CN112745787A - High-heat-dissipation pressure-sensitive adhesive and high-heat-dissipation sub-sensitive adhesive tape - Google Patents
High-heat-dissipation pressure-sensitive adhesive and high-heat-dissipation sub-sensitive adhesive tape Download PDFInfo
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- CN112745787A CN112745787A CN202110065487.1A CN202110065487A CN112745787A CN 112745787 A CN112745787 A CN 112745787A CN 202110065487 A CN202110065487 A CN 202110065487A CN 112745787 A CN112745787 A CN 112745787A
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/003—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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Abstract
The invention provides a high-heat-dissipation pressure-sensitive adhesive which comprises the following components in parts by weight: 30-50 parts of cis-1, 4-polyisoprene, 50-70 parts of acrylate soft monomer, 10-20 parts of acrylate hard monomer, 1-5 parts of internal crosslinking monomer, 1-3 parts of initiator, 2-5 parts of crosslinking agent, 5-15 parts of heat conducting particles, 12-20 parts of coumarone resin and 15-30 parts of dodecyl mercaptan. According to the invention, the specially prepared heat-conducting particles and the special preparation method are adopted, so that the heat-conducting and electricity-conducting performances are stable, the heat-conducting particles and the pressure-sensitive adhesive are better fused, and the whole heat conduction of the adhesive tape is uniform.
Description
Technical Field
The invention belongs to the technical field of adhesive tape preparation, and relates to high-heat-dissipation pressure-sensitive adhesive and a high-heat-dissipation sub-sensitive adhesive tape.
Background
With the development of microelectronic integration technology and high-density assembly technology of hollow printed boards, heat generated by electronic components is rapidly accumulated, so that the components can still reliably and normally work, and the timely and efficient heat dissipation capability becomes a key factor influencing the service life of the components. When the heat conducting pressure sensitive adhesive used as a thermal interface material is filled between a radiator and a heat source by virtue of the characteristics of good compressibility deformability and the like, the heating body and the radiator can be fixed together to form a whole, the existence of air with low heat conductivity coefficient is eliminated, the two interfaces are in close contact, and the heat radiating effect is improved.
Patent document CN107057600A discloses a preparation method of a water-based acrylic heat-conducting pressure-sensitive adhesive tape, which relies on coating heat-conducting pressure-sensitive adhesive on a glass fiber fabric layer, and the subsequent process needs to be cured for 24 hours at room temperature, which is long in time and troublesome in operation. Patent document CN105778845A discloses a preparation method of a solvent-based heat conductive pressure sensitive adhesive, which uses a volatile and toxic reagent in the preparation process, and the preparation method needs to be improved in terms of environmental protection and safety. Patent document CN106634724A discloses an acrylate solvent-free pressure-sensitive adhesive and a preparation method thereof, wherein a solvent is used to dissolve a mixed glue solution, and then the solvent is removed in vacuum to obtain the solvent-free pressure-sensitive adhesive.
In addition, aiming at heating devices such as an LED (light emitting diode) oversized screen, the heat generated by electronic equipment can be effectively removed, and the reliability and the service life of the product are directly influenced. The heat conducting adhesive tape is widely used because of the integration of heat conducting insulation and bonding functions, and has the characteristics of repeated use under the condition of no pollution, no pollution to the bonded surface after peeling, and the like. The conventional heat-conducting adhesive tape usually adopts a mode of coating a heat-conducting functional layer with a pressure-sensitive adhesive, and although the heat-conducting functional layer has high heat dissipation efficiency, the pressure-sensitive adhesive is a high-molecular compound and has low heat dissipation efficiency, so that the conventional heat-conducting adhesive tape has low comprehensive heat dissipation efficiency.
Disclosure of Invention
The invention aims to solve the problems that the common pressure-sensitive adhesive in electronic equipment and vehicle-mounted equipment in the prior art is difficult to dissipate heat and affects the service life of the electronic equipment, and the formula and the preparation method of the pressure-sensitive adhesive are deeply researched and developed to obtain the high-heat-dissipation pressure-sensitive adhesive and the preparation method thereof.
