CN113322039B - Single-component silane modified polyether heat conduction material and preparation method thereof - Google Patents
Single-component silane modified polyether heat conduction material and preparation method thereof Download PDFInfo
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- CN113322039B CN113322039B CN202110564268.8A CN202110564268A CN113322039B CN 113322039 B CN113322039 B CN 113322039B CN 202110564268 A CN202110564268 A CN 202110564268A CN 113322039 B CN113322039 B CN 113322039B
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
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Abstract
The invention discloses a single-component silane modified polyether heat conduction material which comprises the following components in parts by weight: 5-30 parts of double-end siloxy modified polyether resin, 0-15 parts of single-end siloxy modified polyether diluent, 50-90 parts of aluminum hydroxide, 0.5-5.0 parts of graphene, 0.05-3.0 parts of cross-linking agent, 0.05-2.0 parts of coupling agent prepolymer and 0.05-2.0 parts of catalyst. The invention also discloses a preparation method of the single-component silane modified polyether heat conduction material. The single-component silane modified polyether heat conduction material has excellent insulating and heat conduction effects and good bonding effects, improves the adjustment space of the formula and the long-term use stability, has little abrasion to equipment, is particularly suitable for the electronic industry with high automation and high dispensing precision, can effectively reduce the loss of the equipment, and greatly reduces the use cost.
Description
Technical Field
The invention belongs to the field of adhesives, and particularly relates to a single-component silane modified polyether heat conduction material and a preparation method thereof.
Background
Along with the rapid development of the electronic industry, electronic equipment is more and more exquisite, and the integration degree of electronic components is higher and higher, so that heat dissipation gradually becomes an important demand which is not negligible in the electronic industry. Traditional heat dissipation materials often adopt alumina as heat conduction filler, not only can provide higher coefficient of heat conductivity, better insulating properties, have good simultaneously and fall this effect. However, the mohs hardness of alumina is 9, which is only slightly lower than that of diamond, so that the equipment is seriously abraded in the using process. Modern electronic industry has gradually developed into high automation and high dispensing precision, and accurate automatic production can be easily realized by adopting equipment such as a screw type dispensing machine and the like. However, the heat conductive material using alumina has a very large loss in the dispenser during long-term use, and the cost caused by replacing the dispensing parts is not negligible.
The modified silane polyether material has the advantages of good durability, wide adhesion, paintability, low pollution, environmental friendliness, weather resistance and the like, and is generally concerned and developed in the building, industrial and electronic industries. The traditional modified silane polyether material usually needs to be added with a large amount of plasticizer to achieve the effects of reducing viscosity and hardness, the method is very effective, but the problems of oil bleeding, poor aging stability and the like in the long-term use process are also brought.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a single-component silane modified polyether heat conduction material and a preparation method thereof. The single-component silane modified polyether heat conduction material has excellent insulating and heat conduction effects and good bonding effects, is suitable for bonding of various materials such as metal, plastic and the like, and is a functional bonding material capable of effectively dissipating heat. According to the invention, the single-ended siloxy modified polyether diluent is adopted, so that the adjustment space and the long-term use stability of the formula are improved, and the problems of oil bleeding and aging are avoided; meanwhile, the heat conduction system adopting the aluminum hydroxide composite graphene not only has a high heat conduction effect, but also has small abrasion to equipment, is particularly suitable for the electronic industry with high automation and high dispensing precision, can effectively reduce the loss of the equipment, and greatly reduces the use cost.
The specific technical scheme is as follows:
one of the purposes of the invention is to provide a single-component silane modified polyether heat conduction material which is a functional bonding material capable of effectively dissipating heat, and comprises the following components (A) to (G) in parts by weight:
(A) 5-30 parts of bi-terminal siloxy modified polyether resin;
(B) 0-15 parts of single-end siloxy modified polyether diluent;
(C) 50-90 parts of aluminum hydroxide;
(D) 0.5-5.0 parts of graphene;
(E) 0.05 to 3.0 portions of cross-linking agent
(F) 0.05-2.0 parts of a coupling agent prepolymer;
(G) 0.05-2.0 parts of catalyst.
On the basis of the patent, the adjustment of corresponding application requirements can be carried out: such as addition of fluorescent agents, antioxidants, photostability, UV absorbers, etc.
