WO2019095397A1 - Highly thermally and electrically conductive environmentally-friendly adhesive and preparation method therefor - Google Patents

Highly thermally and electrically conductive environmentally-friendly adhesive and preparation method therefor Download PDF

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Publication number
WO2019095397A1
WO2019095397A1 PCT/CN2017/112000 CN2017112000W WO2019095397A1 WO 2019095397 A1 WO2019095397 A1 WO 2019095397A1 CN 2017112000 W CN2017112000 W CN 2017112000W WO 2019095397 A1 WO2019095397 A1 WO 2019095397A1
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conductive
vacuum
thermal conductivity
parts
friendly adhesive
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PCT/CN2017/112000
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French (fr)
Chinese (zh)
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杨定宽
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苏州锐特捷化工制品有限公司
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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
    • 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
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • 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
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • 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
    • 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

Definitions

  • the invention relates to the field of chemical products, in particular to a high thermal conductivity conductive environmentally friendly adhesive.
  • Conductive and thermal conductive adhesive is a special conductive polymer composite material which can effectively bond various materials and has electrical and thermal conductivity.
  • the conductive and thermal conductive adhesives on the market are usually composed of conductive and thermally conductive filler materials and polymer resins. .
  • the existing conductive and thermal conductive adhesives have poor filling and dispersing properties due to the aggregation of the conductive and thermally conductive fillers, which limits the electrical and thermal conductivity, especially the thermal conductivity, and the thermal conductivity is usually lower than 2w/(m ⁇ K). Above and below 0.2w/(m ⁇ K), the thermal conductivity is low and cannot meet the needs of use.
  • the polymer resin has disadvantages such as poor toughness and environmental protection.
  • the technical problem mainly solved by the invention is to provide a high thermal conductivity conductive environment-friendly adhesive and a preparation method thereof, which can solve the above problems of the existing heat conductive conductive adhesive.
  • a technical solution adopted by the present invention is to provide a high thermal conductivity conductive environmentally friendly adhesive, comprising the following components by weight: 40-50 parts of modified epoxy resin, konjac glucomannan 20 ⁇ 30 parts, 15-20 parts of chitosan, 15-25 parts of heat conductive filler, 10-15 parts of conductive filler, 5-8 parts of diluent, 5-8 parts of curing agent, 1-3 parts of curing accelerator, rheology control 3 to 5 parts of the agent.
  • the modified epoxy resin is a nitrile rubber toughened modified epoxy Resin.
  • the thermally conductive filler comprises Ag-AIN particles, aluminum nitride and aluminum oxide in a mass ratio of 5 to 7:3 to 5:1 to 3.
  • the conductive filler comprises silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 2 to 3:2 to 4.
  • another technical solution adopted by the present invention is to provide a method for preparing a high thermal conductivity conductive environmentally friendly adhesive, comprising the following steps:
  • thermally conductive mixed components weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, Ag-AIN particles prepared in step (1) and other thermally conductive fillers of formula amount and 1/4 ⁇ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, and stirred and mixed under a certain degree of vacuum to obtain a thermally conductive mixed component;
  • conductive mixed components weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ⁇ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, stirred and mixed under a certain degree of vacuum to obtain a conductive mixed component;
  • the high temperature treatment conditions are: temperature 600 to 800 ° C, time 3 to 5 h; the acidic cleaning liquid is potassium perchromate and high manganese A mixture of potassium acid in a molar volume of 1:0.5.
  • the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 300 to 400 r/min, and a stirring time of 35 to ⁇ at room temperature. 45min.
  • the acidifying solution is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 55-65%;
  • the ultrasonic treatment method is: 70 ⁇ Ultrasonic treatment at 80 ° C for 1.5 ⁇ 2h.
  • the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 300 to 400 r/min, and a stirring time of 35 to ⁇ at room temperature. 45min.
  • the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 600 to 1000 r/min, and a stirring time of 20 at room temperature. ⁇ 40min.
  • the invention has the beneficial effects that the invention selects the heat conductive filler and the conductive multi-wall carbon nanotube by electroless silver plating through reasonable raw material selection and formulation design, especially the selection of the heat conductive filler and the conductive filler, and then electrically conductive filler and conductive
  • the filler is distributed in a part of the matrix resin and mixed into a mixed component, and the other matrix components are mixed, thereby effectively improving the compatibility between the nano-scale thermal conductive filler and the conductive filler and the matrix resin, thereby improving the dispersion effect, thereby maximizing the functionality thereof.
  • through epoxy resin and konjac glucomannan The combination with chitosan broadens the performance of the substrate while improving environmental friendliness.
  • a high thermal conductivity conductive environmentally friendly adhesive comprising the following components by weight: 40 parts of modified epoxy resin, 20 parts of konjac glucomannan, 15 parts of chitosan, 15 parts of thermally conductive filler, 10 parts of conductive filler, diluted 5 parts of the agent, 5 parts of the curing agent, 1 part of the curing accelerator, and 3 parts of the rheology control agent.
  • the modified epoxy resin is a nitrile rubber toughened modified epoxy resin.
