CN105733196A - Heat conduction type composite material and preparation method thereof - Google Patents
Heat conduction type composite material and preparation method thereof Download PDFInfo
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- CN105733196A CN105733196A CN201610295247.XA CN201610295247A CN105733196A CN 105733196 A CN105733196 A CN 105733196A CN 201610295247 A CN201610295247 A CN 201610295247A CN 105733196 A CN105733196 A CN 105733196A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- 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
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- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- 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
Abstract
The invention relates to a heat conduction type composite material and a preparation method thereof. The preparation method comprises the following steps: (1) mixing diamond powder, nano titanium dioxide and absolute ethyl alcohol, and performing ultrasonic stirring by using ultrasound equipment; (2) adding 3-aminopropyl triethoxy silane and gamma-(2,3-epoxypropyloxy) propyl trimethoxy silane, and leaving to stand at the room temperature after reflux; (3) filtering, and drying in a drying oven; (4) taking out, crushing by using a mortar, and screening; (5) performing oil bath treatment on bisphenol A epoxy resin, adding residual components, and stirring by using a high-speed stirring machine; (6) adding treated diamond powder and nano titanium dioxide, heating to 180-190 DEG C, and further uniformly stirring; (7) putting into a baking oven, defoaming, pouring into a mold, and curing, thereby obtaining the heat conduction type composite material. The prepared heat conduction type composite material is excellent in heat conduction property, relatively high in glass-transition temperature, high in use temperature upper limit, relatively good in thermal resistance and relatively good in mechanical property as well.
Description
Technical field
The invention belongs to Material Field, relate to a kind of heat-conducting type composite and preparation method thereof.
Background technology
In recent years, along with China's economy and the high speed development of science and technology, the kind of material gets more and more, and performance is more and more multiple
Miscellaneous, wherein, the application of Heat Conduction Material is more and more extensive, is primarily used to electron trade and heat exchange heating industry etc..And along with meter
Calculation machine becomes people's Working Life and entertains a requisite part, and its performance is also required to improve further, wherein, by
The high heat production caused in high energy consumption is the most increasingly taken seriously.People are general using metal material as Heat Conduction Material, but metal
Material has the most corrosion-resistant, non-oxidizability difference and high in cost of production shortcoming, although have researcher to have studied the sides such as corrosion resistance coating
Method improves its performance, but coating also reduces the heat conductivity of material.Therefore, a kind of heat conductivity with brilliance is researched and developed
Can, there is again preferable mechanical property, easy machine-shaping and the material of the advantage such as with low cost simultaneously, be trend of the times, have
Important realistic meaning and wide market prospect.
Summary of the invention
Solve the technical problem that: it is an object of the invention to disclose a kind of novel heat-conducting type composite and preparation side thereof
Method, this material has the heat conductivility of brilliance, and glass transition temperature is higher simultaneously, uses temperature upper limit high, and heat resistance is relatively
Good, there is preferable mechanical property simultaneously.
Technical scheme: the invention discloses a kind of heat-conducting type composite, following component be prepared from weight portion:
Bortz powder 20-30 part,
Nano titanium oxide 1-2 part,
Carboxyl end of the liquid acrylonitrile-butadiene rubber 1-3 part,
Bisphenol A type epoxy resin 40-55 part,
Ergocalciferol 0.1-0.2 part,
3,4-4-dihydroxy benzaldehyde 1-2 part,
DADPS 3-5 part,
N-aminoethyl piperazine 7-10 part,
3-aminopropyl triethoxysilane 1-2 part,
γ-(2,3-glycidoxy) propyl trimethoxy silicane 1-3 part,
Tissuemat E 0.1-0.3 part,
Dioctyl phthalate 2-4 part,
BBP(Butyl Benzyl Phthalate 1-3 part,
Dehydrated alcohol 20-40 part,
Absolute methanol 8-15 part.