Further, the double-terminal siloxy modified polyether resin of the component (A) is a polyether resin with both ends of a molecular chain blocked by trimethoxy silane, and the viscosity range of the polyether resin is preferably 500 to 30000 mPas. The concrete choice is Wake
STP-E10, wake
STP-E30, wacke XB502, KANEKAMS polymer S203H, KANEKA SAT010, KANEKA SAX400 or more.
Further, the single-terminal siloxy modified polyether diluent of component (B) is a polyether diluent in which one end of the molecular chain is blocked by trimethoxy silane and the other end is blocked by trimethyl silane, and the viscosity thereof is preferably 200 to 5000 mPas. In particular, KANEKA SAT145 may be used, and custom products may also be used.
Further, the aluminum hydroxide of the component (C) is spherical aluminum hydroxide, and the particle diameter thereof is preferably 50 μm or less. It is preferable to use a mixture of several aluminum hydroxides having different particle sizes.
Further, the component (D), graphene, is subjected to oxidation coating treatment; specifically, the graphene as the component (D) is graphene subjected to oxidation treatment and silane surface modification.
And further, the graphene is subjected to hydrogen peroxide oxidation treatment. Wherein the dosage of the hydrogen peroxide is preferably 1 to 5wt percent, most preferably 2.5wt percent based on the weight of the raw material graphene.
And further, carrying out silane surface modification by using hexamethyl silazane after graphene oxidation treatment. The hexamethyl silazane is preferably used in an amount of 0.5 to 10wt%, most preferably 5wt%, based on the weight of the raw material graphene.
Specifically, the graphene treatment process comprises the following steps:
adding raw material graphene into a roller dryer, spraying hydrogen peroxide which is 1-5 wt% of the weight of the raw material graphene, and rolling and dispersing uniformly at room temperature; and then, spraying hexamethyl silazane accounting for 0.5-10 wt% of the weight of the graphene as the raw material, rolling and dispersing for 1 hour at room temperature, gradually heating to 100 ℃, and drying for later use.
Further, the crosslinking agent of the component (E) is one or more than two of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, methyl orthosilicate, ethyl orthosilicate, phenyltrimethoxysilane, phenylvinyldimethoxysilane and dimethyldimethoxysilane.
Further, the prepolymer of the coupling agent of component (F) is a prepolymer of gamma- (2,3-glycidoxy) propyltrimethoxysilane (KH-560) and 3-aminopropyltrimethoxysilane (KH-540).
Wherein the mass ratio of KH-560 to KH-540 is preferably 4: (2 to 5), most preferably 4:3.
specifically, the preparation method of the coupling agent prepolymer comprises the following steps:
under the nitrogen atmosphere, mixing a mixture of 4: and (2) adding KH-560 and KH-540 into a reaction kettle, gradually heating to 100 ℃, keeping the temperature for reaction for 6 hours, cooling to room temperature, and introducing nitrogen for storage to obtain the coupling agent prepolymer.
Further, the component (G) catalyst is a titanate catalyst.
Still further, the titanate catalyst can be one or more than two of common commercially available titanate coupling agents such as TYZOR 722, TYZOR 726, KR-38S, KR-12, KR-TTS, KRTi-1, KRTi-2 and the like.
The invention also aims to provide a preparation method of the silane modified polyether heat conduction material, which comprises the following steps:
under the environment that the humidity is lower than 30RH%, adding (A) double-end siloxy modified polyether resin, (B) single-end siloxy modified polyether diluent, and (D) graphene into a stirring kettle, uniformly mixing, adding (C) aluminum hydroxide, uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, finally adding (E) cross-linking agent, (F) coupling agent prepolymer and (G) catalyst, and uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
The invention has the following beneficial effects:
(1) The aluminum oxide heat-conducting filler with the Mohs hardness of 9 is abandoned, and the heat-conducting system of aluminum hydroxide (Mohs hardness of 3.0) composite graphene is selected, so that the high heat-conducting coefficient of 2.0W/m.k can be prepared in a compounding manner, the aluminum hydroxide has low hardness, and the graphite has a lubricating effect, so that the aluminum hydroxide has small abrasion to equipment, is particularly suitable for the electronic industry with high automation and high dispensing precision, can effectively reduce the loss of the equipment, and greatly reduces the use cost.
(2) The graphene is subjected to oxidation coating treatment, so that the insulativity of the graphene material is increased, the thermal conductivity of the composite material is improved, and the insulativity of the material is not sacrificed.
