CN106280279A - A kind of preparation method of high heat conduction epoxy molding plastic - Google Patents
A kind of preparation method of high heat conduction epoxy molding plastic Download PDFInfo
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- CN106280279A CN106280279A CN201610650828.0A CN201610650828A CN106280279A CN 106280279 A CN106280279 A CN 106280279A CN 201610650828 A CN201610650828 A CN 201610650828A CN 106280279 A CN106280279 A CN 106280279A
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K3/34—Silicon-containing 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
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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
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
Abstract
The invention discloses the preparation method of a kind of high heat conduction epoxy molding plastic, belong to microelectronic packaging technology field.Serpentine is activated by the present invention by calcining, acidleach carries out remove impurity, again with methanol, after the mixing such as dicyclopentadiene, be placed in reactor carry out laser irradiate react, to its modifying surface, increase high hot, last and o-cresol formaldehyde epoxy resin, white carbon black, the ball milling mixing such as triethylene tetramine, extruding pelletization i.e. obtains high heat conduction epoxy molding plastic, the present invention is with serpentine as raw material, by being modified being fabricated to filler to it, thus it is the highest to compensate for tradition moulding compound heat conductivility, cause its defect that thermal shock resistance is the best under the high temperature conditions, there is prospect of production widely.
Description
Technical field
The invention discloses the preparation method of a kind of high heat conduction epoxy molding plastic, belong to microelectronic packaging technology field.
Background technology
Epoxy resin is the high molecular polymer of the epoxide group in molecule containing two or more, epoxy resin
Relative molecular mass typically the highest, about 300~8000, be solid-state or liquid under room temperature, main chain backbone mostly be alicyclic,
Linear thermoplastic's structure that aliphatic and aromatic series segment are constituted, the epoxide group in its strand has higher reaction and lives
Property, can under the effect of light and heat open loop and with firming agent react formed crosslinking tridimensional network.
Epoxy molding plastic is with epoxy resin as matrix resin, adds firming agent, inorganic filler, curing accelerator, fire-retardant
Various ingredients is mixing forms for agent, coloring agent, coupling agent etc..Wherein the Main Function of inorganic filler is to reduce thermal coefficient of expansion, suction
Water rate, molding shrinkage and production cost, it is also possible to reduce potentiation, improve reliability.Conventional inorganic filler is mainly two
Silica powder, has that joint behavior is excellent, thermal coefficient of expansion is low, lower-price characteristic, uses the silicon powder can as inserts
To effectively reduce the thermal coefficient of expansion of epoxy molding plastic, water absorption rate, improve the thermostability of moulding compound, mechanical strength, dielectricity
Energy.But, along with electronic package small, lightweight, encapsulation is the most not only related to the packaging protection of components and parts
Problem, and to the size of components and parts, heat distributes and device fire resistance proposes the highest requirement.Encapsulating material
Become the important aspect affecting electronic devices and components performance with packaged type, the performance the most even becoming new increases
Point.Using high heat conduction inorganic filler and environmental protection fire retarding agent is to improve epoxy molding plastic heat conduction and the important channel of fire resistance,
Through obtaining the highest attention of researcher.The inorganic filler of the high heat conduction generally used is mainly aluminium nitride, boron nitride, silicon nitride etc.
The oxide fillers such as the nitride of synthetic and aluminium oxide.Along with in electronic package material halogen flame be magnesium hydroxide and
Aluminium hydroxide etc., they have Heat stability is good, efficiently, press down cigarette, resistance is dripped, fill safety, to features such as environment are the most pollution-free,
Environmental-protection flame-retardant filler is used widely.But traditional moulding compound exists, and thermal conductivity is low, thermal shock resistance is the best
Defect, make the range of moulding compound there is limitation.
