CN105838028A - High-heat-conductive resin composition and preparation method thereof - Google Patents
High-heat-conductive resin composition and preparation method thereof Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to a high-heat-conductive resin composition and a preparation method thereof and aims to provide the high-heat-conductive resin composition which has excellent electric-insulation performance. The preparation method is simple and is low-cost. The high-heat-conductive resin composition comprises the following raw materials: electronic-grade bisphenol-A epoxy resin, heat conductive resin, a curing agent, a curing accelerator, a high-heat-conductive inorganic filling material, a coupling agent and an organic solvent. The preparation method includes the steps of: 1) preparing an acetone solution of the coupling agent, adding the high-heat-conductive inorganic filling material, stirring the liquid uniformly, and removing the solvent and drying and grinding the material to prepare a surface-treated inorganic filling material; and 2) preparing a solution with the curing agent and the organic solvent, and successively adding the electronic-grade bisphenol-A epoxy resin, multifunctional epoxy grain, the heat conductive resin, the surface-treated inorganic filling material and the curing accelerator, performing mixing emulsification and dispersion to prepare the high-heat-conductive resin composition.
Description
Technical field
The present invention relates to a kind of highly thermal-conductive resin composition and preparation method thereof.
Background technology
Along with society and economic fast development, the whole world is caused to face energy shortage with complete owing to excessively developing
The threat of ball border drastic change, studying a kind of novel LED light source with power saving function just becomes 21
The new problem in century.LED light source needs the greatest problem solved to be " heat radiation ", and current LED light source is mainly adopted
Dispelling the heat with the PCB with heat conductivility, what common heat-conducting type PCB predominantly had a heat conductivity covers copper
Plate is made.
Heat-conductive copper-clad plate includes aluminum-based copper-clad plate and heat-conducting type CEM-3 copper-clad plate, and aluminum-based copper-clad plate has superior
Heat conductivility, but due to the thinnest reason of insulating barrier, its electrical insulation capability is compared heat-conducting type CEM-3 and is covered copper
There is a big difference for plate, and the especially distance of lamp batten circuit and sheet edge is closer, and electrical insulation capability is difficult to
Ensure；Although general heat-conducting type CEM-3 electrical insulation capability is better than aluminum-based copper-clad plate, but electrical insulation capability is same
Sample has much room for improvement.
Chinese patent CN 101848604 B discloses a kind of employing epoxy resin, Nitrogen-containing Phenolic Resins, oxidation
The materials such as aluminum, boron nitride, aluminium nitride prepare heat conduction glue, impregnated glass fiber cloth/felt, are dried into semi-solid preparation
Sheet, makes the CEM-3 copper-clad plate with heat conductivity through hot pressing.Patent CN 102205675 A discloses one
The materials such as epoxy resin, phenol novolacs, DADPS, aluminium oxide are used to prepare heat conduction glue,
Impregnated glass fiber cloth/felt is dried into prepreg, makes the CEM-3 copper-clad plate with heat conductivity through hot pressing.
Patent CN 105172262 A disclose a kind of use epoxy resin, dicyandiamide, aluminium oxide etc., carborundum,
Heat conduction glue prepared by the materials such as graphenic surface modification boron nitride and aluminium nitride, and impregnated glass fiber cloth/felt is dried
Become prepreg, make the CEM-3 copper-clad plate with heat conductivity through hot pressing.Patent CN 105269916 A is public
Open a kind of employing epoxy resin, toughener B, dicyandiamide, phenyl amines firming agent, aluminium oxide etc. material system
Standby heat conduction glue, impregnated glass fiber cloth/felt is dried into prepreg, makes through hot pressing and have heat conductivity
CEM-3 copper-clad plate.Patent CN 104669710 A discloses a kind of employing resin adhesive liquid and prepares heat conduction glue,
Impregnated glass fiber cloth is dried into prepreg, is mingled with polymer graphite film and makes through hot pressing and have heat conductivity
CEM-3 copper-clad plate.These technology all fail effectively to promote the electrical insulation capability of heat-conductive copper-clad plate, it is therefore desirable to enter
One step is improved.
Summary of the invention
It is an object of the invention to overcome the deficiency in above-mentioned background technology, it is provided that one has good electrical insulating properties
The highly thermal-conductive resin composition of energy, to be applied to heat-conductive copper-clad plate.
The present invention also provides for the preparation method of a kind of highly thermal-conductive resin composition, and this preparation method should have technique
Simply, lower-cost feature.
The technical scheme is that
A kind of highly thermal-conductive resin composition, including the raw material of following weight portion:
The electron level bisphenol A type epoxy resin of 80-90 part, the heat-conducting type resin of 10-20 part, 0.5-30 part
Firming agent, the curing accelerator of 0.05-0.15 part, the high heat conduction inorganic filler of 100-300 part, 0.5-3 part
Coupling agent, the organic solvent of 50-100 part.