(3) The self-made coupling agent prepolymer is adopted, the epoxy group is opened in advance, so that the material has a good bonding effect, is suitable for bonding of various materials such as metal, plastic and the like, eliminates the existence of primary amine, and improves the high-temperature stability of the material.
(4) The single-end silicon alkoxy modified polyether diluent is adopted, so that the introduction of a plasticizer is avoided, no micromolecule is separated out in the long-term use process, no pollution is caused to components, and the material reliability is excellent.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
In a specific embodiment, the graphene oxidation coating treatment process comprises the following steps:
adding raw material graphene into a drum dryer, spraying hydrogen peroxide with the weight of 2.5wt% of the raw material graphene, and rolling and dispersing uniformly at room temperature; and then, spraying hexamethyl silazane accounting for 5wt% of the weight of the raw material graphene, rolling and dispersing for 1 hour at room temperature, gradually heating to 100 ℃, and drying for later use.
In a specific embodiment, the coupling agent prepolymer is prepared as follows:
under the nitrogen atmosphere, mixing a mixture of 4: adding KH-560 and KH-540 of 3 into a reaction kettle, gradually heating to 100 ℃, keeping the temperature for reaction for 6 hours, cooling to room temperature, and filling nitrogen for storage to obtain a coupling agent prepolymer.
In specific embodiments, the "parts" are all parts by weight.
Example 1
Under the environment of room temperature and humidity lower than 30RH%, 8 parts of 10000 mPas double-end siloxy modified polyether resin STP-E10, 6.45 parts of 2000 mPas double-end siloxy modified polyether resin XB502 and 1 part of graphene after oxidation coating treatment are weighed and evenly mixed, 40 parts of spherical aluminum hydroxide with the average particle size of 5 mu m and 45 parts of spherical aluminum hydroxide with the average particle size of 25 mu m are added and evenly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, and finally 0.2 part of vinyl trimethoxy silane, 0.1 part of methyl trimethoxy silane, 0.1 part of dimethyl dimethoxy silane, 0.05 part of coupling agent prepolymer and 0.1 part of catalyst TYR 722 are added and evenly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, so that the single-component silane modified polyether heat conduction material is obtained.
Example 2
Under the environment of room temperature and humidity lower than 30RH%, 22 parts of 10000 mPas double-end siloxy modified polyether resin STP-E10, 5.85 parts of 3000 mPas single-end siloxy modified polyether diluent SAT145 and 4.8 parts of graphene after oxidation coating are weighed and evenly mixed, 15 parts of spherical aluminum hydroxide with the average particle size of 5 microns and 50 parts of spherical aluminum hydroxide with the average particle size of 10 microns are added, the mixture is evenly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, finally, 0.2 part of vinyl trimethoxy silane, 0.1 part of methyl trimethoxy silane, 0.05 part of methyl phenyl dimethoxy silane, 1 part of coupling agent prepolymer and 1 part of catalyst KR-TTS are added, and the mixture is evenly stirred under the vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, so that the single-component silane modified polyether heat conduction material is obtained.
Example 3
Weighing 8 parts of 8000 mPas double-end siloxy modified polyether resin S203H, 2 parts of 600 mPas double-end siloxy modified polyether resin SAT010, 3 parts of 1000 mPas customized single-end siloxy modified polyether diluent and 0.75 part of graphene after oxidation coating treatment at room temperature and under the environment of humidity lower than 30RH%, uniformly mixing, adding 20 parts of spherical aluminum hydroxide with the average particle size of 5 mu m and 65 parts of spherical aluminum hydroxide with the average particle size of 25 mu m, uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, finally adding 0.2 part of vinyl trimethoxy silane, 0.05 part of methyl trimethoxy silane, 0.7 part of coupling agent prepolymer and 0.3 part of catalyst KRTi-2, and uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
Example 4
