CN105348734A - An environmental-friendly heat-resistant epoxy resin material specially used for printed circuit boards - Google Patents
An environmental-friendly heat-resistant epoxy resin material specially used for printed circuit boards Download PDFInfo
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- CN105348734A CN105348734A CN201510780516.7A CN201510780516A CN105348734A CN 105348734 A CN105348734 A CN 105348734A CN 201510780516 A CN201510780516 A CN 201510780516A CN 105348734 A CN105348734 A CN 105348734A
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Abstract
An environmental-friendly heat-resistant epoxy resin material specially used for printed circuit boards is disclosed. Raw materials of the material comprise epoxy resin, epoxy-capped nitrile butadiene rubber, methylhexahydrophthalic anhydride, m-xylylenediamine, N,N-diethyl diethylene triamine, recycled phenolic resin, 2-ethyl-4-methylimidazole, butyl epoxystearate, acetyl tributyl citrate, pentaerythritol, microencapsulated ammonium polyphosphate, nanometer carbon fiber, nanometer calcium carbonate, recycled polyethylene, epoxy-capped polydimethylsiloxane, bisphenol A bisphthalonitrile, diphenylsilanediol and stannous octoate. The material is good in heat resistance, excellent in flame retardance, long in service lifetime and good in environmental protection performance.
Description
Technical field
The present invention relates to epoxide resin material technical field, particularly relate to the special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB).
Background technology
Printed circuit board (PCB) refers to a kind of circuit card formed by printed circuit pattern on the electrically insulating base with electro-conductive material, it is configured such that the position for installing each element is determined, and the circuit-line for connecting described element is printed and is fixed to dull and stereotyped surface, thus makes multiple electronic component be arranged on thick and fast on described flat board.Epoxy resin has the advantages such as excellent adhesive property, wear resisting property, electrical insulation capability, mechanical property, chemical stability and good processing characteristics, shrinking percentage are low and with low cost, increase year by year at the consumption in electric field in recent years, and become one of resin material conventional in circuit card.Along with the development of semi-conductor and electron trade, the size of circuit card is partial to miniaturization, lightweight, multifunction development, adds the needs in multilayer printed circuit board market, strong to the heat resistant requirements of circuit card.In the circuit board, the consumption of plastics accounts for more than 30%, and therefore, the thermotolerance improving epoxy resin used is the task of top priority.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes the special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB), its good heat resistance, excellent fireproof performance, long service life, the feature of environmental protection is good.
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 20-35 part, methyl hexahydrophthalic anhydride 0.5-1.5 part, m-xylene diamine 0.2-1 part, N, N-diethyl diethylene triamine 0.3-1.5 part, resol reworked material 0.5-1.5 part, 2-ethyl-4-methylimidazole 0.2-1 part, butyl epoxy stearate 2-8 part, tributyl acetylcitrate 1-5 part, tetramethylolmethane 2-6 part, micro encapsulation ammonium polyphosphate 5-15 part, carbon nano fiber 3-10 part, nano-calcium carbonate 3-10 part, recycled polyethylene 3-10 part, Epoxy-Terminated Polydimethylsiloxane 2-10 part, bisphenol A-type bi-phthalonitrile 3-10 part, Diphenylsilanediol 10-20 part, stannous octoate 1-2.5 part.
Preferably, the weight ratio of methyl hexahydrophthalic anhydride, m-xylene diamine, N, N-diethyl diethylene triamine, resol reworked material, 2-ethyl-4-methylimidazole is 0.8-1.3:0.5-1:0.7-1.3:0.7-1.3:0.4-1.
Preferably, the weight ratio of tetramethylolmethane, micro encapsulation ammonium polyphosphate, bisphenol A-type bi-phthalonitrile is 4.5-5.2:8-12:6.5-7.2.