Further, described a kind of heat-conducting type composite, following component it is prepared from weight portion:
Bortz powder 22-28 part,
Nano titanium oxide 1.2-1.7 part,
Carboxyl end of the liquid acrylonitrile-butadiene rubber 1.5-2.5 part,
Bisphenol A type epoxy resin 45-50 part,
Ergocalciferol 0.13-0.18 part,
3,4-4-dihydroxy benzaldehyde 1.3-1.8 part,
DADPS 3.5-4.5 part,
N-aminoethyl piperazine 8-9 part,
3-aminopropyl triethoxysilane 1.2-1.8 part,
γ-(2,3-glycidoxy) propyl trimethoxy silicane 1.5-2.5 part,
Tissuemat E 0.15-0.25 part,
Dioctyl phthalate 2.5-3.5 part,
BBP(Butyl Benzyl Phthalate 1.5-2.5 part,
Dehydrated alcohol 25-35 part,
Absolute methanol 9-14 part.
The preparation method of described a kind of heat-conducting type composite, comprises the steps:
(1) bortz powder, nano titanium oxide and dehydrated alcohol are mixed, by Ultrasound Instrument ultrasonic agitation 10-30 minute；
(2) 3-aminopropyl triethoxysilane and γ-(2,3-glycidoxy) propyl trimethoxy silicane are added, at 80-90
12 hours are at room temperature stood after refluxing 3-4 hour at DEG C；
(3) filter, be placed in baking oven, be dried 23-25 hour at temperature 90-100 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin carrying out at 160-170 DEG C oil bath, add remaining ingredient, homogenizer is at rotating speed
Stir 5-10 minute under 2000-4000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 180-190 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 175-185 DEG C, solidify 2-3 hour at 180-190 DEG C
Obtain.
Further, the preparation method of described a kind of heat-conducting type composite, in described step (1), mixing time is
15-25 minute.
Further, the preparation method of described a kind of heat-conducting type composite, in described step (2), reflux temperature is
85 DEG C, return time is 3.5 hours.
Further, the preparation method of described a kind of heat-conducting type composite, in described step (3), baking temperature is
95 DEG C, drying time is 23.5-24.5 hour.
Further, the preparation method of described a kind of heat-conducting type composite, in described step (5), oil bath temperature is
165 DEG C, speed of agitator is 2500-3500r/min, and mixing time is 6-9 minute.
Further, the preparation method of described a kind of heat-conducting type composite, described step (6) is warming up to 185
℃。
Further, the preparation method of described a kind of heat-conducting type composite, in described step (7), deaeration temperature is
180 DEG C, solidification temperature is 185 DEG C, and hardening time is 2.5 hours.
Beneficial effect: the glass transition temperature of heat-conducting type composite prepared by the method for the present invention is higher, the highest can
Reaching 210 DEG C, glass transition temperature is used to weigh the use temperature range of macromolecular material, and transition temperature is the highest, uses temperature
The degree upper limit is the highest.Heat resistance is preferable, 5% thermal weight loss temperature up to 379.1 DEG C, simultaneously hot strength the highest also up to
45.6MPa, has preferable mechanical property.On heat conductivility, its heat conductivity reaches as high as 2.25W/ (m K), heat conductivity
Can be remarkable.
Detailed description of the invention
Embodiment 1
(1) by bortz powder 20 parts, nano titanium oxide 1 part and dehydrated alcohol 20 parts mixing, by Ultrasound Instrument ultrasonic agitation 10 points
Clock；
(2) 3-aminopropyl triethoxysilane 1 part and γ-(2,3-glycidoxy) propyl trimethoxy silicane 1 part are added,
12 hours are at room temperature stood after refluxing 3 hours at 80 DEG C；
(3) filter, be placed in baking oven, be dried 23 hours at temperature 90 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 40 parts is carried out at 160 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 1 part, Ergota
Calciferol 0.1 part, 3,4-4-dihydroxy benzaldehyde 1 part, DADPS 3 parts, N-aminoethyl piperazine 7 parts, Tissuemat E 0.1
Part, dioctyl phthalate 2 parts, BBP(Butyl Benzyl Phthalate 1 part, absolute methanol 8 parts, homogenizer is at rotating speed 2000r/
Stir 5 minutes under min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 180 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 175 DEG C, solidify 2 hours at 180 DEG C and get final product.