Summary of the invention
The technical problem that present invention mainly solves: there is thermal conductivity for tradition moulding compound at present low, cause its heat resistanceheat resistant
The defect that impact property is the best, serpentine is activated by the present invention by calcining, and acidleach carries out remove impurity, then with methanol, dicyclo penta 2
After the mixing such as alkene, it is placed in reactor and carries out laser and irradiate and react, to its modifying surface, increase high hot, finally
Mixing with the ball milling such as o-cresol formaldehyde epoxy resin, white carbon black, triethylene tetramine, extruding pelletization i.e. obtains high heat conduction epoxy molding plastic, this
Invention, with serpentine as raw material, by being modified being fabricated to filler to it, thus compensate for tradition moulding compound heat conductivility not
Height, causes its defect that thermal shock resistance is the best under the high temperature conditions, has prospect of production widely.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen protection,
Design temperature is 900~1000 DEG C, insulation calcining 1~2h, cools to room temperature with the furnace, is 29% salt by calcined material and mass fraction
Acid solution presses solid-to-liquid ratio 1:3, with 180r/min stirring mixing 30~40min, filters subsequently, in using distilled water wash filtering residue extremely
Property, place in air-dry machine and air-dry;
(2) filtering residue after above-mentioned air-drying is put in mill and milled, cross 200 mesh sieves, collect the granule that sieves, by weight
Number meter, take 40~45 parts of granules that sieve, 24~26 parts of methanol, 13~16 parts of dicyclopentadienes, 8~12 parts of 1.2mol/L ammonia, 3
~6 parts of lauryl mercaptans and 1~2 part of benzoin ethyl ether, put in glass reaction still, use gaseous mixture by the sky in reactor
After gas displacement completely, and boosting to 3~5MPa, with 200r/min stirring mixing 20~30min, described gaseous mixture is nitrogen and first
Silane 2:1 by volume mixes;
(3) after above-mentioned stirring mixes, temperature rising glass temperature of reaction kettle to 120~130 DEG C, use carbon dioxide laser to irradiate
Glass reaction still, wavelength is 10.6 μm, and power setting is 40~70W, irradiates 2~4min, is cooled to 2 DEG C/min speed subsequently
Room temperature, is depressurized to normal atmosphere, and discharging is also filtered, and is put into by filtering residue in calcining furnace, and design temperature is 1100~1200 DEG C, protects
Temperature calcining 13~22min, cools to room temperature with the furnace, calcined material is taken out and pulverize, and crosses 200 mesh sieves, obtains high heat conduction epoxy mold
Material filler;
(4) count by weight, take 45~55 parts of o-cresol formaldehyde epoxy resins, 26~29 parts of above-mentioned high heat conduction epoxy molding plastics are filled out
Material, 8~12 parts of white carbon blacks, 4~7 parts of triethylene tetramines, 1~2 part of tetrabutyl titanate and 1~2 part of stearic acid, put in ball mill,
By ratio of grinding media to material 10:1, in ball mill, add alloying pellet, mix 10~15min with 300r/min ball milling, mixture is put into double
In screw extruder, design temperature is 105~115 DEG C, carries out extruding pelletization, high heat conduction epoxy molding plastic.
The physical property of the present invention is: heat conductivity is 0.6~0.8W/ (m K), and bending strength is 130~190MPa,
Bending modulus is 6~12GPa, and high temperature resistant is 500~600 DEG C.
The invention has the beneficial effects as follows:
(1) present invention uses serpentine to be raw material, reduces the cost of this epoxy molding plastic, thus has reached the system of performance and cost
One, can be applicable to encapsulate various semiconductor device and integrated circuit, it will have good application prospect;
(2) epoxy molding plastic has heat conductivility preferably, the feature that mechanical strength is high, thermal coefficient of expansion is low, water absorption rate is low.
Detailed description of the invention
First taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen
Protection, design temperature is 900~1000 DEG C, insulation calcining 1~2h, cools to room temperature with the furnace, by calcined material with mass fraction is
29% hydrochloric acid solution presses solid-to-liquid ratio 1:3, with 180r/min stirring mixing 30~40min, filters subsequently, uses distilled water wash filter
Slag, to neutral, place in air-dry machine and air-dries;Filtering residue after above-mentioned air-drying is put in mill and mills, cross 200 mesh sieves,
Collection is sieved granule, counts by weight, take 40~45 parts of granules that sieve, 24~26 parts of methanol, 13~16 parts of dicyclopentadienes,
8~12 parts of 1.2mol/L ammonia, 3~6 parts of lauryl mercaptans and 1~2 part of benzoin ethyl ether, put in glass reaction still, make
After being replaced completely by air in reactor with gaseous mixture, and boost to 3~5MPa, with 200r/min stirring mixing 20~
30min, described gaseous mixture is nitrogen and monosilane 2:1 by volume mixes;After above-mentioned stirring mixes, temperature rising glass is anti-
Answering still temperature to 120~130 DEG C, use carbon dioxide laser to irradiate glass reaction still, wavelength is 10.6 μm, and power setting is
40~70W, to irradiate 2~4min, be cooled to room temperature with 2 DEG C/min speed subsequently, be depressurized to normal atmosphere, discharging is also filtered,
Being put into by filtering residue in calcining furnace, design temperature is 1100~1200 DEG C, insulation calcining 13~22min, cools to room temperature with the furnace, will
Calcined material is taken out and is pulverized, and crosses 200 mesh sieves, obtains high heat conduction epoxy molding plastic filler;Count by weight, take 45~55 parts of adjacent first
Novolac epoxy resin, 26~29 parts of above-mentioned high heat conduction epoxy molding plastic fillers, 8~12 parts of white carbon blacks, 4~7 parts of triethylene tetramines, 1
~2 parts of tetrabutyl titanates and 1~2 part of stearic acid, put in ball mill, by ratio of grinding media to material 10:1, in ball mill, add alloying pellet,
Mixing 10~15min with 300r/min ball milling, put into by mixture in double screw extruder, design temperature is 105~115 DEG C,
Carry out extruding pelletization, high heat conduction epoxy molding plastic.