Preferably, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 28-32 part, methyl hexahydrophthalic anhydride 1-1.2 part, m-xylene diamine 0.7-0.9 part, N, N-diethyl diethylene triamine 1-1.2 part, resol reworked material 0.9-1.2 part, 2-ethyl-4-methylimidazole 0.6-0.8 part, butyl epoxy stearate 5-6.5 part, tributyl acetylcitrate 3.2-4 part, tetramethylolmethane 4.8-5 part, micro encapsulation ammonium polyphosphate 8-10 part, carbon nano fiber 7-8.5 part, nano-calcium carbonate 7-8 part, recycled polyethylene 5-7 part, Epoxy-Terminated Polydimethylsiloxane 5-6.5 part, bisphenol A-type bi-phthalonitrile 6.8-7 part, Diphenylsilanediol 13-17 part, stannous octoate 1.7-2.2 part.
Preferably, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 30 parts, methyl hexahydrophthalic anhydride 1.1 parts, m-xylene diamine 0.85 part, N, N-diethyl diethylene triamine 1.1 parts, resol reworked material 1 part, 2-ethyl-4-methylimidazole 0.7 part, butyl epoxy stearate 5.8 parts, tributyl acetylcitrate 3.7 parts, tetramethylolmethane 4.9 parts, micro encapsulation ammonium polyphosphate 9 parts, carbon nano fiber 7.6 parts, nano-calcium carbonate 7.8 parts, recycled polyethylene 6 parts, Epoxy-Terminated Polydimethylsiloxane 6.2 parts, bisphenol A-type bi-phthalonitrile 6.9 parts, Diphenylsilanediol 15 parts, stannous octoate 2 parts.
Preferably, described epoxy resin is one or more the mixture in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin.
Preferably, described epoxy resin is that bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin are by weight the mixture for 1-5:2-7:1-3.
Preferably, in described epoxy terminated paracril, oxirane value is 0.08-0.15%, and acrylonitrile content is 15-20%.
Preferably, the mean diameter of described carbon nano fiber is 60-100nm, and tensile strength is 3-6GPa, and density is 1.5-2g/cm
3, thermal conductivity is 1000-1300W/mk; The median size of described nano-calcium carbonate is 30-50nm.
In the present invention, have selected epoxy resin is major ingredient, and with the addition of epoxy terminated paracril modification is carried out to it, by the ratio of gate ring epoxy resins and epoxy terminated paracril, make both consistencies good, in the process of epoxy resin cure, epoxy terminated paracril take part in the solidification of epoxy resin, cross-linked network is defined with epoxy resin, when environment-friendly materials stand under load, epoxy terminated paracril can cause crackle and stop crackle, thus consume a large amount of energy, thus improve the toughness of environment-friendly materials, and improve erosion resistance and the oil-proofness of environment-friendly materials, the methyl hexahydrophthalic anhydride added, m-xylene diamine, N, N-diethyl diethylene triamine, resol reworked material, 2-ethyl-4-methylimidazole are as curing system, by regulating the content of each material in curing system, the performance of each material is worked in coordination with, improve the activity of reaction, reduce the temperature of solidification and the viscosity of matrix, improve processing characteristics, improve the mechanical property of cured article simultaneously, the butyl epoxy stearate added, tributyl acetylcitrate, tetramethylolmethane coordinate, improve thermotolerance and the weathering resistance of environment-friendly materials, Tributyl O-acetylcitrate, butyl epoxy stearate and tetramethylolmethane are safe material simultaneously, and after adding system, the feature of environmental protection is good, in system, stannous octoate auxiliary under, bisphenol A-type bi-phthalonitrile can react with Diphenylsilanediol, with tetramethylolmethane, micro encapsulation ammonium polyphosphate coordinates, in the process of environment-friendly materials burning, what define densification expand into layer of charcoal, serve heat insulation, the effect of oxygen barrier, thus inhibit flame transmission, give the flame retardant resistance of environment-friendly materials excellence, simultaneously bisphenol A-type bi-phthalonitrile can form the reticulated structure of rigidity with epoxy resin, further increase the mechanical property of environment-friendly materials, in addition, after bisphenol A-type bi-phthalonitrile coordinates with Epoxy-Terminated Polydimethylsiloxane with the reaction product of Diphenylsilanediol, improve toughness and the thermotolerance of environment-friendly materials.