In order to achieve the purposes, the specific scheme is as follows:
the high-heat-dissipation pressure-sensitive adhesive comprises the following components in parts by weight: 30-50 parts of cis-1, 4-polyisoprene, 50-70 parts of acrylate soft monomer, 10-20 parts of acrylate hard monomer, 1-5 parts of internal crosslinking monomer, 1-3 parts of initiator, 2-5 parts of crosslinking agent, 5-15 parts of heat conducting particles, 12-20 parts of coumarone resin and 15-30 parts of dodecyl mercaptan.
The cross-linking agent is hexamethylene diisocyanate.
The internal crosslinking monomer is a mixture of N-hydroxymethyl acrylamide and glycidyl methacrylate in a weight ratio of 1: 2-5.
The acrylate soft monomer is a mixture of butyl acrylate and isooctyl acrylate;
preferably, the weight part ratio of butyl acrylate to isooctyl acrylate is 2-3: 1.
The acrylate hard monomer is a mixture of isobornyl methacrylate, methyl acrylate and methyl methacrylate;
preferably, the weight part ratio of isobornyl methacrylate, methyl acrylate and methyl methacrylate is 1:2-5: 1-3.
The initiator is azobisisoheptonitrile.
The preparation method of the heat conducting particle comprises the following steps: a) dissolving urea, epoxy resin and an initiator into formaldehyde, wherein the weight ratio of the urea to the formaldehyde is that sodium hydroxide is used for adjusting the pH value to 7-8, stirring at a low speed under the condition that the temperature is 60-80 ℃, carrying out heat preservation reaction for 0.5-4 hours to generate viscous and transparent urea-formaldehyde resin, adding deionized water which is equal to the total weight of the urea and the formaldehyde, and stirring at a low speed to obtain an epoxy resin modified urea-formaldehyde resin aqueous solution; b) putting the carbon nano tube with the diameter less than 20nm and an emulsifier into solvent water at normal temperature, uniformly stirring, and then shearing at the rotating speed of 2000 revolutions per minute for 10-20 minutes to form stable carbon nano tube suspension; c) reducing the shearing speed, firstly adding an epoxy resin modified urea-formaldehyde resin aqueous solution under the stirring condition, then dropwise adding dilute hydrochloric acid to adjust the pH value to 3.0, heating to 40-60 ℃, reacting for 1 hour, and adding a proper amount of dispersing agent after the particle wall solidification is finished; d) discharging: adding sodium hydroxide aqueous solution to adjust the pH value to 7.0, and then dehydrating and drying to 30-40% of the prior weight to obtain the heat conducting particles.
Preferably, the weight part ratio of the urea to the epoxy resin is as follows: 5-20:1
Preferably, the weight parts of the raw materials are respectively as follows: 30-40 parts of urea; 40-80 parts of formaldehyde and 5-10 parts of epoxy resin; 1-5 parts of initiator and 2-5 parts of emulsifier;
preferably, the emulsifier is one or more of alkylphenol polyoxyethylene ether, styrylphenol polyoxyethylene ether, alkylaryl phenol polyoxyethylene ether phosphate, castor oil polyoxyethylene ether, alkylbenzene sulfonate, alkylphenol polyoxyethylene phosphate, di-sec-octyl maleate sodium sulfonate, polyol fatty acid ester and ethylene oxide adduct thereof; the dispersant is one or more of SOPA-270, dispersant NNO, sodium lignin sulfonate and dispersant 2700.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) adding cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol into a reaction kettle for mixing, heating to 85-88 ℃, 2) adding an initiator and a crosslinking agent into the reaction kettle, keeping the temperature of 85-88 ℃ for 15-30min, and then cooling to obtain the high-heat-dissipation pressure-sensitive adhesive of example 1. The preparation method of the high-heat-dissipation pressure-sensitive adhesive tape comprises the steps of coating the high-heat-dissipation pressure-sensitive adhesive on a base material, attaching a release film, and preparing the high-heat-dissipation sub-sensitive adhesive tape.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, the specially prepared heat-conducting particles and the special preparation method are adopted, so that the heat-conducting and electricity-conducting performances are stable, the heat-conducting particles and the pressure-sensitive adhesive are better fused, and the whole heat conduction of the adhesive tape is uniform.