  • the thermally conductive filler includes Ag-AIN particles, aluminum nitride, and aluminum oxide in a mass ratio of 5:3:1.
  • the conductive filler includes silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 2:2.
  • the preparation method of the above high thermal conductivity conductive environment-friendly adhesive comprises the following steps:
  • the acidic cleaning solution is a mixture of potassium perchromate and potassium permanganate in a molar volume of 1:0.5;
  • thermally conductive mixed components weigh 1/4 to 1/3 of the amount of modified epoxy resin, step (1)
  • the Ag-AIN particles prepared in the formula and other thermally conductive fillers of the formula amount and the diluent of 1/4 to 1/3 of the formula amount are added to the vacuum mixing stirrer at room temperature at a vacuum of 0.1 to 0.3 MPa at 300 r/min. Stirring and mixing for 45 min at a rate to obtain a thermally conductive mixed component;
  • the acidification liquid is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 55%;
  • the ultrasonic treatment method is: ultrasonic treatment at 70 ° C for 2 h;
  • conductive mixed components weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ⁇ 3% of the formula amount of diluent is added to a vacuum mixer, and the mixture is stirred and mixed at a rate of 300 r/min for 45 min at room temperature under a vacuum of 0.1 to 0.3 MPa to obtain a conductive mixed component;
  • Preparation of adhesive weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan
  • the polysaccharide, the formula amount of chitosan, the formula amount of the rheology control agent and the remaining formula amount of the diluent are stirred and mixed at a rate of 600 r/min for 40 min at room temperature under a vacuum of 0.1 to 0.3 MPa until homogeneous, and then added.
  • a formulation amount of a curing agent and a curing accelerator are stirred and mixed under the same vacuum conditions to obtain the adhesive.
  • a high thermal conductivity conductive environmentally friendly adhesive comprising the following components by weight: 50 parts of modified epoxy resin, 30 parts of konjac glucomannan, 20 parts of chitosan, 25 parts of thermally conductive filler, 15 parts of conductive filler, diluted 8 parts of the agent, 8 parts of the curing agent, 3 parts of the curing accelerator, and 5 parts of the rheology control agent.
  • the modified epoxy resin is a nitrile rubber toughened modified epoxy resin.
  • the thermally conductive filler includes Ag-AIN particles, aluminum nitride, and aluminum oxide in a mass ratio of 7:5:3.
  • the conductive filler includes silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 3:4.
  • the preparation method of the above high thermal conductivity conductive environment-friendly adhesive comprises the following steps:
  • the acidic cleaning solution is a mixture of potassium perchromate and potassium permanganate in a molar volume of 1:0.5;
  • thermally conductive mixed components weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, Ag-AIN particles prepared in step (1) and other thermally conductive fillers of formula amount and 1/4 ⁇ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, and stirred at a rate of 400 r/min under a vacuum of 0.1 to 0.3 MPa for 35 minutes at room temperature to obtain a thermally conductive mixed component;
  • the acidification liquid is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 65%;
  • the ultrasonic treatment method is: ultrasonic treatment at 80 ° C for 1.5 h;
  • conductive mixed components weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ⁇ 3% of the formula amount of diluent is added to a vacuum mixer, and the mixture is stirred and mixed at a rate of 400 r/min for 35 min at room temperature under a vacuum of 0.1 to 0.3 MPa to obtain a conductive mixed component;
  • Preparation of adhesive weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan
  • the polysaccharide, the formula amount of chitosan, the formula amount of the rheology control agent and the remaining formula amount of the diluent are stirred and mixed at a rate of 1000 r/min for 20 min at room temperature under a vacuum of 0.1 to 0.3 MPa until homogeneous, and then added.
  • a formulation amount of a curing agent and a curing accelerator are stirred and mixed under the same vacuum conditions to obtain the adhesive.
  • the high thermal conductivity conductive environmentally friendly adhesive obtained by the above method has been tested to have a conductivity higher than 8.9 S/cm, a thermal conductivity higher than 3.8 W/(m ⁇ K), high bonding strength, and excellent overall performance. .
  • the invention combines the heat conductive filler and the conductive multi-wall carbon nanotube by electroless silver plating through reasonable raw material selection and formula design, especially the selection of the heat conductive filler and the conductive filler, and then distributes the heat conductive filler and the conductive filler to the partial matrix resin.
  • the mixed component is mixed with other matrix components, which effectively improves the compatibility between the nano-scale thermal conductive filler and the conductive filler and the matrix resin, and improves the dispersion effect, thereby maximizing its functionality; through epoxy resin and konjac
  • the combination of glucomannan and chitosan broadens the performance of the matrix while improving environmental friendliness.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Chemically Coating (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Disclosed is a highly thermally and electrically conductive environmentally-friendly adhesive comprising the following components: a modified epoxy resin, konjak glucomannan, chitosan, a thermally conductive filler, an electrically conductive filler, a diluent, a curing agent, a curing accelerator, and a rheology controller. The adhesive effectively improves the compatibility between the fillers and the resin as a matrix, and improves the dispersion effect and the environmental protection properties.

