CN106566199A - Epoxy heat conduction composite material and preparing method thereof - Google Patents
Epoxy heat conduction composite material and preparing method thereof Download PDFInfo
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- CN106566199A CN106566199A CN201610917345.2A CN201610917345A CN106566199A CN 106566199 A CN106566199 A CN 106566199A CN 201610917345 A CN201610917345 A CN 201610917345A CN 106566199 A CN106566199 A CN 106566199A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- 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
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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
- 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
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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
Abstract
The invention discloses an epoxy heat conduction composite material. The epoxy heat conduction composite material is composed of raw materials including, by weight, 0.3-1 part of diisopropyl cholamine, 10-13 parts of nanometer aluminium oxide, 1-2 parts of 3,5-diaminobenzoic acid, 0.3-0.7 parts of pyridine, 2-3 parts of triphenyl phosphate, 0.1-0.2 part of lithium chloride, 0.6-1 part of a silane coupling agent kh560, 0.7-1 part of acetylacetone neodymium, 1.6-2 parts of methyl hexahydrophthalic anhydride, 80-90 parts of epoxy resin6101, 0.1-0.2 part of trimethylolpropane, 0.4-1 part of stannous sulfide, 5-7 parts of 2-ethylhexyl acrylate, 3-4 parts of lauryl mercaptan, 0.4-1 part of diphenyl imidazoline, 3-4 parts of magnesium stearate and 0.3-1 part of polyglycerol-10 oleate. The composite material has the very good stability, and is long in storage time and excellent in comprehensive performance.
Description
Technical field
The present invention relates to Heat Conduction Material technical field, more particularly to a kind of epoxy heat-conductive composite material and preparation method thereof.
Background technology
Epoxy resin has excellent mechanical property, electrical property, adhesive property and thermally-stabilised, is widely used to aviation boat
My god, the field such as electric.Epoxy resin is various in style, and what this work was selected is cycloaliphatic epoxy resin, due to aliphatic ring
Epoxide group in oxygen resinous molecular structure is not from expoxy propane, and epoxy radicals is connected directly between on alicyclic ring, so alicyclic
Epoxy resin compared with bisphenol A type epoxy resin, with good heat endurance, excellent electrical insulation capability and weather resisteant,
Many advantages, such as high security.But the thermal conductivity factor of epoxy resin relatively low (0.23W/mK), heat dispersion is poor, is difficult to
Meet the fast development of microelectric technique and encapsulation technology.Therefore, the research about the heat conductivility of epoxy resin has become electricity
The focus that the subject such as son and material is paid close attention to jointly；
Improving the approach of the thermal conductivity factor of polymer mainly has two kinds of Intrinsical and filled-type.Former approach difficulty is big, cost compared with
Height, studies less.The latter's method is simple, is widely used.At present, relevant filled-type thermally conductive epoxy resin composite wood
The research of material is much reported.In heat filling, nano aluminium oxide has higher thermal conductivity factor (30W/mK), excellent
Heat endurance and resistance to chemical corrosion, good electrical insulating property, and cheap and wide material sources and be used widely.But
It is, because nano oxidized aluminium particle size is little, surface energy is high, in thermodynamics unsteady state, easily to assemble agglomerating, so as to have impact on
The practical application effect of nano alumina particles.So must nano alumina particles be carried out with surface be modified, to reduce surface
Can, reduce the agglomeration power between nano particle, its dispersiveness and dispersion stabilization in the base is improved, reduce two-phase interface
Power, the wetability, adhesion and compatibility between raising nano alumina particles and matrix resin, so as to improve composite
Combination property.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of epoxy heat-conductive composite material and its preparation
Method.