2. The invention adopts the combination of the acrylate hard monomer and the acrylate soft elastomer, and adopts the acrylate monomer and the hexamethylene diisocyanate for crosslinking to form the adhesive tape with strong mechanical property and strong adhesive force on the base material.
3. According to the invention, through a large number of innovations and tests, the fact that the coumarone resin is coupled with the acrylic ester monomer and the 1, 4-polyisoprene through the azodiisoheptanonitrile is found, and the prepared pressure-sensitive adhesive is moderate in viscosity and enhanced in acid and alkali resistance.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A first part: preparing heat conducting particles: a) dissolving urea, epoxy resin and an initiator into formaldehyde, wherein the weight ratio of the urea to the formaldehyde is 1: 1-1: 2.5, adjusting the pH value to 7-8 by using sodium hydroxide, stirring at a low speed under the condition of a temperature of 60-80 ℃, carrying out heat preservation reaction for 0.5-4 hours to generate viscous and transparent urea-formaldehyde resin, adding deionized water which is equal to the total weight of the urea and the formaldehyde, and stirring at a low speed to obtain an epoxy resin modified urea-formaldehyde resin aqueous solution; b) putting the carbon nano tube with the diameter less than 20nm and an emulsifier into solvent water at normal temperature, uniformly stirring, and then shearing at the rotating speed of 2000 revolutions per minute for 10-20 minutes to form stable carbon nano tube suspension; c) reducing the shearing speed, firstly adding an epoxy resin modified urea-formaldehyde resin aqueous solution under the stirring condition, then dropwise adding dilute hydrochloric acid to adjust the pH value to 3.0, heating to 40-60 ℃, reacting for 1 hour, and adding a proper amount of dispersing agent after the particle wall solidification is finished; d) discharging: adding sodium hydroxide aqueous solution to adjust the pH value to 7.0, and then dehydrating and drying to 30-40% of the prior weight to obtain the heat conducting particles.
Example 1
Weighing the following raw materials in parts by weight: 30kg of cis 1, 4-polyisoprene, 50kg of acrylate soft monomer, 13kg of acrylate hard monomer, 5kg of internal crosslinking monomer, 1kg of azobisisoheptonitrile, 5kg of hexamethylene diisocyanate, 10kg of heat conducting particles, 20kg of coumarone resin and 30kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 1 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 1 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 1.
Example 2
Weighing the following raw materials in parts by weight: 32kg of cis 1, 4-polyisoprene, 70kg of acrylate soft monomer, 15kg of acrylate hard monomer, 3kg of internal crosslinking monomer, 2kg of azobisisoheptonitrile, 4kg of hexamethylene diisocyanate, 15kg of heat conducting particles, 12kg of coumarone resin and 20kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azodiisoheptanonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 2 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 2 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 2.
Example 3
Weighing the following raw materials in parts by weight: 40kg of cis 1, 4-polyisoprene, 52kg of acrylate soft monomer, 14kg of acrylate hard monomer, 1kg of internal crosslinking monomer, 3kg of azobisisoheptonitrile, 3kg of hexamethylene diisocyanate, 5kg of heat conducting particles, 18kg of coumarone resin and 18kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 3 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 3 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 3.
Example 4
Weighing the following raw materials in parts by weight: 42kg of cis 1, 4-polyisoprene, 55kg of acrylate soft monomer, 10kg of acrylate hard monomer, 4kg of internal crosslinking monomer, 3kg of azobisisoheptonitrile, 2kg of hexamethylene diisocyanate, 12kg of thermally conductive particles, 15kg of coumarone resin and 26kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 4 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 4 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 4.
Example 5
Weighing the following raw materials in parts by weight: 48kg of cis 1, 4-polyisoprene, 60kg of acrylate soft monomer, 20kg of acrylate hard monomer, 2kg of internal crosslinking monomer, 2kg of azobisisoheptonitrile, 2kg of hexamethylene diisocyanate, 14kg of thermally conductive particles, 16kg of coumarone resin and 28kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 5 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 5 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 5.
Example 6
Weighing the following raw materials in parts by weight: 50kg of cis 1, 4-polyisoprene, 65kg of acrylate soft monomer, 18kg of acrylate hard monomer, 3kg of internal crosslinking monomer, 1kg of azobisisoheptonitrile, 4kg of hexamethylene diisocyanate, 8kg of heat conducting particles, 17kg of coumarone resin and 22kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 6 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 6 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 6.