Description

一种高导热导电环保胶黏剂及其制备方法High thermal conductivity conductive environment-friendly adhesive and preparation method thereof 技术领域Technical field
本发明涉及化工产品领域，特别是涉及一种高导热导电环保胶黏剂。The invention relates to the field of chemical products, in particular to a high thermal conductivity conductive environmentally friendly adhesive.
背景技术Background technique
导电导热胶黏剂是一种既能有效黏接各种材料，又具有导电和导热性能的特殊导电高分子复合材料，市面上的导电导热胶黏剂通常由导电导热填充材料和高分子树脂组成。但现有的导电导热胶黏剂由于导电导热填料的聚集，填充分散性能不好，使得导电导热性能受限，尤其是导热性能，其热导率通常低于于2w/(m·K)，在0.2w/(m·K)上下，导热性能低，不能满足使用需求。另外，高分子树脂存在韧性差、不环保等缺点。Conductive and thermal conductive adhesive is a special conductive polymer composite material which can effectively bond various materials and has electrical and thermal conductivity. The conductive and thermal conductive adhesives on the market are usually composed of conductive and thermally conductive filler materials and polymer resins. . However, the existing conductive and thermal conductive adhesives have poor filling and dispersing properties due to the aggregation of the conductive and thermally conductive fillers, which limits the electrical and thermal conductivity, especially the thermal conductivity, and the thermal conductivity is usually lower than 2w/(m·K). Above and below 0.2w/(m·K), the thermal conductivity is low and cannot meet the needs of use. Further, the polymer resin has disadvantages such as poor toughness and environmental protection.
发明内容Summary of the invention
本发明主要解决的技术问题是提供一种高导热导电环保胶黏剂及其制备方法，能够解决现有导热导电胶黏剂存在的上述问题The technical problem mainly solved by the invention is to provide a high thermal conductivity conductive environment-friendly adhesive and a preparation method thereof, which can solve the above problems of the existing heat conductive conductive adhesive.
为解决上述技术问题，本发明采用的一个技术方案是：提供一种高导热导电环保胶黏剂，包括如下重量份组分：改性环氧树脂40～50份、魔芋葡甘聚糖20～30份、壳聚糖15～20份、导热填料15～25份、导电填料10～15份、稀释剂5～8份、固化剂5～8份、固化促进剂1～3份、流变控制剂3～5份。In order to solve the above technical problem, a technical solution adopted by the present invention is to provide a high thermal conductivity conductive environmentally friendly adhesive, comprising the following components by weight: 40-50 parts of modified epoxy resin, konjac glucomannan 20~ 30 parts, 15-20 parts of chitosan, 15-25 parts of heat conductive filler, 10-15 parts of conductive filler, 5-8 parts of diluent, 5-8 parts of curing agent, 1-3 parts of curing accelerator, rheology control 3 to 5 parts of the agent.
在本发明一个较佳实施例中，所述改性环氧树脂为丁腈橡胶增韧改性环氧 树脂。In a preferred embodiment of the present invention, the modified epoxy resin is a nitrile rubber toughened modified epoxy Resin.
在本发明一个较佳实施例中，所述导热填料包括质量比为5～7：3～5:1～3的Ag-AIN颗粒、氮化铝和氧化铝。In a preferred embodiment of the invention, the thermally conductive filler comprises Ag-AIN particles, aluminum nitride and aluminum oxide in a mass ratio of 5 to 7:3 to 5:1 to 3.
在本发明一个较佳实施例中，所述导电填料包括质量比为2～3:2～4的镀银多壁碳纳米管和微米银粉。In a preferred embodiment of the present invention, the conductive filler comprises silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 2 to 3:2 to 4.
为解决上述技术问题，本发明采用的另一个技术方案是：提供一种高导热导电环保胶黏剂的制备方法，包括如下步骤：In order to solve the above technical problem, another technical solution adopted by the present invention is to provide a method for preparing a high thermal conductivity conductive environmentally friendly adhesive, comprising the following steps:
(1)制备Ag-AIN颗粒：首先将A1N颗粒放在马弗炉中高温处理，之后采用酸性清洗液清洗并用冷却的去离子水冲洗、干燥，最后采用无钯化学镀法在其表面沉积上一层致密的金属Ag镀层，得到所述Ag-AIN颗粒；(1) Preparation of Ag-AIN particles: The A1N particles are first placed in a muffle furnace for high temperature treatment, then washed with an acidic cleaning solution, rinsed with cooled deionized water, dried, and finally deposited on the surface by palladium-free electroless plating. a layer of dense metal Ag plating to obtain the Ag-AIN particles;
(2)制备导热混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(1)中制备的Ag-AIN颗粒和配方量的其他导热填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在一定真空度下搅拌混合得到导热混合组分；(2) Preparation of thermally conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, Ag-AIN particles prepared in step (1) and other thermally conductive fillers of formula amount and 1/4~ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, and stirred and mixed under a certain degree of vacuum to obtain a thermally conductive mixed component;
(3)制备镀银碳纳米管：称取配方量的多壁碳纳米管放入盛有酸化液的烧瓶中，超声处理，洗涤至中性并干燥，最后采用无钯化学镀法在其表面及管内沉积上一层致密的金属Ag镀层，得到所述镀银碳纳米管；(3) Preparation of silver-plated carbon nanotubes: Weigh a formula of multi-walled carbon nanotubes into a flask containing an acidified solution, sonicate, wash to neutrality and dry, and finally use palladium-free electroless plating on the surface. And depositing a dense metal Ag plating layer in the tube to obtain the silver-plated carbon nanotube;
(4)制备导电混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(3)中制备的镀银碳纳米管和配方量的其他导电填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在一定真空度下搅拌混合得到导电混合组分；(4) Preparation of conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ~ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, stirred and mixed under a certain degree of vacuum to obtain a conductive mixed component;
(5)制备胶黏剂：称取剩余配方量的改性环氧树脂、步骤(2)中制备的导热混合组分、步骤(3)中制备的导电混合组分、配方量的魔芋葡甘聚糖、配方量的壳聚糖、配方量的流变控制剂以及剩余配方量的稀释剂，在真空下搅拌 混合均匀，然后加入配方量的固化剂和固化促进剂，真空搅拌混合，得到所述胶黏剂。(5) Preparation of adhesive: weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan Glycan, formula amount of chitosan, formula amount of rheology control agent and remaining formula amount of diluent, stirring under vacuum The mixture is uniformly mixed, and then a formula amount of a curing agent and a curing accelerator are added, and the mixture is stirred under vacuum to obtain the adhesive.