Embodiment 2
(1) by bortz powder 22 parts, nano titanium oxide 1.2 parts and dehydrated alcohol 25 parts mixing, by Ultrasound Instrument ultrasonic agitation 15
Minute；
(2) 3-aminopropyl triethoxysilane 1.2 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 1.5 are added
Part, at room temperature stand 12 hours after refluxing 3.5 hours at 85 DEG C；
(3) filter, be placed in baking oven, be dried 23.5 hours at temperature 95 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 45 parts is carried out at 165 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 1.5 parts, wheat
Angle calciferol 0.13 part, 3,4-4-dihydroxy benzaldehyde 1.3 parts, DADPS 3.5 parts, N-aminoethyl piperazine 8 parts, polyethylene
0.15 part of wax, dioctyl phthalate 2.5 parts, BBP(Butyl Benzyl Phthalate 1.5 parts, absolute methanol 9 parts, homogenizer exists
Stir 6 minutes under rotating speed 2500r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 185 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 180 DEG C, solidify 2.5 hours at 185 DEG C and get final product.
Embodiment 3
(1) by bortz powder 25 parts, nano titanium oxide 1.5 parts and dehydrated alcohol 30 parts mixing, by Ultrasound Instrument ultrasonic agitation 20
Minute；
(2) 3-aminopropyl triethoxysilane 1.5 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 2 are added
Part, at room temperature stand 12 hours after refluxing 3.5 hours at 85 DEG C；
(3) filter, be placed in baking oven, be dried 24 hours at temperature 95 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 47 parts is carried out at 165 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 2 parts, Ergota
Calciferol 0.15 part, 3,4-4-dihydroxy benzaldehyde 1.5 parts, DADPS 4 parts, N-aminoethyl piperazine 8.5 parts, Tissuemat E
0.2 part, dioctyl phthalate 3 parts, BBP(Butyl Benzyl Phthalate 2 parts, absolute methanol 11.5 parts, homogenizer is at rotating speed
Stir 7 minutes under 3000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 185 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 180 DEG C, solidify 2.5 hours at 185 DEG C and get final product.
Embodiment 4
(1) by bortz powder 28 parts, nano titanium oxide 1.7 parts and dehydrated alcohol 35 parts mixing, by Ultrasound Instrument ultrasonic agitation 25
Minute；
(2) 3-aminopropyl triethoxysilane 1.8 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 2.5 are added
Part, at room temperature stand 12 hours after refluxing 3.5 hours at 85 DEG C；
(3) filter, be placed in baking oven, be dried 24.5 hours at temperature 95 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 50 parts is carried out at 165 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 2.5 parts, wheat
Angle calciferol 0.18 part, 3,4-4-dihydroxy benzaldehyde 1.8 parts, DADPS 4.5 parts, N-aminoethyl piperazine 9 parts, polyethylene
0.25 part of wax, dioctyl phthalate 3.5 parts, BBP(Butyl Benzyl Phthalate 2.5 parts, absolute methanol 14 parts, homogenizer
Stir 9 minutes under rotating speed 3500r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 185 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 180 DEG C, solidify 2.5 hours at 185 DEG C and get final product.
Further, the preparation method of described a kind of heat-conducting type composite, in described step (5), oil bath temperature is
165 DEG C, speed of agitator is 2500-3500r/min, and mixing time is 6-9 minute.
Embodiment 5
(1) by bortz powder 30 parts, nano titanium oxide 2 parts and dehydrated alcohol 40 parts mixing, by Ultrasound Instrument ultrasonic agitation 30 points
Clock；
(2) 3-aminopropyl triethoxysilane 2 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 3 parts are added,
12 hours are at room temperature stood after refluxing 4 hours at 90 DEG C；
(3) filter, be placed in baking oven, be dried 25 hours at temperature 100 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 55 parts is carried out at 170 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 3 parts, Ergota
Calciferol 0.2 part, 3,4-4-dihydroxy benzaldehyde 2 parts, DADPS 5 parts, N-aminoethyl piperazine 10 parts, Tissuemat E 0.3
Part, dioctyl phthalate 4 parts, BBP(Butyl Benzyl Phthalate 3 parts, absolute methanol 15 parts, homogenizer is at rotating speed
Stir 10 minutes under 4000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 190 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 185 DEG C, solidify 3 hours at 190 DEG C and get final product.