The present invention is achieved by the following technical solutions：
A kind of epoxy heat-conductive composite material, it is made up of the raw material of following weight parts：
Diisopropyl ethanolamine 0.3-1, nano aluminium oxide 10-13,3,5- diaminobenzoic acid 1-2, pyridine 0.3-0.7, phosphorous
Triphenyl phosphate ester 2-3, lithium chloride 0.1-0.2, silane coupler kh5600.6-1, acetylacetone,2,4-pentanedione neodymium 0.7-1, methyl hexahydro neighbour's benzene two
Formic anhydride 1.6-2, epoxy resin 6101 80-90, trimethylolpropane 0.1-0.2, stannous sulfide 0.4-1, Isooctyl acrylate monomer
5-7, lauryl mercaptan 3-4, diphenyl-imidazole quinoline 0.4-1, magnesium stearate 3-4, Natrulon H-10 oleate 0.3-1.
A kind of preparation method of described epoxy heat-conductive composite material, comprises the following steps：
（1）Above-mentioned nano aluminium oxide, silane coupler kh560 are mixed, the absolute ethyl alcohol of compound weight 4-6 times is added to
In, in sending into 110-120 DEG C of oil bath, insulated and stirred 3-5 hour, discharging is filtered, and will be deposited in 120-130 DEG C of baking oven true
Sky is dried 1-2 hours, obtains silane oxidation aluminium；
（2）Above-mentioned lauryl mercaptan is added in 70-76 DEG C of water-bath, above-mentioned trimethylolpropane, insulated and stirred is added
20-30 minutes, discharging mixes with above-mentioned epoxy resin 6101, stirs to normal temperature, obtains modified epoxy solution；
（3）Above-mentioned lithium chloride is added in the methyl alcohol of its weight 900-1000 times, above-mentioned diphenyl-imidazole quinoline is added, in 57-
Insulated and stirred 20-30 minute at 60 DEG C, obtain methyl alcohol dispersion liquid；
（4）Above-mentioned stannous sulfide is added in the 1-METHYLPYRROLIDONE of its weight 4-7 times, it is 65-70 DEG C to rise high-temperature, is protected
Temperature stirring 10-20 minutes, above-mentioned magnesium stearate is added, stirred to normal temperature, obtain alkanone dispersion liquid；
（5）Above-mentioned silane oxidation aluminium is added in the 1-METHYLPYRROLIDONE of its weight 47-60 times, is stirred, added successively
Enter above-mentioned 3,5- diaminobenzoic acids, pyridine, triphenyl phosphite, be passed through nitrogen, above-mentioned alkanone dispersion liquid is added, in 98-100
Reaction 3-4 hours, are cooled to normal temperature at DEG C, in being added to above-mentioned methyl alcohol dispersion liquid, stand 3-4 hours, filter, and will precipitate to use and divide
Do not rinsed 3-4 time successively with DMF and methyl alcohol, mixed with above-mentioned magnesium stearate, be placed in 87-90 DEG C of baking oven
In, 1-2 hours are vacuum dried, obtain grafting aluminum oxide；
（6）Above-mentioned acetylacetone,2,4-pentanedione neodymium is added in modified epoxy solution, 30-40 minutes, vacuum are stirred at 80-86 DEG C
Degassing, is cooled to room temperature, obtains epoxy solution；
（7）Above-mentioned grafting aluminum oxide is taken, in being added to the acetone of its weight 4-6 times, is stirred, add above-mentioned epoxy solution,
Ultrasonic 20-30 minutes, in being sent to 68-70 DEG C of constant temperature oil bath, 10-12 hours are incubated, add above-mentioned methyl hexahydro neighbour benzene two
Formic anhydride, stirs, vacuum outgas 30-40 minutes, mixes with remaining each raw material, first preheats 100-120 at 130-140 DEG C
Minute, it is 160-170 DEG C to rise high-temperature, solidifies 10-15 hours, is cooled to room temperature, obtains heat-conductive composite material.