在本发明一个较佳实施例中，所述步骤(1)中，所述高温处理的条件为：温度600～800℃，时间3～5h；所述酸性清洗液为高铬酸钾和高锰酸钾以1:0.5的摩尔体积混合的混合液。In a preferred embodiment of the present invention, in the step (1), the high temperature treatment conditions are: temperature 600 to 800 ° C, time 3 to 5 h; the acidic cleaning liquid is potassium perchromate and high manganese A mixture of potassium acid in a molar volume of 1:0.5.
在本发明一个较佳实施例中，所述步骤(2)中，所述真空搅拌混合的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率300～400r/min，搅拌时间35～45min。In a preferred embodiment of the present invention, in the step (2), the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 300 to 400 r/min, and a stirring time of 35 to ～ at room temperature. 45min.
在本发明一个较佳实施例中，所述步骤(3)中，所述酸化液为质量浓度为55～65％的浓硫酸和浓盐酸的混合酸；所述超声处理的方法为：70～80℃超声处理1.5～2h。In a preferred embodiment of the present invention, in the step (3), the acidifying solution is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 55-65%; the ultrasonic treatment method is: 70~ Ultrasonic treatment at 80 ° C for 1.5 ~ 2h.
在本发明一个较佳实施例中，所述步骤(4)中，所述真空搅拌混合的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率300～400r/min，搅拌时间35～45min。In a preferred embodiment of the present invention, in the step (4), the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 300 to 400 r/min, and a stirring time of 35 to ～ at room temperature. 45min.
在本发明一个较佳实施例中，所述步骤(5)中，所述真空搅拌混合的的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率600～1000r/min，搅拌时间20～40min。In a preferred embodiment of the present invention, in the step (5), the conditions of the vacuum stirring and mixing are: a vacuum degree of 0.1 to 0.3 MPa, a stirring rate of 600 to 1000 r/min, and a stirring time of 20 at room temperature. ~40min.
本发明的有益效果是：本发明通过合理的原料选择及配方设计，尤其是导热填料和导电填料的选择，通过化学镀银处理导热填料和导电的多壁碳纳米管，然后将导热填料与导电填料分布于部分基体树脂混合成混合组分，在于其他基体成分混合，有效提高了纳米级导热填料和导电填料与基体树脂之间的相容性，提高分散效果，从而最大程度地发挥其功能性；通过环氧树脂与魔芋葡甘聚糖 和壳聚糖的混合使用，拓宽了基体的性能，同时提高了环保性。The invention has the beneficial effects that the invention selects the heat conductive filler and the conductive multi-wall carbon nanotube by electroless silver plating through reasonable raw material selection and formulation design, especially the selection of the heat conductive filler and the conductive filler, and then electrically conductive filler and conductive The filler is distributed in a part of the matrix resin and mixed into a mixed component, and the other matrix components are mixed, thereby effectively improving the compatibility between the nano-scale thermal conductive filler and the conductive filler and the matrix resin, thereby improving the dispersion effect, thereby maximizing the functionality thereof. ; through epoxy resin and konjac glucomannan The combination with chitosan broadens the performance of the substrate while improving environmental friendliness.
具体实施方式Detailed ways
下面对本发明的较佳实施例进行详细阐述，以使本发明的优点和特征能更易于被本领域技术人员理解，从而对本发明的保护范围做出更为清楚明确的界定。The preferred embodiments of the present invention are described in detail below, so that the advantages and features of the present invention can be more readily understood by those skilled in the art.