Example 1
First taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen to protect
Protecting, design temperature is 900 DEG C, insulation calcining 1h, cools to room temperature with the furnace, is 29% hydrochloric acid solution by calcined material and mass fraction
By solid-to-liquid ratio 1:3, with 180r/min stirring mixing 30min, filter subsequently, use distilled water wash filtering residue to neutral, place into
Air-dry machine air-dries;Filtering residue after above-mentioned air-drying is put in mill and mills, cross 200 mesh sieves, collect the granule that sieves, press
Parts by weight meter, takes 40 parts of granules that sieve, 24 parts of methanol, 13 parts of dicyclopentadienes, 8 parts of 1.2mol/L ammonia, 3 parts of dodecyls
Mercaptan and 1 part of benzoin ethyl ether, put in glass reaction still, after using gaseous mixture to be replaced completely by the air in reactor, and
Boost to 3MPa, with 200r/min stirring mixing 20min, described gaseous mixture be nitrogen and monosilane 2:1 by volume mixing and
Become;After above-mentioned stirring mixes, temperature rising glass temperature of reaction kettle to 120 DEG C, use carbon dioxide laser to irradiate glass reaction
Still, wavelength is 10.6 μm, and power setting is 40W, irradiates 2min, is cooled to room temperature with 2 DEG C/min speed subsequently, is depressurized to standard
Atmospheric pressure, discharging also filters, put into by filtering residue in calcining furnace, and design temperature is 1100 DEG C, insulation calcining 13min, furnace cooling
To room temperature, calcined material taken out and pulverizes, crossing 200 mesh sieves, obtain high heat conduction epoxy molding plastic filler;Count by weight, take 45
Part o-cresol formaldehyde epoxy resin, 26 parts of above-mentioned high heat conduction epoxy molding plastic fillers, 8 parts of white carbon blacks, 4 parts of triethylene tetramines, 1 part of metatitanic acid
N-butyl and 1 part of stearic acid, put in ball mill, by ratio of grinding media to material 10:1, adds alloying pellet, with 300r/min ball in ball mill
Mill mixing 10min, mixture is put in double screw extruder, design temperature is 105 DEG C, carries out extruding pelletization, high
Heat conduction epoxy molding plastic.
The physical property of the present invention is: heat conductivity is 0.6W/ (m K), and bending strength is 130MPa, and bending modulus is
6GPa, high temperature resistant is 500 DEG C.