Embodiment
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: bisphenol f type epoxy resin 70 parts, bisphenol-A epoxy resin 30 parts, epoxy terminated paracril 20 parts, methyl hexahydrophthalic anhydride 1.5 parts, m-xylene diamine 0.2 part, N, N-diethyl diethylene triamine 1.5 parts, resol reworked material 0.5 part, 2-ethyl-4-methylimidazole 1 part, butyl epoxy stearate 2 parts, tributyl acetylcitrate 5 parts, tetramethylolmethane 2 parts, micro encapsulation ammonium polyphosphate 15 parts, carbon nano fiber 3 parts, nano-calcium carbonate 10 parts, recycled polyethylene 3 parts, Epoxy-Terminated Polydimethylsiloxane 10 parts, bisphenol A-type bi-phthalonitrile 3 parts, Diphenylsilanediol 20 parts, stannous octoate 1 part.
Embodiment 2
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 35 parts, methyl hexahydrophthalic anhydride 0.5 part, m-xylene diamine 1 part, N, N-diethyl diethylene triamine 0.3 part, resol reworked material 1.5 parts, 2-ethyl-4-methylimidazole 0.2 part, butyl epoxy stearate 8 parts, tributyl acetylcitrate 1 part, tetramethylolmethane 6 parts, micro encapsulation ammonium polyphosphate 5 parts, carbon nano fiber 10 parts, nano-calcium carbonate 3 parts, recycled polyethylene 10 parts, Epoxy-Terminated Polydimethylsiloxane 2 parts, bisphenol A-type bi-phthalonitrile 10 parts, Diphenylsilanediol 10 parts, stannous octoate 2.5 parts,
Wherein, described epoxy resin is that bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin are by weight the mixture for 1:7:1;
In described epoxy terminated paracril, oxirane value is 0.08%, and acrylonitrile content is 20%;
The mean diameter of described carbon nano fiber is 100nm, and tensile strength is 3GPa, and density is 2g/cm
3, thermal conductivity is 1000W/mk; The median size of described nano-calcium carbonate is 50nm.
Embodiment 3
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 30 parts, methyl hexahydrophthalic anhydride 1.1 parts, m-xylene diamine 0.85 part, N, N-diethyl diethylene triamine 1.1 parts, resol reworked material 1 part, 2-ethyl-4-methylimidazole 0.7 part, butyl epoxy stearate 5.8 parts, tributyl acetylcitrate 3.7 parts, tetramethylolmethane 4.9 parts, micro encapsulation ammonium polyphosphate 9 parts, carbon nano fiber 7.6 parts, nano-calcium carbonate 7.8 parts, recycled polyethylene 6 parts, Epoxy-Terminated Polydimethylsiloxane 6.2 parts, bisphenol A-type bi-phthalonitrile 6.9 parts, Diphenylsilanediol 15 parts, stannous octoate 2 parts,
Wherein, described epoxy resin is that bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin are by weight the mixture for 5:2:3;
In described epoxy terminated paracril, oxirane value is 0.15%, and acrylonitrile content is 15%;
The mean diameter of described carbon nano fiber is 60nm, and tensile strength is 6GPa, and density is 1.5g/cm
3, thermal conductivity is 1300W/mk; The median size of described nano-calcium carbonate is 30nm.
Embodiment 4
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 32 parts, methyl hexahydrophthalic anhydride 1 part, m-xylene diamine 0.9 part, N, N-diethyl diethylene triamine 1 part, resol reworked material 1.2 parts, 2-ethyl-4-methylimidazole 0.6 part, butyl epoxy stearate 6.5 parts, tributyl acetylcitrate 3.2 parts, tetramethylolmethane 5 parts, micro encapsulation ammonium polyphosphate 8 parts, carbon nano fiber 8.5 parts, nano-calcium carbonate 7 parts, recycled polyethylene 7 parts, Epoxy-Terminated Polydimethylsiloxane 5 parts, bisphenol A-type bi-phthalonitrile 7 parts, Diphenylsilanediol 13 parts, stannous octoate 2.2 parts,
Wherein, described epoxy resin is that bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin are by weight the mixture for 3:5:2.