本发明实施例包括：Embodiments of the invention include:
实施例1Example 1
一种高导热导电环保胶黏剂，包括如下重量份组分：改性环氧树脂40份、魔芋葡甘聚糖20份、壳聚糖15份、导热填料15份、导电填料10份、稀释剂5份、固化剂5份、固化促进剂1份、流变控制剂3份。A high thermal conductivity conductive environmentally friendly adhesive comprising the following components by weight: 40 parts of modified epoxy resin, 20 parts of konjac glucomannan, 15 parts of chitosan, 15 parts of thermally conductive filler, 10 parts of conductive filler, diluted 5 parts of the agent, 5 parts of the curing agent, 1 part of the curing accelerator, and 3 parts of the rheology control agent.
其中，所述改性环氧树脂为丁腈橡胶增韧改性环氧树脂。Wherein, the modified epoxy resin is a nitrile rubber toughened modified epoxy resin.
所述导热填料包括质量比为5：3:1的Ag-AIN颗粒、氮化铝和氧化铝。The thermally conductive filler includes Ag-AIN particles, aluminum nitride, and aluminum oxide in a mass ratio of 5:3:1.
所述导电填料包括质量比为2:2的镀银多壁碳纳米管和微米银粉。The conductive filler includes silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 2:2.
上述高导热导电环保胶黏剂的制备方法，包括如下步骤：The preparation method of the above high thermal conductivity conductive environment-friendly adhesive comprises the following steps:
(1)制备Ag-AIN颗粒：首先将A1N颗粒放在马弗炉中于600℃下高温处理5h，之后采用酸性清洗液清洗并用冷却的去离子水冲洗、真空干燥，最后采用无钯化学镀法在其表面沉积上一层致密的金属Ag镀层，得到所述Ag-AIN颗粒；(1) Preparation of Ag-AIN particles: First, the A1N particles were placed in a muffle furnace at 600 ° C for 5 h, then washed with an acidic cleaning solution and rinsed with cooled deionized water, vacuum dried, and finally palladium-free electroless plating. The method deposits a dense metal Ag plating on the surface thereof to obtain the Ag-AIN particles;
所述酸性清洗液为高铬酸钾和高锰酸钾以1:0.5的摩尔体积混合的混合液；The acidic cleaning solution is a mixture of potassium perchromate and potassium permanganate in a molar volume of 1:0.5;
(2)制备导热混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(1) 中制备的Ag-AIN颗粒和配方量的其他导热填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在室温下，于0.1～0.3MPa的真空度下300r/min的速率搅拌混合45min，得到导热混合组分；(2) Preparation of thermally conductive mixed components: weigh 1/4 to 1/3 of the amount of modified epoxy resin, step (1) The Ag-AIN particles prepared in the formula and other thermally conductive fillers of the formula amount and the diluent of 1/4 to 1/3 of the formula amount are added to the vacuum mixing stirrer at room temperature at a vacuum of 0.1 to 0.3 MPa at 300 r/min. Stirring and mixing for 45 min at a rate to obtain a thermally conductive mixed component;
(3)制备镀银碳纳米管：称取配方量的多壁碳纳米管放入盛有酸化液的烧瓶中，超声处理，洗涤至中性并干燥，最后采用无钯化学镀法在其表面及管内沉积上一层致密的金属Ag镀层，得到所述镀银碳纳米管；(3) Preparation of silver-plated carbon nanotubes: Weigh a formula of multi-walled carbon nanotubes into a flask containing an acidified solution, sonicate, wash to neutrality and dry, and finally use palladium-free electroless plating on the surface. And depositing a dense metal Ag plating layer in the tube to obtain the silver-plated carbon nanotube;
其中，所述酸化液为质量浓度为55％的浓硫酸和浓盐酸的混合酸；所述超声处理的方法为：70℃超声处理2h；Wherein, the acidification liquid is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 55%; the ultrasonic treatment method is: ultrasonic treatment at 70 ° C for 2 h;
(4)制备导电混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(3)中制备的镀银碳纳米管和配方量的其他导电填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在室温下，真空度为0.1～0.3MPa下以300r/min的速率搅拌混合45min，得到导电混合组分；(4) Preparation of conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ～ 3% of the formula amount of diluent is added to a vacuum mixer, and the mixture is stirred and mixed at a rate of 300 r/min for 45 min at room temperature under a vacuum of 0.1 to 0.3 MPa to obtain a conductive mixed component;
(5)制备胶黏剂：称取剩余配方量的改性环氧树脂、步骤(2)中制备的导热混合组分、步骤(3)中制备的导电混合组分、配方量的魔芋葡甘聚糖、配方量的壳聚糖、配方量的流变控制剂以及剩余配方量的稀释剂，在室温下，0.1～0.3MPa的真空下以600r/min的速率搅拌混合40min至均匀，然后加入配方量的固化剂和固化促进剂，以相同的真空条件搅拌混合，得到所述胶黏剂。(5) Preparation of adhesive: weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan The polysaccharide, the formula amount of chitosan, the formula amount of the rheology control agent and the remaining formula amount of the diluent are stirred and mixed at a rate of 600 r/min for 40 min at room temperature under a vacuum of 0.1 to 0.3 MPa until homogeneous, and then added. A formulation amount of a curing agent and a curing accelerator are stirred and mixed under the same vacuum conditions to obtain the adhesive.