It is an advantage of the invention that：Hyperbranched Aromatic Polyamides are grafted to nano alumina particles table by the present invention using two-step method
Face:Nano particle carries out first silane coupler and processes grafting over-expense on introducing amino group, then nano-particle after modification
Fluidized polymer；
Jing after coupling processing, particle is transformed into hydrophobicity to aluminum oxide nanoparticle by hydrophily, so can significantly improve and epoxy
The compatibility of resin.During the silane coupled process of also aluminum oxide nanoparticle Jing, silane coupler one end and aluminium oxide nano
Particle is combined with chemical bond, and other end of amido functional group occurs chemical reaction with epoxy resin, enhances epoxy resin
The combination of matrix and nano particle boundary, reduces interface void and defect, so as to be conducive to the raising of thermal conductivity factor；
Secondly as the skin effect of nano-particle, silane oxidation aluminum nanoparticles are with very big specific surface area, Er Qiejing
Nano-particle after silane treatment can be preferably distributed in epoxy resin-base, at this moment silane oxidation aluminum nanoparticles and epoxy
The chemical bond that chemical reaction between resin is formed just serves more and more important effect.One nano particle can be used as three
A heat conduction node in dimension network, increasing for this heat conduction node not only reduce further interface resistance, but also be formed
The bridged bond of polymer network, therefore it is effectively improved the thermal conductivity factor of epoxy resin/silane oxidation aluminium composite material；
Due to the alumina nanoparticles good dispersion in the epoxy and compatibility of grafted by super branched polymer;Its
The secondary alumina nanoparticles surface due to Hyperbranched Aromatic Polyamides grafting has more ammonia than silane oxidation aluminum nanoparticles
Base functional group, can form more chemical bonds, thermal conductivity of this heat conduction node in composite between epoxy resin-base
In serve leading role;Last point is that itself is excellent compared with epoxy resin because Nomex is rigid main chain
Heat conductivility can play more preferable conduction of heat in the transmittance process of hot-fluid.
The composite of the present invention has good stability, and period of storage is long, and combination property is superior.
Specific embodiment
A kind of epoxy heat-conductive composite material, it is made up of the raw material of following weight parts：
Diisopropyl ethanolamine 0.3, the diaminobenzoic acid 1 of nano aluminium oxide 10,3,5, pyridine 0.3, triphenyl phosphite 2, chlorine
Change lithium 0.1, silane coupler kh5600.6, acetylacetone,2,4-pentanedione neodymium 0.7, methylhexahydrophthalic anhydride 1.6, epoxy resin
610180th, trimethylolpropane 0.1, stannous sulfide 0.4, Isooctyl acrylate monomer 5, lauryl mercaptan 3, diphenyl-imidazole quinoline
0.4th, magnesium stearate 3, Unigly GO 102S 0.3.
A kind of preparation method of described epoxy heat-conductive composite material, comprises the following steps：
（1）Above-mentioned nano aluminium oxide, silane coupler kh560 are mixed, in being added to the absolute ethyl alcohol of 4 times of compound weight,
In sending into 110 DEG C of oil bath, insulated and stirred 3 hours, discharging is filtered, and will be deposited in 120 DEG C of baking oven and is vacuum dried 1 hour,
Obtain silane oxidation aluminium；
（2）Above-mentioned lauryl mercaptan is added in 70 DEG C of water-bath, above-mentioned trimethylolpropane, 20 points of insulated and stirred is added
Clock, discharging, mixes with above-mentioned epoxy resin 6101, stirs to normal temperature, obtains modified epoxy solution；
（3）Above-mentioned lithium chloride is added in the methyl alcohol of 900 times of its weight, above-mentioned diphenyl-imidazole quinoline is added, is protected at 57 DEG C