Described electron level bisphenol A type epoxy resin includes that epoxide equivalent is between 350-500eq/100g and bromine content
Brominated bisphenol a type epoxy resin between 16-50%；Epoxide equivalent is between the bis-phenol of 190-1000eq/100g
A type epoxy resin；Epoxide equivalent one in the multifunctional type epoxy resin of 180-300eq/100g or
Two or more mixture.
Described heat-conducting type resin is the low polymer with biphenyl structural, including biphenyl type epoxy resin or
Biphenyl type phenolic resin.
Described firming agent is latent curing agent, aromatic amine curing agent, line style curable synthetic resin agent, double
One or more mixture in phenol A type phenolic resin.
Described latent curing agent is dicyandiamide；Described aromatic amine curing agent is DADPS, diamino
One in yl diphenyl ether, 3,3'-bis-chloro-4,4'-diaminodiphenyl-methane or diaminodiphenyl-methane or
Two or more mixture；Described line style curable synthetic resin agent is that hydroxyl equivalent is between 90-110eq/100g
Phenol type phenolic resin；The hydroxyl equivalent of described bisphenol A-type phenolic resin is between 90 120eq/100g.
Described curing accelerator is imidazoles, including 2-methylimidazole, 2-phenylimidazole or 2-ethyl-4-first
One or more mixture in base imidazoles.
Described high heat conduction inorganic filler is in aluminium oxide, aluminium nitride, boron nitride, carborundum, magnesium oxide
Kind or two or more mixture, mean diameter is 0.1-100 μm.
Described coupling agent is silane coupling agent, including KH-550 or KH-560.
Described organic solvent be dimethylformamide, dimethyl acetylamide, ethylene glycol monomethyl ether, propylene glycol monomethyl ether,
At least one in acetone, butanone.
The preparation method of a kind of highly thermal-conductive resin composition, comprises the following steps:
1) first coupling agent is configured to the acetone soln of 2% concentration, is subsequently adding high heat conduction inorganic filler, stirring
After Jun Yun through desolvation, dry, grind after make surface treatment inorganic filling material；
2) firming agent and organic solvent are configured to the solution of 25% concentration, are sequentially added into electron level bisphenol A-type
Epoxy resin, multifunctional type epoxy resin, heat-conducting type resin, surface treatment inorganic filling material and curing accelerator,
Mixing and emulsifying disperses 6-10 hour, makes highly thermal-conductive resin composition.
Described step 1) in organic solvent be acetone or butanone.
Described step 2) in organic solvent be: dimethylformamide, dimethyl acetylamide, ethylene glycol monomethyl ether,
At least one in propylene glycol monomethyl ether, acetone, butanone.
The invention has the beneficial effects as follows:
The heat-conducting type CEM-3 copper-clad plate using highly thermal-conductive resin composition to make, not only has good heat conduction
Performance (heat conductivity reaches 1.5W/m K), and (breakdown voltage reaches to be obviously improved electrical insulation capability
53-60KV), the safety of LED product has been effectively ensured and has extended service life；This high heat conduction simultaneously
The production technology of resin combination is simple, production cost is relatively low.
Detailed description of the invention
In the present invention:
1) epoxide equivalent between 350-500eq/100g and bromine content between the bmminated bisphenol-A type ring of 16-50%
Epoxy resins:
Product type BEB 530A80, BEB 400A70, manufacturer is the Changchun artificial resin factory limited public affairs of share
Department (Chang Chun Plastics Co.Ltd.)；Product type NPEB-450A80, NPEB-400A80,
Manufacturer is Nanya Plastic Cement Industry Co., Ltd (NAN YA PLASTICS CORPORATION)；
2) epoxide equivalent is between the bisphenol A type epoxy resin of 190-1000eq/100g:
Product type BE-501, BE-504, manufacturer is Changchun Artificial Resin Factory Co. Ltd.；Product
Model NPSN-901K80, NPES904, manufacturer is Nanya Plastic Cement Industry Co., Ltd；
3) epoxide equivalent is between the multifunctional type epoxy resin of 180-300eq/100g:
Product type BNE200, CNE200, manufacturer is Changchun Artificial Resin Factory Co. Ltd.；
4) biphenyl type epoxy resin:
Product type SE-350, manufacturer is letter A science and technology (SHIN-A T&C)；
5) biphenyl type phenolic resin:
Product type 7851M, manufacturer is bright and chemical conversion Co., Ltd. (MEIWA PLASTIC
INDUSTRIES,LTD.)；
6) hydroxyl equivalent is between the phenol type phenolic resin of 90-110eq/100g:
Product type PN-8110, manufacturer is Changchun Artificial Resin Factory Co. Ltd.；
Product type PF-8020, manufacturer is holy well group (SQ GROUP)；
7) hydroxyl equivalent is between the bisphenol A-type phenolic resin of 90 120eq/100g:
Product type BN-120, manufacturer is Changchun Artificial Resin Factory Co. Ltd.；
Product type SH-2120, manufacturer is holy well group.