实施例2Example 2
一种高导热导电环保胶黏剂，包括如下重量份组分：改性环氧树脂50份、魔芋葡甘聚糖30份、壳聚糖20份、导热填料25份、导电填料15份、稀释剂8份、固化剂8份、固化促进剂3份、流变控制剂5份。 A high thermal conductivity conductive environmentally friendly adhesive comprising the following components by weight: 50 parts of modified epoxy resin, 30 parts of konjac glucomannan, 20 parts of chitosan, 25 parts of thermally conductive filler, 15 parts of conductive filler, diluted 8 parts of the agent, 8 parts of the curing agent, 3 parts of the curing accelerator, and 5 parts of the rheology control agent.
其中，所述改性环氧树脂为丁腈橡胶增韧改性环氧树脂。Wherein, the modified epoxy resin is a nitrile rubber toughened modified epoxy resin.
所述导热填料包括质量比为7：5:3的Ag-AIN颗粒、氮化铝和氧化铝。The thermally conductive filler includes Ag-AIN particles, aluminum nitride, and aluminum oxide in a mass ratio of 7:5:3.
所述导电填料包括质量比为3:4的镀银多壁碳纳米管和微米银粉。The conductive filler includes silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 3:4.
上述高导热导电环保胶黏剂的制备方法，包括如下步骤：The preparation method of the above high thermal conductivity conductive environment-friendly adhesive comprises the following steps:
(1)制备Ag-AIN颗粒：首先将A1N颗粒放在马弗炉中于800℃下高温处理3h，之后采用酸性清洗液清洗并用冷却的去离子水冲洗、真空干燥，最后采用无钯化学镀法在其表面沉积上一层致密的金属Ag镀层，得到所述Ag-AIN颗粒；(1) Preparation of Ag-AIN particles: First, the A1N particles were placed in a muffle furnace at 800 ° C for 3 h, then washed with an acidic cleaning solution and rinsed with cooled deionized water, vacuum dried, and finally palladium-free electroless plating. The method deposits a dense metal Ag plating on the surface thereof to obtain the Ag-AIN particles;
所述酸性清洗液为高铬酸钾和高锰酸钾以1:0.5的摩尔体积混合的混合液；The acidic cleaning solution is a mixture of potassium perchromate and potassium permanganate in a molar volume of 1:0.5;
(2)制备导热混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(1)中制备的Ag-AIN颗粒和配方量的其他导热填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在室温下，于0.1～0.3MPa的真空度下400r/min的速率搅拌混合35min，得到导热混合组分；(2) Preparation of thermally conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, Ag-AIN particles prepared in step (1) and other thermally conductive fillers of formula amount and 1/4~ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, and stirred at a rate of 400 r/min under a vacuum of 0.1 to 0.3 MPa for 35 minutes at room temperature to obtain a thermally conductive mixed component;
(3)制备镀银碳纳米管：称取配方量的多壁碳纳米管放入盛有酸化液的烧瓶中，超声处理，洗涤至中性并干燥，最后采用无钯化学镀法在其表面及管内沉积上一层致密的金属Ag镀层，得到所述镀银碳纳米管；(3) Preparation of silver-plated carbon nanotubes: Weigh a formula of multi-walled carbon nanotubes into a flask containing an acidified solution, sonicate, wash to neutrality and dry, and finally use palladium-free electroless plating on the surface. And depositing a dense metal Ag plating layer in the tube to obtain the silver-plated carbon nanotube;
其中，所述酸化液为质量浓度为65％的浓硫酸和浓盐酸的混合酸；所述超声处理的方法为：80℃超声处理1.5h；Wherein the acidification liquid is a mixed acid of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 65%; the ultrasonic treatment method is: ultrasonic treatment at 80 ° C for 1.5 h;
(4)制备导电混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(3)中制备的镀银碳纳米管和配方量的其他导电填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在室温下，真空度为0.1～0.3MPa下以400r/min的速率搅拌混合35min，得到导电混合组分； (4) Preparation of conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, silver-plated carbon nanotubes prepared in step (3) and other conductive fillers of the formula and 1/4 ～ 3% of the formula amount of diluent is added to a vacuum mixer, and the mixture is stirred and mixed at a rate of 400 r/min for 35 min at room temperature under a vacuum of 0.1 to 0.3 MPa to obtain a conductive mixed component;
(5)制备胶黏剂：称取剩余配方量的改性环氧树脂、步骤(2)中制备的导热混合组分、步骤(3)中制备的导电混合组分、配方量的魔芋葡甘聚糖、配方量的壳聚糖、配方量的流变控制剂以及剩余配方量的稀释剂，在室温下，0.1～0.3MPa的真空下以1000r/min的速率搅拌混合20min至均匀，然后加入配方量的固化剂和固化促进剂，以相同的真空条件搅拌混合，得到所述胶黏剂。(5) Preparation of adhesive: weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan The polysaccharide, the formula amount of chitosan, the formula amount of the rheology control agent and the remaining formula amount of the diluent are stirred and mixed at a rate of 1000 r/min for 20 min at room temperature under a vacuum of 0.1 to 0.3 MPa until homogeneous, and then added. A formulation amount of a curing agent and a curing accelerator are stirred and mixed under the same vacuum conditions to obtain the adhesive.