Weighing 6 parts of 30000 mPas double-end siloxy modified polyether resin STP-E30, 12 parts of 3000 mPas single-end siloxy modified polyether diluent SAT145 and 2 parts of graphene after oxidation coating treatment at room temperature and humidity of less than 30RH%, uniformly mixing, adding 10 parts of spherical aluminum hydroxide with the average particle size of 2 mu m and 65 parts of spherical aluminum hydroxide with the average particle size of 10 mu m, uniformly stirring under the vacuum conditions of less than 35 ℃ and more than 0.09MPa, finally adding 1.5 parts of vinyltrimethoxysilane, 1.0 part of methyltrimethoxysilane, 1.5 parts of coupling agent prepolymer and 1.0 part of catalyst KRTi-1, and uniformly stirring under the vacuum conditions of less than 35 ℃ and more than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
Example 5
Weighing 10 parts of 24000 mPas double-end siloxy modified polyether resin SAX400, 12 parts of 1000 mPas customized single-end siloxy modified polyether diluent and 2.5 parts of graphene after oxidation coating treatment at room temperature and humidity lower than 30RH%, uniformly mixing, adding 5 parts of spherical aluminum hydroxide with the average particle size of 2 microns, 25 parts of spherical aluminum hydroxide with the average particle size of 10 microns and 40 parts of spherical aluminum hydroxide with the average particle size of 20 microns, uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, finally adding 1.5 parts of vinyltrimethoxysilane, 1.0 part of methyltrimethoxysilane, 1.0 part of coupling agent prepolymer and 2.0 parts of catalyst KR-38S, and uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
Comparative example 1
Under the environment of room temperature and humidity lower than 30RH%, 22 parts of 10000 mPas double-end siloxy modified polyether resin STP-E10, 5.85 parts of 3000 mPas single-end siloxy modified polyether diluent SAT145 and 4.8 parts of graphene which is not subjected to peroxide coating treatment are weighed and uniformly mixed, 15 parts of spherical aluminum hydroxide with the average particle size of 5 mu m and 50 parts of spherical aluminum hydroxide with the average particle size of 10 mu m are added and uniformly stirred under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, and finally 0.2 part of vinyltrimethoxysilane, 0.1 part of methyltrimethoxysilane, 0.05 part of methylphenyldimethoxysilane, 1 part of coupling agent prepolymer and 1 part of KR-TTS are added and uniformly stirred under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, so that the single-component silane modified polyether heat conduction material is obtained.
The difference from example 2 is that graphene after the oxidative coating treatment was replaced with graphene without the oxidative coating treatment in equal amount.
Comparative example 2
Weighing 6 parts of 30000 mPas double-end siloxy modified polyether resin STP-E30, 12 parts of 3000 mPas single-end siloxy modified polyether diluent SAT145 and 2 parts of graphene after oxidation coating treatment at room temperature and humidity of less than 30RH%, uniformly mixing, adding 10 parts of spherical aluminum hydroxide with the average particle size of 2 mu m and 65 parts of spherical aluminum hydroxide with the average particle size of 10 mu m, uniformly stirring under the vacuum conditions of less than 35 ℃ and more than 0.09MPa, finally adding 1.5 parts of vinyltrimethoxysilane, 1.0 part of methyltrimethoxysilane, 1.5 parts of KH-550 and 1.0 part of KRTi-1, and uniformly stirring under the vacuum conditions of less than 35 ℃ and more than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
The difference from example 4 is that the coupling agent prepolymer was replaced with the coupling agent KH-550 in equal amounts.
Comparative example 3
Weighing 6 parts of 30000 mPas double-end siloxy modified polyether resin STP-E30, 12 parts of dioctyl phthalate and 2 parts of graphene subjected to oxidation coating treatment at room temperature and humidity of lower than 30RH%, uniformly mixing, adding 10 parts of spherical aluminum hydroxide with the average particle size of 2 mu m and 65 parts of spherical aluminum hydroxide with the average particle size of 10 mu m, uniformly stirring under vacuum conditions of lower than 35 ℃ and higher than 0.09MPa, finally adding 1.5 parts of vinyl trimethoxy silane, 1.0 part of methyl trimethoxy silane, 1.5 parts of coupling agent prepolymer and 1.0 part of KRTi-1, and uniformly stirring under vacuum conditions of lower than 35 ℃ and higher than 0.09MPa to obtain the single-component high-thermal-conductivity silane modified polyether composite material.
The difference from example 4 was that dioctyl phthalate was substituted for 3000 mPas of the single-terminal siloxy-modified polyether diluent SAT145 in equal amounts.