Embodiment 5
The special heat-resistance epoxy resin environment-friendly materials of a kind of printed circuit board (PCB) that the present invention proposes, its raw material comprises following component by weight: bisphenol A type epoxy resin 100 parts, epoxy terminated paracril 28 parts, methyl hexahydrophthalic anhydride 1.2 parts, m-xylene diamine 0.7 part, N, N-diethyl diethylene triamine 1.2 parts, resol reworked material 0.9 part, 2-ethyl-4-methylimidazole 0.8 part, butyl epoxy stearate 5 parts, tributyl acetylcitrate 4 parts, tetramethylolmethane 4.8 parts, micro encapsulation ammonium polyphosphate 10 parts, carbon nano fiber 7 parts, nano-calcium carbonate 8 parts, recycled polyethylene 5 parts, Epoxy-Terminated Polydimethylsiloxane 6.5 parts, bisphenol A-type bi-phthalonitrile 6.8 parts, Diphenylsilanediol 17 parts, stannous octoate 1.7 parts,
Wherein, in described epoxy terminated paracril, oxirane value is 0.12%, and acrylonitrile content is 17%;
The mean diameter of described carbon nano fiber is 80nm, and tensile strength is 5GPa, and density is 1.7g/cm
3, thermal conductivity is 1200W/mk; The median size of described nano-calcium carbonate is 45nm.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (9)
1. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB), it is characterized in that, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 20-35 part, methyl hexahydrophthalic anhydride 0.5-1.5 part, m-xylene diamine 0.2-1 part, N, N-diethyl diethylene triamine 0.3-1.5 part, resol reworked material 0.5-1.5 part, 2-ethyl-4-methylimidazole 0.2-1 part, butyl epoxy stearate 2-8 part, tributyl acetylcitrate 1-5 part, tetramethylolmethane 2-6 part, micro encapsulation ammonium polyphosphate 5-15 part, carbon nano fiber 3-10 part, nano-calcium carbonate 3-10 part, recycled polyethylene 3-10 part, Epoxy-Terminated Polydimethylsiloxane 2-10 part, bisphenol A-type bi-phthalonitrile 3-10 part, Diphenylsilanediol 10-20 part, stannous octoate 1-2.5 part.
2. special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to claim 1, it is characterized in that, the weight ratio of methyl hexahydrophthalic anhydride, m-xylene diamine, N, N-diethyl diethylene triamine, resol reworked material, 2-ethyl-4-methylimidazole is 0.8-1.3:0.5-1:0.7-1.3:0.7-1.3:0.4-1.
3. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to claim 1 or 2, is characterized in that, the weight ratio of tetramethylolmethane, micro encapsulation ammonium polyphosphate, bisphenol A-type bi-phthalonitrile is 4.5-5.2:8-12:6.5-7.2.
4. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-3, it is characterized in that, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 28-32 part, methyl hexahydrophthalic anhydride 1-1.2 part, m-xylene diamine 0.7-0.9 part, N, N-diethyl diethylene triamine 1-1.2 part, resol reworked material 0.9-1.2 part, 2-ethyl-4-methylimidazole 0.6-0.8 part, butyl epoxy stearate 5-6.5 part, tributyl acetylcitrate 3.2-4 part, tetramethylolmethane 4.8-5 part, micro encapsulation ammonium polyphosphate 8-10 part, carbon nano fiber 7-8.5 part, nano-calcium carbonate 7-8 part, recycled polyethylene 5-7 part, Epoxy-Terminated Polydimethylsiloxane 5-6.5 part, bisphenol A-type bi-phthalonitrile 6.8-7 part, Diphenylsilanediol 13-17 part, stannous octoate 1.7-2.2 part.
5. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-4, it is characterized in that, its raw material comprises following component by weight: epoxy resin 100 parts, epoxy terminated paracril 30 parts, methyl hexahydrophthalic anhydride 1.1 parts, m-xylene diamine 0.85 part, N, N-diethyl diethylene triamine 1.1 parts, resol reworked material 1 part, 2-ethyl-4-methylimidazole 0.7 part, butyl epoxy stearate 5.8 parts, tributyl acetylcitrate 3.7 parts, tetramethylolmethane 4.9 parts, micro encapsulation ammonium polyphosphate 9 parts, carbon nano fiber 7.6 parts, nano-calcium carbonate 7.8 parts, recycled polyethylene 6 parts, Epoxy-Terminated Polydimethylsiloxane 6.2 parts, bisphenol A-type bi-phthalonitrile 6.9 parts, Diphenylsilanediol 15 parts, stannous octoate 2 parts.
6. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-5, it is characterized in that, described epoxy resin is one or more the mixture in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin.
7. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-6, it is characterized in that, described epoxy resin is that bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-A epoxy resin are by weight the mixture for 1-5:2-7:1-3.
8. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-7, is characterized in that, in described epoxy terminated paracril, oxirane value is 0.08-0.15%, and acrylonitrile content is 15-20%.
9. the special heat-resistance epoxy resin environment-friendly materials of printed circuit board (PCB) according to any one of claim 1-8, is characterized in that, the mean diameter of described carbon nano fiber is 60-100nm, and tensile strength is 3-6GPa, and density is 1.5-2g/cm
3, thermal conductivity is 1000-1300W/mk; The median size of described nano-calcium carbonate is 30-50nm.
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| CN201510780516.7A CN105348734A (en) | 2015-11-13 | 2015-11-13 | An environmental-friendly heat-resistant epoxy resin material specially used for printed circuit boards |
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| CN201510780516.7A CN105348734A (en) | 2015-11-13 | 2015-11-13 | An environmental-friendly heat-resistant epoxy resin material specially used for printed circuit boards |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108003411A (en) * | 2017-12-21 | 2018-05-08 | 扬州市金鑫电缆有限公司 | Can be into porcelain low-smoke halogen-free polyolefin cable material and preparation method thereof |
| US10640598B2 (en) | 2016-03-31 | 2020-05-05 | 3M Innovative Properties Company | Resin blends of resorcinol diphthalonitrile ether with bisphenol M diphthalonitrile ether and/or bisphenol T diphthalonitrile ether |
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| CN101654605A (en) * | 2008-08-21 | 2010-02-24 | 中山市东溢新材料有限公司 | Modified epoxy resin adhesive and preparation method thereof |
| CN102492140A (en) * | 2011-11-18 | 2012-06-13 | 电子科技大学 | Bi-phthalonitrile prepolymer as well as preparation method and application thereof, bi-phthalonitrile prepolymer/epoxy resin copolymer and preparation method thereof as well as bi-phthalonitrile prepolymer/epoxy resin cured material |
| CN104311794A (en) * | 2014-10-23 | 2015-01-28 | 卢儒 | Organosilicone modified epoxy resin and preparation method thereof as well as mica capacitor |
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2015
- 2015-11-13 CN CN201510780516.7A patent/CN105348734A/en active Pending
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| CN101654605A (en) * | 2008-08-21 | 2010-02-24 | 中山市东溢新材料有限公司 | Modified epoxy resin adhesive and preparation method thereof |
| CN102492140A (en) * | 2011-11-18 | 2012-06-13 | 电子科技大学 | Bi-phthalonitrile prepolymer as well as preparation method and application thereof, bi-phthalonitrile prepolymer/epoxy resin copolymer and preparation method thereof as well as bi-phthalonitrile prepolymer/epoxy resin cured material |
| CN104311794A (en) * | 2014-10-23 | 2015-01-28 | 卢儒 | Organosilicone modified epoxy resin and preparation method thereof as well as mica capacitor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10640598B2 (en) | 2016-03-31 | 2020-05-05 | 3M Innovative Properties Company | Resin blends of resorcinol diphthalonitrile ether with bisphenol M diphthalonitrile ether and/or bisphenol T diphthalonitrile ether |
| US10899865B2 (en) | 2016-03-31 | 2021-01-26 | 3M Innovative Properties Company | Bisphenol M diphthalonitrile ether resin blends including a filler, and articles |
| US11401364B2 (en) | 2016-03-31 | 2022-08-02 | 3M Innovative Properties Company | Bisphenol M diphthalonitrile ether resin, bisphenol P diphthalonitrile ether resin, methods of making same, resin blends, and two component systems |
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