Temperature stirring 20 minutes, obtains methyl alcohol dispersion liquid；
（4）Above-mentioned stannous sulfide is added in the N methyl pyrrolidones of 4 times of its weight, it is 65 DEG C to rise high-temperature, insulated and stirred
10 minutes, above-mentioned magnesium stearate is added, stirred to normal temperature, obtain alkanone dispersion liquid；
（5）Above-mentioned silane oxidation aluminium is added in the N methyl pyrrolidones of 47 times of its weight, is stirred, sequentially added
3,5 diaminobenzoic acids, pyridine, triphenyl phosphite are stated, nitrogen is passed through, above-mentioned alkanone dispersion liquid is added, at 98 DEG C 3 are reacted
Hour, normal temperature is cooled to, in being added to above-mentioned methyl alcohol dispersion liquid, 3 hours are stood, filter, precipitation is used and use respectively N, N dimethyl
Formamide and methyl alcohol are rinsed successively 3 times, are mixed with above-mentioned magnesium stearate, in being placed in 87 DEG C of baking oven, are vacuum dried 1 hour, are obtained
Grafting aluminum oxide；
（6）Above-mentioned acetylacetone,2,4-pentanedione neodymium is added in modified epoxy solution, is stirred 30 minutes at 80 DEG C, vacuum outgas,
Room temperature is cooled to, epoxy solution is obtained；
（7）Above-mentioned grafting aluminum oxide is taken, in being added to the acetone of 4 times of its weight, is stirred, add above-mentioned epoxy solution, surpassed
Sound 20 minutes, in being sent to 68 DEG C of constant temperature oil bath, is incubated 10 hours, adds above-mentioned methylhexahydrophthalic anhydride, stirring
Uniformly, vacuum outgas 30 minutes, mix with remaining each raw material, first preheat 100 minutes at 130 DEG C, and it is 160 DEG C to rise high-temperature,
Solidification 10 hours, is cooled to room temperature, obtains heat-conductive composite material.
The thermal conductivity factor of material of the present invention is 0.347W/mK.
Claims (2)
1. a kind of epoxy heat-conductive composite material, it is characterised in that it is made up of the raw material of following weight parts：
Diisopropyl ethanolamine 0.3-1, nano aluminium oxide 10-13,3,5- diaminobenzoic acid 1-2, pyridine 0.3-0.7, phosphorous
Triphenyl phosphate ester 2-3, lithium chloride 0.1-0.2, silane coupler kh5600.6-1, acetylacetone,2,4-pentanedione neodymium 0.7-1, methyl hexahydro neighbour's benzene two
Formic anhydride 1.6-2, epoxy resin 6101 80-90, trimethylolpropane 0.1-0.2, stannous sulfide 0.4-1, Isooctyl acrylate monomer
5-7, lauryl mercaptan 3-4, diphenyl-imidazole quinoline 0.4-1, magnesium stearate 3-4, Natrulon H-10 oleate 0.3-1.
2. a kind of preparation method of epoxy heat-conductive composite material as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Above-mentioned nano aluminium oxide, silane coupler kh560 are mixed, the absolute ethyl alcohol of compound weight 4-6 times is added to
In, in sending into 110-120 DEG C of oil bath, insulated and stirred 3-5 hour, discharging is filtered, and will be deposited in 120-130 DEG C of baking oven true
Sky is dried 1-2 hours, obtains silane oxidation aluminium；
（2）Above-mentioned lauryl mercaptan is added in 70-76 DEG C of water-bath, above-mentioned trimethylolpropane, insulated and stirred is added
20-30 minutes, discharging mixes with above-mentioned epoxy resin 6101, stirs to normal temperature, obtains modified epoxy solution；
（3）Above-mentioned lithium chloride is added in the methyl alcohol of its weight 900-1000 times, above-mentioned diphenyl-imidazole quinoline is added, in 57-
Insulated and stirred 20-30 minute at 60 DEG C, obtain methyl alcohol dispersion liquid；
（4）Above-mentioned stannous sulfide is added in the 1-METHYLPYRROLIDONE of its weight 4-7 times, it is 65-70 DEG C to rise high-temperature, is protected
