CN105237950A - Environmental-friendly halogen-free flame-retardant epoxy resin used for copper-clad plates, and preparation method thereof - Google Patents
Environmental-friendly halogen-free flame-retardant epoxy resin used for copper-clad plates, and preparation method thereof Download PDFInfo
- Publication number
- CN105237950A CN105237950A CN201510615526.5A CN201510615526A CN105237950A CN 105237950 A CN105237950 A CN 105237950A CN 201510615526 A CN201510615526 A CN 201510615526A CN 105237950 A CN105237950 A CN 105237950A
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- China
- Prior art keywords
- parts
- epoxy resin
- copper
- bisphenol
- friendly halogen
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 55
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000003063 flame retardant Substances 0.000 title abstract description 12
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title abstract description 7
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims abstract description 21
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007822 coupling agent Substances 0.000 claims abstract description 16
- -1 polyoxy Polymers 0.000 claims abstract description 15
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 14
- HGQSXVKHVMGQRG-UHFFFAOYSA-N dioctyltin Chemical compound CCCCCCCC[Sn]CCCCCCCC HGQSXVKHVMGQRG-UHFFFAOYSA-N 0.000 claims abstract description 14
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 14
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 39
- 229930185605 Bisphenol Natural products 0.000 claims description 13
- JWQMZGJKIAJVFE-UHFFFAOYSA-L azanium copper phosphate Chemical compound [NH4+].[Cu+2].[O-]P([O-])([O-])=O JWQMZGJKIAJVFE-UHFFFAOYSA-L 0.000 claims description 13
- 150000004985 diamines Chemical class 0.000 claims description 13
- 229920001451 polypropylene glycol Polymers 0.000 claims description 13
- 238000010792 warming Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract 1
- 239000000440 bentonite Substances 0.000 abstract 1
- 229910000278 bentonite Inorganic materials 0.000 abstract 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 abstract 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 abstract 1
- GQDHEYWVLBJKBA-UHFFFAOYSA-H copper(ii) phosphate Chemical compound [Cu+2].[Cu+2].[Cu+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GQDHEYWVLBJKBA-UHFFFAOYSA-H 0.000 abstract 1
- 229920005610 lignin Polymers 0.000 abstract 1
- 229910052736 halogen Inorganic materials 0.000 description 4
- 239000012776 electronic material Substances 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 101150051314 tin-10 gene Proteins 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses an environmental-friendly halogen-free flame-retardant epoxy resin used for copper-clad plates. The environmental-friendly halogen-free flame-retardant epoxy resin is prepared from bisphenol-F epoxy resin, bisphenol-A epoxy resin, polyoxy propylidene diamine, ammonium cupric phosphate, talcum powder, bentonite, dioctyltin, sodium dodecyl sulfonate, zinc borate, lignin, and a coupling agent. The invention also discloses a preparation method of the environmental-friendly halogen-free flame-retardant epoxy resin. The environmental-friendly halogen-free flame-retardant epoxy resin possesses excellent flame resistance and peel strength, and relatively low dielectric loss and thermal expansion coefficient, and is suitable to be used for preparing copper-clad plates; the raw materials are easily available; the preparation method is simple; and it is convenient for popularization and application.
Description
Technical field
The invention belongs to field of electronic materials, particularly a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin and preparation method thereof.
Background technology
In field of electronic materials, the metal in copper-clad plate and glass-fiber-fabric base material are all nonflammable, but the epoxy resin film adopted in copper-clad plate very easily fires.If during the problems such as electronic material is short-circuited, the inflammable epoxy resin in copper-clad plate can burning at once, not only can damage equipment, also can cause fire time serious.Usually, in order to reduce the incendivity of epoxy resin, various fire retardant can be added, but the fire retardant added on the market mostly is halogen-containing, not only not environmental protection, in addition, if temperature is too high, these halogen-containing fire retardants also can burn, and halogen-containing fire retardant burning can discharge a large amount of harmful and noxious substances, healthy to human body of serious threat, brings various potential safety hazard, is unfavorable for actual use.