Comparative example 1
(1) by bortz powder 30 parts and dehydrated alcohol 40 parts mixing, by Ultrasound Instrument ultrasonic agitation 30 minutes；
(2) 3-aminopropyl triethoxysilane 2 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 3 parts are added,
12 hours are at room temperature stood after refluxing 4 hours at 90 DEG C；
(3) filter, be placed in baking oven, be dried 25 hours at temperature 100 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 55 parts is carried out at 170 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 3 parts, Ergota
Calciferol 0.2 part, DADPS 5 parts, N-aminoethyl piperazine 10 parts, Tissuemat E 0.3 part, dioctyl phthalate 4
Part, BBP(Butyl Benzyl Phthalate 3 parts, absolute methanol 15 parts, homogenizer stirs 10 minutes under rotating speed 4000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 190 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 185 DEG C, solidify 3 hours at 190 DEG C and get final product.
Comparative example 2
(1) by bortz powder 30 parts, nano titanium oxide 2 parts and dehydrated alcohol 40 parts mixing, by Ultrasound Instrument ultrasonic agitation 30 points
Clock；
(2) 3-aminopropyl triethoxysilane 2 parts and γ-(2,3-glycidoxy) propyl trimethoxy silicane 3 parts are added,
12 hours are at room temperature stood after refluxing 4 hours at 90 DEG C；
(3) filter, be placed in baking oven, be dried 25 hours at temperature 100 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin 55 parts is carried out at 170 DEG C oil bath, add carboxyl end of the liquid acrylonitrile-butadiene rubber 3 parts, Ergota
Calciferol 0.2 part, 3,4-4-dihydroxy benzaldehyde 2 parts, N-aminoethyl piperazine 15 parts, Tissuemat E 0.3 part, phthalic acid two are pungent
Ester 4 parts, BBP(Butyl Benzyl Phthalate 3 parts, absolute methanol 15 parts, homogenizer stirs 10 minutes under rotating speed 4000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 190 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 185 DEG C, solidify 3 hours at 190 DEG C and get final product.
The performance of heat-conducting type composite prepared by the present invention is as follows, and its glass transition temperature is higher, reaches as high as 210
DEG C, glass transition temperature is used to weigh the use temperature range of macromolecular material, and transition temperature is the highest, uses temperature upper limit
The highest.Heat resistance is preferable, and 5% thermal weight loss temperature is up to 379.1 DEG C, and hot strength is the highest also up to 45.6MPa simultaneously, has
Preferably mechanical property.On heat conductivility, its heat conductivity reaches as high as 2.25W/ (m K), and heat conductivility is remarkable.