Temperature stirring 10-20 minutes, above-mentioned magnesium stearate is added, stirred to normal temperature, obtain alkanone dispersion liquid；
（5）Above-mentioned silane oxidation aluminium is added in the 1-METHYLPYRROLIDONE of its weight 47-60 times, is stirred, added successively
Enter above-mentioned 3,5- diaminobenzoic acids, pyridine, triphenyl phosphite, be passed through nitrogen, above-mentioned alkanone dispersion liquid is added, in 98-100
Reaction 3-4 hours, are cooled to normal temperature at DEG C, in being added to above-mentioned methyl alcohol dispersion liquid, stand 3-4 hours, filter, and will precipitate to use and divide
Do not rinsed 3-4 time successively with DMF and methyl alcohol, mixed with above-mentioned magnesium stearate, be placed in 87-90 DEG C of baking oven
In, 1-2 hours are vacuum dried, obtain grafting aluminum oxide；
（6）Above-mentioned acetylacetone,2,4-pentanedione neodymium is added in modified epoxy solution, 30-40 minutes, vacuum are stirred at 80-86 DEG C
Degassing, is cooled to room temperature, obtains epoxy solution；
（7）Above-mentioned grafting aluminum oxide is taken, in being added to the acetone of its weight 4-6 times, is stirred, add above-mentioned epoxy solution,
Ultrasonic 20-30 minutes, in being sent to 68-70 DEG C of constant temperature oil bath, 10-12 hours are incubated, add above-mentioned methyl hexahydro neighbour benzene two
Formic anhydride, stirs, vacuum outgas 30-40 minutes, mixes with remaining each raw material, first preheats 100-120 at 130-140 DEG C
Minute, it is 160-170 DEG C to rise high-temperature, solidifies 10-15 hours, is cooled to room temperature, obtains heat-conductive composite material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610917345.2A CN106566199A (en) | 2016-10-21 | 2016-10-21 | Epoxy heat conduction composite material and preparing method thereof |
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| CN201610917345.2A CN106566199A (en) | 2016-10-21 | 2016-10-21 | Epoxy heat conduction composite material and preparing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177169A (en) * | 2017-06-29 | 2017-09-19 | 倪群 | A kind of rich phosphaization grafting flame retardant epoxy material and preparation method thereof |
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|---|---|---|---|---|
| CN1282105A (en) * | 2000-08-25 | 2001-01-31 | 中国科学院化学研究所 | Liquid epoxy composite for packaging semiconductor and its application |
| CN103555140A (en) * | 2013-10-28 | 2014-02-05 | 安徽明都电气有限公司 | High-extinction air-permeable powder paint |
| CN104927232A (en) * | 2015-06-04 | 2015-09-23 | 当涂县华艺金属制品有限公司 | Plasticizing fiber modified plastic door and window |
| CN105754297A (en) * | 2016-05-06 | 2016-07-13 | 陈昌 | Heat-conducting electronic packaging composite and preparation method thereof |
| CN105949695A (en) * | 2015-03-09 | 2016-09-21 | 旭化成株式会社 | Methacrylic resin composition, method for producing the same, and molded article |
-
2016
- 2016-10-21 CN CN201610917345.2A patent/CN106566199A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1282105A (en) * | 2000-08-25 | 2001-01-31 | 中国科学院化学研究所 | Liquid epoxy composite for packaging semiconductor and its application |
| CN103555140A (en) * | 2013-10-28 | 2014-02-05 | 安徽明都电气有限公司 | High-extinction air-permeable powder paint |
| CN105949695A (en) * | 2015-03-09 | 2016-09-21 | 旭化成株式会社 | Methacrylic resin composition, method for producing the same, and molded article |
| CN104927232A (en) * | 2015-06-04 | 2015-09-23 | 当涂县华艺金属制品有限公司 | Plasticizing fiber modified plastic door and window |
| CN105754297A (en) * | 2016-05-06 | 2016-07-13 | 陈昌 | Heat-conducting electronic packaging composite and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107177169A (en) * | 2017-06-29 | 2017-09-19 | 倪群 | A kind of rich phosphaization grafting flame retardant epoxy material and preparation method thereof |
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Application publication date: 20170419 |