Summary of the invention
The technical problem solved is: very easily burn to solve copper-clad plate epoxy resin material, and the fire retardant added mostly is problems such as the halogen-containing organism of human body and bad environmental, provide a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin and preparation method thereof.
Technical scheme: in order to solve the problem, the invention provides a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin, be prepared from by each component following: bisphenol f type epoxy resin, bisphenol A type epoxy resin, polyoxypropylene diamine, ammonium phosphate copper, talcum powder, wilkinite, dioctyl tin, sodium laurylsulfonate, zinc borate, xylogen and coupling agent.
Preferably, described component is counted by weight: bisphenol f type epoxy resin 48 ~ 70 parts, bisphenol A type epoxy resin 55 ~ 80 parts, polyoxypropylene diamine 32 ~ 62 parts, ammonium phosphate copper 12 ~ 30 parts, talcum powder 3 ~ 18 parts, wilkinite 3 ~ 12 parts, dioctyl tin 2 ~ 10 parts, sodium laurylsulfonate 2 ~ 8 parts, zinc borate 1 ~ 12 part, 3 ~ 14 parts, xylogen and coupling agent 0.5 ~ 2 part.
Preferably, described component is counted by weight: bisphenol f type epoxy resin 48 ~ 65 parts, bisphenol A type epoxy resin 55 ~ 78 parts, polyoxypropylene diamine 32 ~ 56 parts, ammonium phosphate copper 14 ~ 30 parts, talcum powder 5 ~ 18 parts, wilkinite 5 ~ 12 parts, dioctyl tin 4 ~ 10 parts, sodium laurylsulfonate 3 ~ 8 parts, zinc borate 3 ~ 12 parts, 3 ~ 12 parts, xylogen and coupling agent 0.5 ~ 1 part.
Preferably, described component is counted by weight: bisphenol f type epoxy resin 60 parts, bisphenol A type epoxy resin 72 parts, polyoxypropylene diamine 45 parts, ammonium phosphate copper 18 parts, talcum powder 7 parts, wilkinite 7 parts, dioctyl tin 5 parts, sodium laurylsulfonate 4 parts, zinc borate 6 parts, 7 parts, xylogen and coupling agent 0.6 part.
Preferably, described coupling agent is KH-550 or KH-570.
The preparation method of a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin described above, preparation process is as follows:
(1) each component is weighed according to certainweight number;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 80 DEG C ~ 120 DEG C, be uniformly mixed 30min ~ 80min;
(3) remaining component is added in reactor, continues stirring 2 ~ 10h.
Preferably, described step is warming up to 90 DEG C in (2), is uniformly mixed 50min.
The present invention has following beneficial effect: a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin prepared by the present invention, not only there is good flame retardant resistance, also there is preferably stripping strength, lower dielectric loss and thermal expansivity simultaneously, be applicable to very much being applied to processing and fabricating copper-clad plate; In addition, in preparation process, raw materials is easy to get and preparation technology is easy, also conveniently applies.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, invention preferred embodiment is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
A preparation method for copper-clad plate environment friendly halogen-free fireproof epoxy resin, preparation process is as follows:
(1) each component is weighed according to certainweight number: bisphenol f type epoxy resin 48 parts, bisphenol A type epoxy resin 55 parts, polyoxypropylene diamine 32 parts, ammonium phosphate copper 12 parts, talcum powder 3 parts, wilkinite 3 parts, dioctyl tin 2 parts, sodium laurylsulfonate 2 parts, zinc borate 1 part, 3 parts, xylogen and coupling agent KH-5500.5 part;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 80 DEG C, be uniformly mixed 30min;
(3) remaining component is added in reactor, continues to stir 2h.