Example 2
First taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen to protect
Protecting, design temperature is 950 DEG C, insulation calcining 1.5h, cools to room temperature with the furnace, is that 29% hydrochloric acid is molten by calcined material and mass fraction
Liquid presses solid-to-liquid ratio 1:3, with 180r/min stirring mixing 35min, filters subsequently, uses distilled water wash filtering residue the most neutral, then put
Enter in air-dry machine and air-dry;Filtering residue after above-mentioned air-drying is put in mill and mills, cross 200 mesh sieves, collect the granule that sieves,
Count by weight, take 43 parts of granules that sieve, 25 parts of methanol, 15 parts of dicyclopentadienes, 10 parts of 1.2mol/L ammonia, 5 part 12
Alkyl hydrosulfide and 1.5 parts of benzoin ethyl ethers, put in glass reaction still, uses gaseous mixture to be replaced completely by the air in reactor
After, and boost to 4MPa, with 200r/min stirring mixing 25min, described gaseous mixture is nitrogen and monosilane 2:1 by volume mixes
Conjunction forms;After above-mentioned stirring mixes, temperature rising glass temperature of reaction kettle to 125 DEG C, use carbon dioxide laser to irradiate glass
Reactor, wavelength is 10.6 μm, and power setting is 50W, irradiates 3min, is cooled to room temperature with 2 DEG C/min speed subsequently, is depressurized to
Normal atmosphere, discharging also filters, put into by filtering residue in calcining furnace, and design temperature is 1150 DEG C, and insulation calcining 18min, with stove
It is cooled to room temperature, calcined material is taken out and pulverizes, cross 200 mesh sieves, obtain high heat conduction epoxy molding plastic filler;Count by weight,
Take 50 parts of o-cresol formaldehyde epoxy resins, 28 parts of above-mentioned high heat conduction epoxy molding plastic fillers, 10 parts of white carbon blacks, 5 parts of triethylene tetramines,
1.5 parts of tetrabutyl titanates and 1.5 parts of stearic acid, put in ball mill, by ratio of grinding media to material 10:1, adds alloying pellet in ball mill,
With 300r/min ball milling mixing 13min, being put into by mixture in double screw extruder, design temperature is 110 DEG C, carries out extrusion and makes
Grain, high heat conduction epoxy molding plastic.
The physical property of the present invention is: heat conductivity is 0.8W/ (m K), and bending strength is 190MPa, and bending modulus is
12GPa, high temperature resistant is 600 DEG C.
Example 3
First taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen to protect
Protecting, design temperature is 1000 DEG C, insulation calcining 2h, cools to room temperature with the furnace, is that 29% hydrochloric acid is molten by calcined material and mass fraction
Liquid presses solid-to-liquid ratio 1:3, with 180r/min stirring mixing 40min, filters subsequently, uses distilled water wash filtering residue the most neutral, then put
Enter in air-dry machine and air-dry;Filtering residue after above-mentioned air-drying is put in mill and mills, cross 200 mesh sieves, collect the granule that sieves,
Count by weight, take 45 parts of granules that sieve, 26 parts of methanol, 16 parts of dicyclopentadienes, 12 parts of 1.2mol/L ammonia, 6 part 12
Alkyl hydrosulfide and 2 parts of benzoin ethyl ethers, put in glass reaction still, uses gaseous mixture to be replaced completely by the air in reactor
After, and boost to 5MPa, with 200r/min stirring mixing 30min, described gaseous mixture is nitrogen and monosilane 2:1 by volume mixes
Conjunction forms;After above-mentioned stirring mixes, temperature rising glass temperature of reaction kettle to 130 DEG C, use carbon dioxide laser to irradiate glass
Reactor, wavelength is 10.6 μm, and power setting is 70W, irradiates 4min, is cooled to room temperature with 2 DEG C/min speed subsequently, is depressurized to
Normal atmosphere, discharging also filters, put into by filtering residue in calcining furnace, and design temperature is 1200 DEG C, and insulation calcining 22min, with stove
It is cooled to room temperature, calcined material is taken out and pulverizes, cross 200 mesh sieves, obtain high heat conduction epoxy molding plastic filler;Count by weight,
Take 55 parts of o-cresol formaldehyde epoxy resins, 29 parts of above-mentioned high heat conduction epoxy molding plastic fillers, 12 parts of white carbon blacks, 7 parts of triethylene tetramines, 2
Part tetrabutyl titanate and 2 parts of stearic acid, put in ball mill, by ratio of grinding media to material 10:1, adds alloying pellet in ball mill, with
300r/min ball milling mixing 15min, puts into mixture in double screw extruder, and design temperature is 115 DEG C, carries out extrusion and makes
Grain, high heat conduction epoxy molding plastic.
The physical property of the present invention is: heat conductivity is 0.7W/ (m K), and bending strength is 160MPa, and bending modulus is
9GPa, high temperature resistant is 550 DEG C.