Below in conjunction with specific embodiment, the invention will be further described, but the invention is not limited in following
Embodiment.
Embodiment one
A kind of highly thermal-conductive resin composition, including the raw material of following weight portion:
The brominated bisphenol a type epoxy resin BEB 530A80 of 60 parts, the bisphenol A type epoxy resin of 10 parts
BE-501, the polyfunctional epoxy resin BNE200 of 20 parts, the biphenyl type epoxy resin SE-350 of 20 parts, 0.5
Part dicyandiamide, the diaminodiphenyl ether of 25 parts, the phenol type phenolic resin PN-8110 of 20 parts, 0.1 part
2-methylimidazole, the aluminium oxide of 280 parts, the KH-560 of 3 parts, the propylene glycol monomethyl ether of 60 parts, 40 parts
Butanone.
Embodiment two
A kind of highly thermal-conductive resin composition, including the raw material of following weight portion:
The brominated bisphenol a type epoxy resin BEB 400A70 of 60 parts, the bisphenol A type epoxy resin of 20 parts
BE-504, the polyfunctional epoxy resin CNE200 of 20 parts, the biphenyl type phenolic resin 7851M of 20 parts, 0.5
Part dicyandiamide, the diaminodiphenyl ether of 25 parts, the 2-methylimidazole of 0.1 part, the aluminium nitride of 280 parts, 3
The KH-550 of part, the propylene glycol monomethyl ether of 60 parts, the butanone of 40 parts.
Embodiment three
A kind of highly thermal-conductive resin composition, including the raw material of following weight portion:
The brominated bisphenol a type epoxy resin NPEB-450A80 of 50 parts, the bisphenol A type epoxy resin of 10 parts
NPSN-901K80, the polyfunctional epoxy resin CNE200 of 20 parts, the biphenyl type epoxy resin SE-350 of 10 parts,
The dicyandiamide of 0.5 part, the DADPS of 25 parts, the phenol type phenolic resin PN-8110 of 20 parts, 0.2
Part 2-phenylimidazole, the boron nitride of 280 parts, the KH-560 of 3 parts, the propylene glycol monomethyl ether of 60 parts, 40 parts
Butanone.
Embodiment four
A kind of highly thermal-conductive resin composition, including the raw material of following weight portion:
The brominated bisphenol a type epoxy resin NPEB-400A80 of 60 parts, the bisphenol A type epoxy resin of 10 parts
NPES904, the polyfunctional epoxy resin CNE200 of 20 parts, the biphenyl type epoxy resin SE-350 of 20 parts, 0.5
Part dicyandiamide, the phenol type phenolic resin PF-8020 of 40 parts, the 2-ethyl-4-methylimidazole of 0.3 part,
The magnesium oxide of 100 parts, the aluminium oxide of 100 parts, the KH-560 of 1 part, the acetone of 80 parts.
Comparative example
Common non-conductive CEM-3 copper-clad laminate is as veneer and glass by FR-4 glass cloth prepreg
Felt prepreg as sandwich combination form through hot pressing, wherein sandwich prepreg resin combination, including with
The raw material of lower weight portion:
The brominated epoxy resin of 80 parts, the bisphenol A epoxide resin of 10 parts, the polyfunctional epoxy resin of 10 parts,
The dicyandiamide of 4 parts, the aluminium hydroxide of 70 parts, the magnesium hydroxide of 30 parts, the KH-560 of 1 part, 0.1 part
2-methylimidazole, the dimethylformamide of 30 parts.
Prepare highly thermal-conductive resin composition
1) first coupling agent is configured to the acetone soln of 2% concentration, is subsequently adding high heat conduction inorganic filler, stirring
After Jun Yun through desolvation, dry, grind after make surface treatment inorganic filling material；
2) firming agent and organic solvent are configured to the solution of 25% concentration, are sequentially added into electron level bisphenol A-type
Epoxy resin, multifunctional type epoxy resin, heat-conducting type resin, surface treatment inorganic filling material and curing accelerator,
Mixing and emulsifying disperses 6-10 hour, makes highly thermal-conductive resin composition.
Make copper-clad laminate
1) highly thermal-conductive resin composition prepared is coated in E-glass cloth, and (7628 E-glass are fine
Wei Bu) with (75 E-glass felt) on glass felt, 150 170 DEG C of oven for baking 3-5 minute,
Make glass cloth prepreg and glass felt prepreg；
2) a glass cloth prepreg is respectively sticked on the two sides of glass cloth prepreg, one the most wherein
An electrolytic copper foil is sticked on glass cloth prepreg；
3) the above-mentioned blank prepared is sent in vacuum hotpressing machine, at 60-210 DEG C of temperature, 6-80kgf/cm2
Hot pressing 2-3 hour under pressure and 10mmHg vacuum, i.e. makes heat-conducting type CEM-3 copper-clad plate.
