dryings are 12 hours.
Beneficial effect
The preparation method of high performance magnetic conductive pressure sensitive adhesive provided by the invention, pressure sensitive adhesive be take solvent type polyacrylate as resin matrix, and modified graphene oxide is the magnetic conductive material.Graphene oxide is originally as isolator, but surface-area is large, and stable dispersion is difficult for reuniting, and has the amphipathic and excellent mechanical property of profit, can be used as good carrier and modified matrix; And polyacrylic ester has good affinity, be applicable to the bonding of a lot of metals and non-metallic material.The magnetic conductive pressure sensitive adhesive that this legal system is standby, simplified relevant preparation technology, widened the research aspect of function pressure sensitive adhesive, thereby had positive meaning.
Embodiment
Embodiment 1~5
A kind of preparation and application of high-performance conductive pressure sensitive adhesive comprises following two steps:
1) magnetic conductive material preparation
After graphene oxide is pulverized, add in deionized water, ultrasonic 12 hours extremely dispersed, obtains graphene oxide/aqueous suspension [M graphene oxide: M deionized water=1: 99].
The PdCl that is 0.3% by massfraction 2the aqueous solution mixes and is made into PdCl with the dilute hydrochloric acid solution of 1mol/L 2/ HCl activation solution [V palladium chloride solution: V hydrochloric acid soln=4: 1].To make graphene oxide/aqueous suspension and PdCl again 2/ HCl activation solution is uniformly mixed [V graphene oxide/water: V activation solution=1: 1], add boric acid to be activated.Mixed solution after activation is washed with a large amount of deionizations.After solid settlement, remove the part supernatant liquor in liquid to be mixed, repeated multiple times washing is until pH approaches 5.
The mixed solution that upwards step obtains adds an excessive hydration sodium hypophosphite solution, reduces processing.After stopping, question response in reduction system, add six hydration nickel sulfate, DL-oxysuccinic acid and ammoniacal liquor to carry out electroless plating again.After reaction finishes, reaction system is filtered, more repeatedly washing leaching cake is to neutral, 70 ℃ of dryings obtain the magnetic conductive filler in 12 hours.
2) preparation of polyacrylic ester magnetic conductive pressure sensitive adhesive
KH570 is dissolved in butanone, then adds polyacrylic ester, be stirred to the solution clarification, then add the magnetic conductive material, mix, each component was uniformly dispersed in ultrasonic 6 hours.The glue composition of 1~3 embodiment is respectively:
A polyacrylic ester 40%
Magnetic conductive material 10%
KH570 0.6%
All the other are solvent;
B polyacrylic ester 40%
Magnetic conductive material 20%
KH570 0.6%
All the other are solvent;
C polyacrylic ester 40%
Magnetic conductive material 30%
KH570 0.6%
All the other are solvent;
D polyacrylic ester 40%
Magnetic conductive material 20%
KH570 0.7%
All the other are solvent;
E polyacrylic ester 40%
Magnetic conductive material 30%
KH570 0.7%
All the other are solvent.

Claims (3)

1. the preparation method of a high performance magnetic conductive pressure sensitive adhesive is characterized in that step is as follows:
Step 1: graphene oxide is mixed with deionized water, under ultrasound condition, graphene oxide is joined in deionized water, ultrasonic time is 12 hours, makes graphene oxide/aqueous suspension after dispersion; Described M graphene oxide: M go from sub-water=1: 99;
Step 2: the PdCl that is 0.3% by massfraction 2solution mixes with the hydrochloric acid soln of 1mol/L, is made into activation solution; Described volume ratio is V palladium chloride solution: V hydrochloric acid soln=4: 1;
Step 3: the graphene oxide/aqueous suspension of step 1 is mixed with the activation solution of step 2, add boric acid postactivated, then give its plated surface one deck nickel, washing and drying, make the magnetic conductive material; The blending ratio of described graphene oxide/aqeous suspension and activation solution is V graphene oxide/water: V activation solution=1: 1;
Step 4: the polyacrylic ester by 40% mixes in solvent with 10%~30% magnetic conductive material, 0.6% coupling agent, after stirring, makes each component be uniformly dispersed, and makes the high performance magnetic conductive pressure sensitive adhesive; Described polyacrylic ester is solvent type polyacrylate; Described coupling agent is γ-methacryloxypropyl trimethoxy silane KH570; Described solvent is butanone.
2. the preparation method of high performance magnetic conductive pressure sensitive adhesive according to claim 1, it is characterized in that: described nickel plating process is electroless plating.
3. the preparation method of high performance magnetic conductive pressure sensitive adhesive according to claim 1, it is characterized in that: the washing and drying of described step 3 is: with washed with de-ionized water, after suction filtration, 70 ℃ of dryings are 12 hours.
CN201310393241.2A 2013-09-02 2013-09-02 Preparation of high-performance magnetic conductive pressure-sensitive adhesive Active CN103450830B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN104087216A (en) * 2014-07-17 2014-10-08 湖南元素密码石墨烯研究院(有限合伙) Method for preparing cooling adhesive agent used between LED (Light-Emitting Diode) aluminum substrate and radiator
CN106366983A (en) * 2016-09-06 2017-02-01 哈尔滨工业大学无锡新材料研究院 Acrylic ester electromagnetic shielding pressure-sensitive adhesive and preparation method thereof
CN107177331A (en) * 2017-06-20 2017-09-19 东莞市联洲知识产权运营管理有限公司 A kind of high-elastic height based on nano material leads polyacrylate pressure-sensitive and preparation method thereof
CN107286876A (en) * 2017-06-20 2017-10-24 东莞市联洲知识产权运营管理有限公司 A kind of conductive pressure sensitive adhesive of charcoal based material of high component and preparation method thereof
CN111040679A (en) * 2019-12-09 2020-04-21 深圳市友事达塑胶制品有限公司 Conductive hot melt adhesive and preparation process thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104087216A (en) * 2014-07-17 2014-10-08 湖南元素密码石墨烯研究院(有限合伙) Method for preparing cooling adhesive agent used between LED (Light-Emitting Diode) aluminum substrate and radiator
CN104087216B (en) * 2014-07-17 2016-04-20 湖南元素密码石墨烯高科技有限公司 For the making method of the tackiness agent that dispels the heat between LED aluminum base plate and scatterer
CN106366983A (en) * 2016-09-06 2017-02-01 哈尔滨工业大学无锡新材料研究院 Acrylic ester electromagnetic shielding pressure-sensitive adhesive and preparation method thereof
CN106366983B (en) * 2016-09-06 2019-02-19 哈尔滨工业大学无锡新材料研究院 Acrylate is electromagnetically shielded pressure sensitive adhesive and preparation method thereof
CN107177331A (en) * 2017-06-20 2017-09-19 东莞市联洲知识产权运营管理有限公司 A kind of high-elastic height based on nano material leads polyacrylate pressure-sensitive and preparation method thereof
CN107286876A (en) * 2017-06-20 2017-10-24 东莞市联洲知识产权运营管理有限公司 A kind of conductive pressure sensitive adhesive of charcoal based material of high component and preparation method thereof
CN111040679A (en) * 2019-12-09 2020-04-21 深圳市友事达塑胶制品有限公司 Conductive hot melt adhesive and preparation process thereof
CN111040679B (en) * 2019-12-09 2021-03-23 深圳市友事达塑胶制品有限公司 Conductive hot melt adhesive and preparation process thereof

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