The performance of embodiment and comparative example is as follows:
| Glass transition temperature (DEG C) | 5% thermal weight loss temperature (DEG C) | Hot strength (MPa) | Heat conductivity (W/ (m K)) | |
| Embodiment 1 | 208 | 378.5 | 45.3 | 2.21 |
| Embodiment 2 | 209 | 378.6 | 45.4 | 2.22 |
| Embodiment 3 | 209 | 378.8 | 45.5 | 2.24 |
| Embodiment 4 | 210 | 379.1 | 45.6 | 2.25 |
| Embodiment 5 | 209 | 378.9 | 45.5 | 2.24 |
| Comparative example 1 | 202 | 373.5 | 45.5 | 2.01 |
| Comparative example 2 | 209 | 378.3 | 42.1 | 2.23 |
Claims (10)
1. a heat-conducting type composite, it is characterised in that described composite is prepared from weight portion by following component:
Bortz powder 20-30 part,
Nano titanium oxide 1-2 part,
Carboxyl end of the liquid acrylonitrile-butadiene rubber 1-3 part,
Bisphenol A type epoxy resin 40-55 part,
Ergocalciferol 0.1-0.2 part,
3,4-4-dihydroxy benzaldehyde 1-2 part,
DADPS 3-5 part,
N-aminoethyl piperazine 7-10 part,
3-aminopropyl triethoxysilane 1-2 part,
γ-(2,3-glycidoxy) propyl trimethoxy silicane 1-3 part,
Tissuemat E 0.1-0.3 part,
Dioctyl phthalate 2-4 part,
BBP(Butyl Benzyl Phthalate 1-3 part,
Dehydrated alcohol 20-40 part,
Absolute methanol 8-15 part.
A kind of heat-conducting type composite the most according to claim 1, it is characterised in that described composite is by following one-tenth
Divide and be prepared from weight portion:
Bortz powder 22-28 part,
Nano titanium oxide 1.2-1.7 part,
Carboxyl end of the liquid acrylonitrile-butadiene rubber 1.5-2.5 part,
Bisphenol A type epoxy resin 45-50 part,
Ergocalciferol 0.13-0.18 part,
3,4-4-dihydroxy benzaldehyde 1.3-1.8 part,
DADPS 3.5-4.5 part,
N-aminoethyl piperazine 8-9 part,
3-aminopropyl triethoxysilane 1.2-1.8 part,
γ-(2,3-glycidoxy) propyl trimethoxy silicane 1.5-2.5 part,
Tissuemat E 0.15-0.25 part,
Dioctyl phthalate 2.5-3.5 part,
BBP(Butyl Benzyl Phthalate 1.5-2.5 part,
Dehydrated alcohol 25-35 part,
Absolute methanol 9-14 part.
3. a kind of heat-conducting type composite as claimed in claim 1, it is characterised in that: described bortz powder particle diameter is 10-30 μ
m。
The preparation method of a kind of heat-conducting type composite the most according to claim 1, it is characterised in that described preparation side
Method comprises the steps:
(1) bortz powder, nano titanium oxide and dehydrated alcohol are mixed, by Ultrasound Instrument ultrasonic agitation 10-30 minute；
(2) 3-aminopropyl triethoxysilane and γ-(2,3-glycidoxy) propyl trimethoxy silicane are added, at 80-90
12 hours are at room temperature stood after refluxing 3-4 hour at DEG C；
(3) filter, be placed in baking oven, be dried 23-25 hour at temperature 90-100 DEG C；
(4) take out, grind with mortar and sieve；
(5) bisphenol A type epoxy resin carrying out at 160-170 DEG C oil bath, add remaining ingredient, homogenizer is at rotating speed
Stir 5-10 minute under 2000-4000r/min；
(6) add the bortz powder handled well and nano titanium oxide, be warming up to 180-190 DEG C, continue to be stirred until homogeneous；
(7) put in baking oven, pour in mould after deaeration at temperature 175-185 DEG C, solidify 2-3 hour at 180-190 DEG C
Obtain.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(1) in, mixing time is 15-25 minute.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(2) in, reflux temperature is 85 DEG C, and return time is 3.5 hours.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(3) in, baking temperature is 95 DEG C, and drying time is 23.5-24.5 hour.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(5) in, oil bath temperature is 165 DEG C, and speed of agitator is 2500-3500r/min, and mixing time is 6-9 minute.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(6) 185 DEG C it are warming up in.
The preparation method of a kind of heat-conducting type composite the most according to claim 4, it is characterised in that described step
(7) in, deaeration temperature is 180 DEG C, and solidification temperature is 185 DEG C, and hardening time is 2.5 hours.
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| CN105385106A (en) * | 2015-12-02 | 2016-03-09 | 安捷利（番禺）电子实业有限公司 | Preparation method for high-conductivity insulating composite material |
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