Claims (1)
1. the preparation method of one kind high heat conduction epoxy molding plastic, it is characterised in that concrete preparation process is:
(1) taking serpentine and put into pulverizing in pulverizer, cross 50 mesh sieves, the granule that will sieve is put in calcining furnace, uses nitrogen protection,
Design temperature is 900~1000 DEG C, insulation calcining 1~2h, cools to room temperature with the furnace, is 29% salt by calcined material and mass fraction
Acid solution presses solid-to-liquid ratio 1:3, with 180r/min stirring mixing 30~40min, filters subsequently, in using distilled water wash filtering residue extremely
Property, place in air-dry machine and air-dry;
(2) filtering residue after above-mentioned air-drying is put in mill and milled, cross 200 mesh sieves, collect the granule that sieves, by weight
Number meter, take 40~45 parts of granules that sieve, 24~26 parts of methanol, 13~16 parts of dicyclopentadienes, 8~12 parts of 1.2mol/L ammonia, 3
~6 parts of lauryl mercaptans and 1~2 part of benzoin ethyl ether, put in glass reaction still, use gaseous mixture by the sky in reactor
After gas displacement completely, and boosting to 3~5MPa, with 200r/min stirring mixing 20~30min, described gaseous mixture is nitrogen and first
Silane 2:1 by volume mixes;
(3) after above-mentioned stirring mixes, temperature rising glass temperature of reaction kettle to 120~130 DEG C, use carbon dioxide laser to irradiate
Glass reaction still, wavelength is 10.6 μm, and power setting is 40~70W, irradiates 2~4min, is cooled to 2 DEG C/min speed subsequently
Room temperature, is depressurized to normal atmosphere, and discharging is also filtered, and is put into by filtering residue in calcining furnace, and design temperature is 1100~1200 DEG C, protects
Temperature calcining 13~22min, cools to room temperature with the furnace, calcined material is taken out and pulverize, and crosses 200 mesh sieves, obtains high heat conduction epoxy mold
Material filler;
(4) count by weight, take 45~55 parts of o-cresol formaldehyde epoxy resins, 26~29 parts of above-mentioned high heat conduction epoxy molding plastics are filled out
Material, 8~12 parts of white carbon blacks, 4~7 parts of triethylene tetramines, 1~2 part of tetrabutyl titanate and 1~2 part of stearic acid, put in ball mill,
By ratio of grinding media to material 10:1, in ball mill, add alloying pellet, mix 10~15min with 300r/min ball milling, mixture is put into double
In screw extruder, design temperature is 105~115 DEG C, carries out extruding pelletization, high heat conduction epoxy molding plastic.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109608691A (en) * | 2018-12-11 | 2019-04-12 | 杭州纳尔森精细化工有限公司 | A kind of preparation method of serpentine-magnesium hydroxide-boric acid magnesium compound fire retardant |
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CN102391473A (en) * | 2011-09-02 | 2012-03-28 | 中国科学院广州地球化学研究所 | Preparation method for anhydride cured epoxy resin/palygorskite nanocomposite material |
CN103408043A (en) * | 2013-08-13 | 2013-11-27 | 中国地质大学(武汉) | Method for preparing high-purity magnesium oxide with serpentine as raw material |
CN104479606A (en) * | 2014-12-24 | 2015-04-01 | 中科院广州化学有限公司 | High-temperature-resistant high-thermal-conductivity boron-dopedorganosilicon epoxy pouring sealant as well as preparation method and application thereof |
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Patent Citations (4)
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CN102020963A (en) * | 2010-12-02 | 2011-04-20 | 浙江科创新材料科技有限公司 | High-temperature-resistant and high thermal conductive adhesive and preparation method thereof |
CN102391473A (en) * | 2011-09-02 | 2012-03-28 | 中国科学院广州地球化学研究所 | Preparation method for anhydride cured epoxy resin/palygorskite nanocomposite material |
CN103408043A (en) * | 2013-08-13 | 2013-11-27 | 中国地质大学(武汉) | Method for preparing high-purity magnesium oxide with serpentine as raw material |
CN104479606A (en) * | 2014-12-24 | 2015-04-01 | 中科院广州化学有限公司 | High-temperature-resistant high-thermal-conductivity boron-dopedorganosilicon epoxy pouring sealant as well as preparation method and application thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109608691A (en) * | 2018-12-11 | 2019-04-12 | 杭州纳尔森精细化工有限公司 | A kind of preparation method of serpentine-magnesium hydroxide-boric acid magnesium compound fire retardant |
CN109608691B (en) * | 2018-12-11 | 2021-03-05 | 杭州纳尔森精细化工有限公司 | Preparation method of serpentine-magnesium hydroxide-magnesium borate composite flame retardant |
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Application publication date: 20170104 |