Example 7
Weighing the following raw materials in parts by weight: 46kg of cis 1, 4-polyisoprene, 62kg of acrylate soft monomer, 11kg of acrylate hard monomer, 5kg of internal crosslinking monomer, 1kg of azobisisoheptonitrile, 5kg of hexamethylene diisocyanate, 6kg of thermally conductive particles, 15kg of coumarone resin and 25kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 7 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 7 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 7.
Example 8
Weighing the following raw materials in parts by weight: 36kg of cis 1, 4-polyisoprene, 68kg of acrylate soft monomer, 12kg of acrylate hard monomer, 1kg of internal crosslinking monomer, 2kg of azobisisoheptonitrile, 4kg of hexamethylene diisocyanate, 9kg of heat conducting particles, 18kg of coumarone resin and 29kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 8 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 8 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 8.
Example 9
Weighing the following raw materials in parts by weight: 38kg of cis 1, 4-polyisoprene, 66kg of acrylate soft monomer, 17kg of acrylate hard monomer, 4kg of internal crosslinking monomer, 3kg of azobisisoheptonitrile, 3kg of hexamethylene diisocyanate, 14kg of heat conducting particles, 14kg of coumarone resin and 24kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 9 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 9 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 9.
Example 10
Weighing the following raw materials in parts by weight: 35kg of cis 1, 4-polyisoprene, 58kg of acrylate soft monomer, 16kg of acrylate hard monomer, 2kg of internal crosslinking monomer, 2kg of azobisisoheptonitrile, 2kg of hexamethylene diisocyanate, 10kg of thermally conductive particles, 12kg of coumarone resin and 21kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol are added into a reaction kettle to be mixed, the temperature is raised to 85-88 ℃, 2) azobisisoheptonitrile and hexamethylene diisocyanate are added into the reaction kettle, the temperature is maintained at 85-88 ℃ for 15-30min, and then the temperature is lowered, so that the high-heat-dissipation pressure-sensitive adhesive of the embodiment 10 is obtained.
The preparation method of the high heat dissipation pressure sensitive adhesive tape comprises the steps of coating the high heat dissipation pressure sensitive adhesive of the embodiment 10 on a substrate, attaching a release film, and preparing the high heat dissipation sub-sensitive adhesive tape of the embodiment 10.
A second part:
comparative example 1
Weighing the following raw materials in parts by weight: 30kg of cis 1, 4-polyisoprene, 50kg of acrylate soft monomer, 13kg of acrylate hard monomer, 5kg of internal crosslinking monomer, 1kg of azobisisoheptonitrile, 5kg of hexamethylene diisocyanate, 10kg of carbon nanotubes, 20kg of coumarone resin and 30kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) adding cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, a carbon nano tube, coumarone resin and dodecanethiol into a reaction kettle for mixing, heating to 85-88 ℃, 2) adding azobisisoheptonitrile and hexamethylene diisocyanate into the reaction kettle, keeping the temperature at 85-88 ℃ for 15-30min, and then cooling to obtain the pressure-sensitive adhesive of the comparative example 1.
The preparation method of the pressure-sensitive adhesive tape comprises the steps of coating the pressure-sensitive adhesive in the comparative example 1 on a substrate, attaching a release film, and preparing the sub-sensitive adhesive tape in the comparative example 1.
Comparative example 2
Weighing the following raw materials in parts by weight: 32kg of cis 1, 4-polyisoprene, 70kg of acrylate soft monomer, 15kg of acrylate hard monomer, 3kg of internal crosslinking monomer, 2kg of azobisisoheptonitrile, 4kg of hexamethylene diisocyanate, 15kg of heat conducting particles and 20kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) adding cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, heat conducting particles and dodecanethiol into a reaction kettle for mixing, heating to 85-88 ℃, 2) adding azodiisoheptanonitrile and hexamethylene diisocyanate into the reaction kettle, keeping the temperature of 85-88 ℃ for 15-30min, and then cooling to obtain the pressure-sensitive adhesive of the comparative example 2.