上述方法得到的所述高导热导电环保胶黏剂，经测试，其电导率为高于8.9S/cm，热导率高于3.8W/(m·K)，粘结强度高，综合性能优异。The high thermal conductivity conductive environmentally friendly adhesive obtained by the above method has been tested to have a conductivity higher than 8.9 S/cm, a thermal conductivity higher than 3.8 W/(m·K), high bonding strength, and excellent overall performance. .
本发明通过合理的原料选择及配方设计，尤其是导热填料和导电填料的选择，通过化学镀银处理导热填料和导电的多壁碳纳米管，然后将导热填料与导电填料分布于部分基体树脂混合成混合组分，在于其他基体成分混合，有效提高了纳米级导热填料和导电填料与基体树脂之间的相容性，提高分散效果，从而最大程度地发挥其功能性；通过环氧树脂与魔芋葡甘聚糖和壳聚糖的混合使用，拓宽了基体的性能，同时提高了环保性。The invention combines the heat conductive filler and the conductive multi-wall carbon nanotube by electroless silver plating through reasonable raw material selection and formula design, especially the selection of the heat conductive filler and the conductive filler, and then distributes the heat conductive filler and the conductive filler to the partial matrix resin. The mixed component is mixed with other matrix components, which effectively improves the compatibility between the nano-scale thermal conductive filler and the conductive filler and the matrix resin, and improves the dispersion effect, thereby maximizing its functionality; through epoxy resin and konjac The combination of glucomannan and chitosan broadens the performance of the matrix while improving environmental friendliness.
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。 The above description is only the preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes can be made to the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and scope of the present invention are intended to be included within the scope of the present invention.

Claims (10)

  1. 一种高导热导电环保胶黏剂，其特征在于，包括如下重量份组分：改性环氧树脂40～50份、魔芋葡甘聚糖20～30份、壳聚糖15～20份、导热填料15～25份、导电填料10～15份、稀释剂5～8份、固化剂5～8份、固化促进剂1～3份、流变控制剂3～5份。A high thermal conductivity conductive environment-friendly adhesive characterized by comprising the following components by weight: 40-50 parts of modified epoxy resin, 20-30 parts of konjac glucomannan, 15-20 parts of chitosan, heat conduction 15 to 25 parts of the filler, 10 to 15 parts of the conductive filler, 5 to 8 parts of the diluent, 5 to 8 parts of the curing agent, 1 to 3 parts of the curing accelerator, and 3 to 5 parts of the rheology control agent.
  2. 根据权利要求1所述的高导热导电环保胶黏剂，其特征在于，所述改性环氧树脂为丁腈橡胶增韧改性环氧树脂。The high thermal conductivity conductive environmentally friendly adhesive according to claim 1, wherein the modified epoxy resin is a nitrile rubber toughened modified epoxy resin.
  3. 根据权利要求1所述的高导热导电环保胶黏剂，其特征在于，所述导热填料包括质量比为5～7：3～5:1～3的Ag-AIN颗粒、氮化铝和氧化铝。The high thermal conductivity conductive environment-friendly adhesive according to claim 1, wherein the thermally conductive filler comprises Ag-AIN particles, aluminum nitride and aluminum oxide in a mass ratio of 5 to 7:3 to 5:1 to 3 .
  4. 根据权利要求1所述的高导热导电环保胶黏剂，其特征在于，所述导电填料包括质量比为2～3:2～4的镀银多壁碳纳米管和微米银粉。The high thermal conductivity conductive environmentally friendly adhesive according to claim 1, wherein the conductive filler comprises silver-plated multi-walled carbon nanotubes and micron silver powder in a mass ratio of 2 to 3:2 to 4.
