CN103450830B - 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
CN103450830B
CN103450830B CN201310393241.2A CN201310393241A CN103450830B CN 103450830 B CN103450830 B CN 103450830B CN 201310393241 A CN201310393241 A CN 201310393241A CN 103450830 B CN103450830 B CN 103450830B
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graphene oxide
magnetic conductive
sensitive adhesive
preparation
solution
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CN201310393241.2A
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CN103450830A (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 method 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 may be used for the occasion that large-scale power station facility etc. needs electromagnetic shielding.
Background technology
Along with the development of new and high technology and increasing input to 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 producing various classification and series specification.And the appearance of the shielding material product of varied excellent performance, greatly improve the military strength of these countries and regions.
In addition, the electromagnetic interference (EMI) that hertzian wave causes and electromagnetic compatibility (EMC) problem are day by day serious, and after noise pollution, atmospheric pollution, water pollutions, Contamination of Electromagnetic Wave becomes the fourth-largest public hazards threatening human health.Explore efficient electromagnetic shielding material, prevent electromagenetic wave radiation from polluting with protection of the environment and HUMAN HEALTH, prevent electromagnetic-wave leakage to ensure information safety, become current problem in the urgent need to address in the world.
Magnetic conductive glue existing on domestic market, great majority are directly mixed by thermosetting resin and metal-powder (as nickel powder, silver powder etc.).The feature of this kind of tackiness agent is, application surface is narrow, cannot repair after solidification and internal stress great Yi causes fatigue of materials.Part scientific research institution and unit have also prepared thermoplastic magnetic conductive glue, but magnetic conductive material selection is unreasonable, process cumbersome and cost is too high, cannot 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 and a kind ofly can meet electromagnetic shielding requirements and the preparation method of the simple magnetic conductive pressure sensitive adhesive of preparation method.
Technical scheme
A preparation method for 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, joined by graphene oxide 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: be the PdCl of 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, it is postactivated to add boric acid, then gives its plated surface one deck nickel, and washing and drying, makes magnetic conductive material; Described graphene oxide/aqeous suspension and the blending ratio of activation solution are V graphene oxide/water: V activation solution=1: 1;
Step 4: mixed in solvent with the magnetic conductive material of 10% ~ 30%, the coupling agent of 0.6% by the polyacrylic ester of 40%, makes each component disperses even, makes high performance magnetic conductive pressure sensitive adhesive after stirring; 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, 70 DEG C of dryings 12 hours after suction filtration.
Beneficial effect
The preparation method of high performance magnetic conductive pressure sensitive adhesive provided by the invention, pressure sensitive adhesive take solvent type polyacrylate as resin matrix, and modified graphene oxide is magnetic conductive material.Graphene oxide is originally as isolator, but surface-area is large, and stable dispersion is not easily reunited, 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 metal and non-metallic material.The magnetic conductive pressure sensitive adhesive that this legal system is standby, simplifies relevant preparation technology, has widened the research aspect of function pressure sensitive adhesive, thus have positive meaning.
Embodiment
Embodiment 1 ~ 5
A preparation and application for high-performance conductive pressure sensitive adhesive, comprises following two steps:
1) magnetic conductive material preparation
Will graphene oxide pulverize after add in deionized water, ultrasonic 12 little of dispersed, obtain graphene oxide/aqueous suspension [M graphene oxide: M deionized water=1: 99].
Be the PdCl of 0.3% by massfraction 2the aqueous solution mixes with the dilute hydrochloric acid solution of 1mol/L and is made into PdCl 2/ HCl activation solution [V palladium chloride solution: V hydrochloric acid soln=4: 1].Graphene oxide/aqueous suspension and PdCl will be made again 2/ HCl activation solution is uniformly mixed [V graphene oxide/water: V activation solution=1: 1], add boric acid to activate.Mixed solution after activation is washed with a large amount of deionization.In liquid to be mixed after solid settlement, remove part supernatant liquor, repeated multiple times washing is until pH is close to 5.
Upwards walk the mixed solution obtained and add an excessive hydration sodium hypophosphite solution, carry out reduction treatment.Question response adds six hydration nickel sulfate, DL-oxysuccinic acid and ammoniacal liquor again after stopping and carrying out electroless plating in reduction system.After reaction terminates, reaction system filtered, more repeatedly washing leaching cake is to neutral, 70 DEG C of dryings obtain magnetic conductive filler in 12 hours.
2) preparation of polyacrylic ester magnetic conductive pressure sensitive adhesive
Be dissolved in by KH570 in butanone, then add polyacrylic ester, be stirred to solution clarification, then add magnetic conductive material, mixing, makes each component disperses even 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 (1)

1. a preparation method for 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, joined by graphene oxide 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: be the PdCl of 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, it is postactivated to add boric acid, then gives its plated surface one deck nickel, and washing and drying, makes magnetic conductive material; Described graphene oxide/aqeous suspension and the blending ratio of activation solution are V graphene oxide/water: V activation solution=1: 1;
Step 4: mixed in solvent with the magnetic conductive material of 10% ~ 30%, the coupling agent of 0.6% by the polyacrylic ester of 40%, makes each component disperses even, makes high performance magnetic conductive pressure sensitive adhesive after stirring; 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, 70 DEG C of dryings 12 hours after suction filtration.
CN201310393241.2A 2013-09-02 2013-09-02 Preparation of high-performance magnetic conductive pressure-sensitive adhesive Active CN103450830B (en)

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Families Citing this family (5)

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Publication number Priority date Publication date Assignee Title
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
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
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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CN101740785A (en) * 2009-12-14 2010-06-16 浙江大学 Palladium/graphene nano electro-catalyst and preparation method thereof
CN102583348A (en) * 2012-02-20 2012-07-18 北京航空航天大学 Surface nano-nickel particle modified graphene nano material and preparation method thereof
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