The preparation method of the pressure-sensitive adhesive tape comprises the steps of coating the pressure-sensitive adhesive of the embodiment 2 on a substrate, attaching a release film, and preparing the sub-sensitive adhesive tape of the embodiment 2.
Comparative example 3
Weighing the following raw materials in parts by weight: 40kg of cis 1, 4-polyisoprene, 52kg of soft acrylate monomer, 1kg of internal crosslinking monomer, 3kg of azobisisoheptonitrile, 3kg of hexamethylene diisocyanate, 5kg of heat conducting particles, 18kg of coumarone resin and 18kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) adding cis-1, 4-polyisoprene, an acrylate soft monomer, an internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol into a reaction kettle for mixing, heating to 85-88 ℃, 2) adding azodiisoheptanonitrile and hexamethylene diisocyanate into the reaction kettle, keeping the temperature of 85-88 ℃ for 15-30min, and then cooling to obtain the pressure-sensitive adhesive of the comparative example 3.
The preparation method of the pressure-sensitive adhesive tape comprises the steps of coating the pressure-sensitive adhesive in the comparative example 3 on a substrate, attaching a release film, and preparing the sub-sensitive adhesive tape in the comparative example 3.
Comparative example 4
Weighing the following raw materials in parts by weight: 42kg of cis 1, 4-polyisoprene, 55kg of acrylate soft monomer, 10kg of acrylate hard monomer, 4kg of internal crosslinking monomer, 3kg of azobisisoheptonitrile, 2kg of hexamethylene diisocyanate, 12kg of carbon nanotubes, 15kg of coumarone resin and 26kg of dodecanethiol.
The preparation method of the high-heat-dissipation pressure-sensitive adhesive comprises the following steps:
1) adding cis-1, 4-polyisoprene, an acrylate soft monomer, an acrylate hard monomer, an internal crosslinking monomer, a carbon nano tube, coumarone resin and dodecanethiol into a reaction kettle for mixing, heating to 85-88 ℃, 2) adding azobisisoheptonitrile and hexamethylene diisocyanate into the reaction kettle, keeping the temperature at 85-88 ℃ for 15-30min, and then cooling to obtain the pressure-sensitive adhesive of the comparative example 4.
The preparation method of the pressure-sensitive adhesive tape comprises the steps of coating the pressure-sensitive adhesive of the comparative example 4 on a substrate, attaching a release film, and preparing the sub-sensitive adhesive tape of the comparative example 4.
The pressure-sensitive adhesive and the sub-sensitive adhesive tape of the 10 examples and the 4 comparative examples described above were subjected to a peel test according to the test method of national standard GB/T2792-2014180 °, three times of which are averaged, and the test method is as follows:
1. 180 ° peel strength of pressure sensitive adhesive:
according to GB/T2792-2014 180-degree peel strength test method of the pressure-sensitive adhesive tape, an electronic universal tester is adopted for measurement (the adhered material is a standard test steel plate, and the peeling rate is 300 mm/min).
2. Coefficient of thermal conductivity:
the heat conductivity was measured according to ASTM D5470 standard, using a thermal conductivity measuring apparatus DRL-III.
3. Tensile strength:
the method for testing the tensile strength of the pressure-sensitive adhesive refers to the GB 7753-871 standard method.
4. Initial viscosity energy: the test was carried out in an oven at 180 ℃ according to the standard GB/T4851-2014 and the time was recorded.
The test results are given in the following table:
it can be seen from the above examples that, in examples 1 to 10, compared with comparative examples 1 to 4, comparative examples 1 and 4 do not use heat conducting particles, although the amount of carbon nanotubes is larger, the heat conducting performance is not as good as that of examples 1 to 10, the viscosity of comparative examples 1 to 4 is greatly reduced, the mechanical strength of comparative example 2 is obviously reduced, and the phenomenon of glue transfer residue is caused while the viscosity is increased. Comparative example 3 has a reduced viscosity but has lower mechanical properties and remains when transferring glue, so it can be seen from the above data that examples 1-10 of the present invention have significant advantages over the prior art.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The high-heat-dissipation pressure-sensitive adhesive comprises the following components in parts by weight: 30-50 parts of cis-1, 4-polyisoprene, 50-70 parts of acrylate soft monomer, 10-20 parts of acrylate hard monomer, 1-5 parts of internal crosslinking monomer, 1-3 parts of initiator, 2-5 parts of crosslinking agent, 5-15 parts of heat conducting particles, 12-20 parts of coumarone resin and 15-30 parts of dodecyl mercaptan.