  5. 一种如权利要求1所述的高导热导电环保胶黏剂的制备方法，其特征在于，包括如下步骤：A method for preparing a high thermal conductivity conductive environmentally friendly adhesive according to claim 1, comprising the steps of:
    (1)制备Ag-AIN颗粒：首先将A1N颗粒放在马弗炉中高温处理，之后采用酸性清洗液清洗并用冷却的去离子水冲洗、干燥，最后采用无钯化学镀法在其表面沉积上一层致密的金属Ag镀层，得到所述Ag-AIN颗粒；(1) Preparation of Ag-AIN particles: The A1N particles are first placed in a muffle furnace for high temperature treatment, then washed with an acidic cleaning solution, rinsed with cooled deionized water, dried, and finally deposited on the surface by palladium-free electroless plating. a layer of dense metal Ag plating to obtain the Ag-AIN particles;
    (2)制备导热混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(1)中制备的Ag-AIN颗粒和配方量的其他导热填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在一定真空度下搅拌混合得到导热混合组分；(2) Preparation of thermally conductive mixed components: weigh 1/4 to 1/3 of the modified amount of modified epoxy resin, Ag-AIN particles prepared in step (1) and other thermally conductive fillers of formula amount and 1/4~ 1/3 of the formula amount of diluent is added to a vacuum mixing agitator, and stirred and mixed under a certain degree of vacuum to obtain a thermally conductive mixed component;
    (3)制备镀银碳纳米管：称取配方量的多壁碳纳米管放入盛有酸化液的烧瓶中，超声处理，洗涤至中性并干燥，最后采用无钯化学镀法在其表面及管内沉积上一层致密的金属Ag镀层，得到所述镀银碳纳米管；(3) Preparation of silver-plated carbon nanotubes: Weigh a formula of multi-walled carbon nanotubes into a flask containing an acidified solution, sonicate, wash to neutrality and dry, and finally use palladium-free electroless plating on the surface. And depositing a dense metal Ag plating layer in the tube to obtain the silver-plated carbon nanotube;
    (4)制备导电混合组分：称取1/4～1/3配方量的改性环氧树脂、步骤(3) 中制备的镀银碳纳米管和配方量的其他导电填料以及1/4～1/3配方量的稀释剂加入真空混合搅拌器中，在一定真空度下搅拌混合得到导电混合组分；(4) Preparation of conductive mixed components: weigh 1/4 to 1/3 of the amount of modified epoxy resin, step (3) The silver-plated carbon nanotubes prepared in the formula and the other conductive fillers of the formula amount and the diluent of 1/4 to 1/3 of the formula amount are added into a vacuum mixing agitator, and stirred and mixed under a certain degree of vacuum to obtain a conductive mixed component;
    (5)制备胶黏剂：称取剩余配方量的改性环氧树脂、步骤(2)中制备的导热混合组分、步骤(3)中制备的导电混合组分、配方量的魔芋葡甘聚糖、配方量的壳聚糖、配方量的流变控制剂以及剩余配方量的稀释剂，在真空下搅拌混合均匀，然后加入配方量的固化剂和固化促进剂，真空搅拌混合，得到所述胶黏剂。(5) Preparation of adhesive: weighing the remaining formula of the modified epoxy resin, the thermally conductive mixed component prepared in the step (2), the conductive mixed component prepared in the step (3), and the formula amount of konjac glucomannan The polysaccharide, the formula amount of chitosan, the formula amount of the rheology control agent and the remaining formula amount of the diluent are stirred and mixed uniformly under vacuum, and then the formula amount of the curing agent and the curing accelerator are added, and the mixture is stirred under vacuum to obtain a solution. Adhesive.
  6. 根据权利要求5所述的高导热导电环保胶黏剂的制备方法，其特征在于，所述步骤(1)中，所述高温处理的条件为：温度600～800℃，时间3～5h；所述酸性清洗液为高铬酸钾和高锰酸钾以1:0.5的摩尔体积混合的混合液。The method for preparing a high thermal conductivity conductive environment-friendly adhesive according to claim 5, wherein in the step (1), the high temperature treatment condition is: a temperature of 600 to 800 ° C, and a time of 3 to 5 h; The acidic cleaning solution is a mixture of potassium perchromate and potassium permanganate in a molar volume of 1:0.5.
  7. 根据权利要求5所述的高导热导电环保胶黏剂的制备方法，其特征在于，所述步骤(2)中，所述真空搅拌混合的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率300～400r/min，搅拌时间35～45min。The method for preparing a high thermal conductivity conductive environment-friendly adhesive according to claim 5, wherein in the step (2), the vacuum agitation mixing condition is: at room temperature, the degree of vacuum is 0.1 to 0.3 MPa, The stirring rate is 300-400 r/min, and the stirring time is 35-45 min.
  8. 根据权利要求5所述的高导热导电环保胶黏剂的制备方法，其特征在于，所述步骤(3)中，所述酸化液为质量浓度为55～65％的浓硫酸和浓盐酸的混合酸；所述超声处理的方法为：70～80℃超声处理1.5～2h。The method for preparing a high thermal conductivity conductive environment-friendly adhesive according to claim 5, wherein in the step (3), the acidifying solution is a mixture of concentrated sulfuric acid and concentrated hydrochloric acid having a mass concentration of 55-65%. The method of sonication is: ultrasonic treatment at 70-80 ° C for 1.5 to 2 h.
  9. 根据权利要求5所述的高导热导电环保胶黏剂的制备方法，其特征在于，所述步骤(4)中，所述真空搅拌混合的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率300～400r/min，搅拌时间35～45min。The method for preparing a high thermal conductivity conductive environment-friendly adhesive according to claim 5, wherein in the step (4), the vacuum agitation mixing condition is: a vacuum degree of 0.1 to 0.3 MPa at room temperature, The stirring rate is 300-400 r/min, and the stirring time is 35-45 min.
  10. 根据权利要求5所述的高导热导电环保胶黏剂的制备方法，其特征在于，所述步骤(5)中，所述真空搅拌混合的的条件为：室温下，真空度为0.1～0.3MPa，搅拌速率600～1000r/min，搅拌时间20～40min。 The method for preparing a high thermal conductivity conductive environment-friendly adhesive according to claim 5, wherein in the step (5), the vacuum agitation mixing condition is: a vacuum degree of 0.1 to 0.3 MPa at room temperature. The stirring rate is 600-1000 r/min, and the stirring time is 20-40 min.
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