Testing
The examples 1 to 5 and comparative examples 1 to 3 were subjected to the test of mechanical properties and adhesive properties in accordance with the standard (GB/T528-2009) after curing for 7 days at 25 ℃ 50% RH at the same time. The high temperature aging test was carried out after the curing was completed by placing the sample in an oven at 110 ℃ for 7 days. The test results are shown in the following table:
from the test results it can be seen that: although aluminum hydroxide is adopted in the single-component high-thermal-conductivity silane modified polyether composite material, the thermal conductivity of the single-component high-thermal-conductivity silane modified polyether composite material is lower than that of aluminum oxide, and after graphene is compounded, the high-thermal-conductivity material of 2.0W/m.k can be prepared. Compared with the comparative example 1, the graphene subjected to oxidation coating treatment is adopted, so that the insulating property of the material can be effectively improved, and the heat conduction is basically not influenced; compared with the comparative example 2, the self-made coupling agent prepolymer is adopted, the epoxy group is opened in advance, the bonding effect on PPA is good, and the strength attenuation of the material is small after high-temperature aging, so that the high-temperature stability is better reflected; compared with the comparative example 3, the single-ended siloxy modified polyether diluent is adopted, and compared with a formula using a large amount of plasticizer, the bulk strength, the bonding property and the high-temperature reliability are obviously improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The single-component silane modified polyether heat conduction material is characterized by comprising the following components in parts by weight:
5-30 parts of double-terminal siloxy modified polyether resin, 0-15 parts of single-terminal siloxy modified polyether diluent, 50-90 parts of aluminum hydroxide, 0.5-5.0 parts of graphene, 0.05-3.0 parts of crosslinking agent, 0.05-2.0 parts of coupling agent prepolymer and 0.05-2.0 parts of catalyst;
the graphene is subjected to hydrogen peroxide oxidation treatment; carrying out silane surface modification by using hexamethyl silazane after graphene oxidation treatment; the graphene treatment process comprises the following steps: adding raw material graphene into a drum dryer, spraying hydrogen peroxide with the weight of 1-5 wt% of the raw material graphene, and uniformly dispersing in a rolling manner at room temperature; then, spraying hexamethyl silazane accounting for 0.5-10wt% of the weight of the raw material graphene, rolling and dispersing for 1 hour at room temperature, gradually heating to 100 ℃, and drying for later use;
the coupling agent prepolymer is a prepolymer of KH-560 and KH-540; the preparation method of the coupling agent prepolymer comprises the following steps: under the nitrogen atmosphere, mixing a mixture of 4: adding KH-560 and KH-540 of (2~5) into a reaction kettle, gradually heating to 100 ℃, keeping the temperature for reaction for 6 hours, cooling to room temperature, charging nitrogen gas for storage, and obtaining a coupling agent prepolymer;
the single-end siloxy modified polyether diluent is a polyether diluent of which one end of a molecular chain is blocked by trimethoxy silane and the other end is blocked by trimethyl silane; the viscosity range of the single-ended siloxy modified polyether diluent is 200-5000 mPa.s.
2. The one-component silane-modified polyether thermal conductive material of claim 1,
the double-end siloxy modified polyether resin is polyether resin with both ends of a molecular chain blocked by trimethoxy silane; the viscosity range of the double-end siloxy modified polyether resin is 500 to 30000mPa & s.
3. The single-component silane-modified polyether thermal conductive material of claim 1, wherein the aluminum hydroxide is spherical aluminum hydroxide with a particle size of 50 μm or less.
4. The single-component silane-modified polyether thermal conductive material of claim 1, wherein the cross-linking agent is one or more of methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, methyl orthosilicate, ethyl orthosilicate, phenyltrimethoxysilane, phenylvinyldimethoxysilane, and dimethyldimethoxysilane.
5. The single component silane modified polyether thermal conductive material of claim 1, wherein the catalyst is a titanate catalyst.
6. A method of making a monocomponent silane modified polyether thermal conductive material of any one of claims 1~5 comprising the steps of:
adding the double-end siloxy modified polyether resin, the single-end siloxy modified polyether diluent and the graphene into a stirring kettle in an environment with the humidity lower than 30RH%, uniformly mixing, adding aluminum hydroxide, uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa, finally adding the cross-linking agent, the coupling agent prepolymer and the catalyst, and uniformly stirring under the vacuum condition of lower than 35 ℃ and higher than 0.09MPa to obtain the single-component silane modified polyether heat conduction material.
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| CN109266282A (en) * | 2018-09-10 | 2019-01-25 | 广州博邦化学科技有限责任公司 | A kind of compound silane modified polyether heat-conducting glue of one-component and preparation method thereof |
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| CN109504333A (en) * | 2018-11-08 | 2019-03-22 | 佛山市真由美化工建材有限公司 | A kind of modified silane polyether seal glue and preparation method thereof |
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