Use the copper-clad laminate that highly thermal-conductive resin composition prepares compared with common CEM-3 copper-clad laminate
Relatively, heat conductivity is significantly increased.Main results is as shown in the table:
In addition to indicating especially, in the present invention, ratio and the content of all the components are by weight.
Claims (9)
1. a highly thermal-conductive resin composition, including the raw material of following weight portion:
The electron level bisphenol A type epoxy resin of 80-90 part, the heat-conducting type resin of 10-20 part, 0.5-30 part
Firming agent, the curing accelerator of 0.05-0.15 part, the high heat conduction inorganic filler of 100-300 part, 0.5-3 part
Coupling agent, the organic solvent of 50-100 part；
Described electron level bisphenol A type epoxy resin is that epoxide equivalent is situated between 350-500eq/100g and bromine content
In the brominated bisphenol a type epoxy resin of 16-50%, epoxide equivalent between the bisphenol-A of 190-1000eq/100g
Type epoxy resin, the epoxide equivalent one or two in the multifunctional type epoxy resin of 180-300eq/100g
Plant above mixture；
Described heat-conducting type resin is the low polymer with biphenyl structural, including biphenyl type epoxy resin or
Biphenyl type phenolic resin；
Described firming agent is latent curing agent, aromatic amine curing agent, line style curable synthetic resin agent, double
One or more mixture in phenol A type phenolic resin.
Highly thermal-conductive resin composition the most according to claim 1, it is characterised in that: described latency is solid
Agent is dicyandiamide；Described aromatic amine curing agent is DADPS, diaminodiphenyl ether, 3,3'-bis-
One or more mixing in chloro-4,4'-diaminodiphenyl-methane or diaminodiphenyl-methane
Thing；Described line style curable synthetic resin agent is the hydroxyl equivalent phenol type phenolic aldehyde tree between 90-110eq/100g
Fat；The hydroxyl equivalent of described bisphenol A-type phenolic resin is between 90 120eq/100g.
Highly thermal-conductive resin composition the most according to claim 1, it is characterised in that: described solidification promotes
Agent is imidazoles, for 2-methylimidazole, the one in 2-phenylimidazole or 2-ethyl-4-methylimidazole or two
Plant above mixture.
Highly thermal-conductive resin composition the most according to claim 1, it is characterised in that: described high heat conduction without
Machine filler is the mixed of one or more in aluminium oxide, aluminium nitride, boron nitride, carborundum, magnesium oxide
Compound, mean diameter is 0.1-100 μm.
Highly thermal-conductive resin composition the most according to claim 1, it is characterised in that: described coupling agent is
Silane coupling agent, including KH-550 or KH-560.
Highly thermal-conductive resin composition the most according to claim 1, it is characterised in that: described organic solvent
For in dimethylformamide, dimethyl acetylamide, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, acetone or butanone
At least one.
7. the preparation method of the highly thermal-conductive resin composition described in claim 1, comprises the following steps:
1) first coupling agent is configured to the acetone soln of 2% concentration, is subsequently adding high heat conduction inorganic filler, stirring
After Jun Yun through desolvation, dry, grind after make surface treatment inorganic filling material；
2) firming agent and organic solvent are configured to the solution of 25% concentration, are sequentially added into electron level bisphenol A-type
Epoxy resin, multifunctional type epoxy resin, heat-conducting type resin, surface treatment inorganic filling material and curing accelerator,
Mixing and emulsifying disperses 6-10 hour, makes highly thermal-conductive resin composition.
Highly thermal-conductive resin composition the most according to claim 7, it is characterised in that: described step 1)
In organic solvent be acetone or butanone.
Highly thermal-conductive resin composition the most according to claim 7, it is characterised in that: described step 2)
In organic solvent be: dimethylformamide, dimethyl acetylamide, ethylene glycol monomethyl ether, propylene glycol monomethyl ether,
At least one in acetone, butanone.
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| CN107177166A (en) * | 2017-06-09 | 2017-09-19 | 格丽泰新材料科技（苏州）有限公司 | A kind of transparent heat-insulated resistance to UV resin and its preparation method and application |
| CN107502253A (en) * | 2017-07-26 | 2017-12-22 | 江苏诺德新材料股份有限公司 | A kind of glue for high heat conduction type copper-clad plate aluminium base and preparation method thereof |
| CN108059926A (en) * | 2017-11-14 | 2018-05-22 | 浙江元集新材料科技股份有限公司 | A kind of preparation method of the special high heat conduction bonding sheet of aluminum-based copper-clad plate |
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Application publication date: 20160810 |