2. The high heat dissipation pressure-sensitive adhesive of claim 1, wherein: the cross-linking agent is hexamethylene diisocyanate, and the initiator is azobisisoheptonitrile.
3. The high heat dissipation pressure-sensitive adhesive of claim 1, wherein: the internal crosslinking monomer is a mixture of N-hydroxymethyl acrylamide and glycidyl methacrylate in a weight ratio of 1: 2-5.
4. The high heat dissipation pressure-sensitive adhesive of claim 1, wherein: the acrylate soft monomer is a mixture of butyl acrylate and isooctyl acrylate;
5. the high heat dissipation pressure-sensitive adhesive of claim 4, wherein: the weight portion ratio of the butyl acrylate to the isooctyl acrylate is 2-3: 1.
6. The high heat dissipation pressure-sensitive adhesive of claim 1, wherein: the acrylate hard monomer is a mixture of isobornyl methacrylate, methyl acrylate and methyl methacrylate;
7. the high heat dissipation pressure-sensitive adhesive of claim 6, wherein: the weight portion ratio of isobornyl methacrylate to methyl acrylate to methyl methacrylate is 1:2-5: 1-3.
8. The high heat dissipation pressure-sensitive adhesive of claim 1, wherein: the preparation method of the heat conducting particle comprises the following steps: a) dissolving urea, epoxy resin and an initiator into formaldehyde, wherein the weight ratio of the urea to the formaldehyde is that sodium hydroxide is used for adjusting the pH value to 7-8, stirring at a low speed under the condition that the temperature is 60-80 ℃, carrying out heat preservation reaction for 0.5-4 hours to generate viscous and transparent urea-formaldehyde resin, adding deionized water which is equal to the total weight of the urea and the formaldehyde, and stirring at a low speed to obtain an epoxy resin modified urea-formaldehyde resin aqueous solution; b) putting the carbon nano tube with the diameter less than 20nm and an emulsifier into solvent water at normal temperature, uniformly stirring, and then shearing at the rotating speed of 2000 revolutions per minute for 10-20 minutes to form stable carbon nano tube suspension; c) reducing the shearing speed, firstly adding an epoxy resin modified urea-formaldehyde resin aqueous solution under the stirring condition, then dropwise adding dilute hydrochloric acid to adjust the pH value to 3.0, heating to 40-60 ℃, reacting for 1 hour, and adding a proper amount of dispersing agent after the particle wall solidification is finished; d) discharging: adding sodium hydroxide aqueous solution to adjust the pH value to 7.0, and then dehydrating and drying to 30-40% of the prior weight to obtain the heat conducting particles.
9. A high heat dissipation sub-sensitive adhesive comprises the following preparation methods: 1) the formulation of any one of claim 18, adding cis 1, 4-polyisoprene, soft acrylate monomer, hard acrylate monomer, internal crosslinking monomer, heat conducting particles, coumarone resin and dodecanethiol into a reaction kettle, mixing, heating to 85-88 ℃, 2) adding initiator and crosslinking agent into the reaction kettle, keeping the temperature at 85-88 ℃ for 15-30min, and then cooling to obtain the high heat dissipation thermosensitive adhesive according to any one of claims 1-8.
10. A high-heat-dissipation sub-sensitive adhesive tape is prepared by the following steps: coating the high heat dissipation pressure-sensitive adhesive prepared in claim 9 on a substrate, and attaching a release film to form a high heat dissipation sub-sensitive adhesive tape.
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| CN113695512A (en) * | 2021-08-31 | 2021-11-26 | 江西特欣实业有限公司 | Preparation method of fast-curing low-temperature collapsible precoated sand |
| CN114316837A (en) * | 2022-01-13 | 2022-04-12 | 东莞市富印胶粘科技有限公司 | Double-curing pressure-sensitive adhesive tape |
| CN114456734A (en) * | 2022-01-13 | 2022-05-10 | 东莞市富印胶粘科技有限公司 | Acrylate pressure-sensitive adhesive and preparation method thereof |
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