Embodiment 2
A preparation method for copper-clad plate environment friendly halogen-free fireproof epoxy resin, preparation process is as follows:
(1) each component is weighed according to certainweight number: bisphenol f type epoxy resin 70 parts, bisphenol A type epoxy resin 80 parts, polyoxypropylene diamine 62 parts, ammonium phosphate copper 30 parts, talcum powder 18 parts, wilkinite 12 parts, dioctyl tin 10 parts, sodium laurylsulfonate 8 parts, zinc borate 12 parts, 14 parts, xylogen and coupling agent kh-570 2 parts;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 120 DEG C, be uniformly mixed 80min;
(3) remaining component is added in reactor, continues to stir 10h.
Embodiment 3
A preparation method for copper-clad plate environment friendly halogen-free fireproof epoxy resin, preparation process is as follows:
(1) each component is weighed according to certainweight number: bisphenol f type epoxy resin 59 parts, bisphenol A type epoxy resin 68 parts, polyoxypropylene diamine 47 parts, ammonium phosphate copper 21 parts, talcum powder 10 parts, wilkinite 7 parts, dioctyl tin 6 parts, sodium laurylsulfonate 5 parts, zinc borate 6 parts, 8 parts, xylogen and coupling agent KH-5501.2 part;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 100 DEG C, be uniformly mixed 55min;
(3) remaining component is added in reactor, continues to stir 6h.
Embodiment 4
A preparation method for copper-clad plate environment friendly halogen-free fireproof epoxy resin, preparation process is as follows:
(1) each component is weighed according to certainweight number: bisphenol f type epoxy resin 65 parts, bisphenol A type epoxy resin 78 parts, polyoxypropylene diamine 56 parts, ammonium phosphate copper 14 parts, talcum powder 5 parts, wilkinite 5 parts, dioctyl tin 4 parts, sodium laurylsulfonate 3 parts, zinc borate 3 parts, 12 parts, xylogen and coupling agent kh-570 1 part;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 100 DEG C, be uniformly mixed 80min;
(3) remaining component is added in reactor, continues to stir 10h.
Embodiment 5
A preparation method for copper-clad plate environment friendly halogen-free fireproof epoxy resin, preparation process is as follows:
(1) each component is weighed according to certainweight number: bisphenol f type epoxy resin 60 parts, bisphenol A type epoxy resin 72 parts, polyoxypropylene diamine 45 parts, ammonium phosphate copper 18 parts, talcum powder 7 parts, wilkinite 7 parts, dioctyl tin 5 parts, sodium laurylsulfonate 4 parts, zinc borate 6 parts, 7 parts, xylogen and coupling agent 0.6 part;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 90 DEG C, be uniformly mixed 50min;
(3) remaining component is added in reactor, continues to stir 8h.
Carry out performance test to embodiment 1 ~ 5 below, conveniently comparison, compares as a comparison case with ordinary epoxy resin, specifically sees the following form:
From above-mentioned experimental result, the epoxide resin material prepared by the present invention has good flame retardant resistance, also has preferably stripping strength, lower dielectric loss and thermal expansivity simultaneously, is applicable to being applied to processing and fabricating copper-clad plate, has a extensive future.
Claims (7)
1. a copper-clad plate environment friendly halogen-free fireproof epoxy resin, it is characterized in that, be prepared from by each component following: bisphenol f type epoxy resin, bisphenol A type epoxy resin, polyoxypropylene diamine, ammonium phosphate copper, talcum powder, wilkinite, dioctyl tin, sodium laurylsulfonate, zinc borate, xylogen and coupling agent.
2. a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to claim 1, it is characterized in that, described component is counted by weight: bisphenol f type epoxy resin 48 ~ 70 parts, bisphenol A type epoxy resin 55 ~ 80 parts, polyoxypropylene diamine 32 ~ 62 parts, ammonium phosphate copper 12 ~ 30 parts, talcum powder 3 ~ 18 parts, wilkinite 3 ~ 12 parts, dioctyl tin 2 ~ 10 parts, sodium laurylsulfonate 2 ~ 8 parts, zinc borate 1 ~ 12 part, 3 ~ 14 parts, xylogen and coupling agent 0.5 ~ 2 part.
3. a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to claim 1, it is characterized in that, described component is counted by weight: bisphenol f type epoxy resin 48 ~ 65 parts, bisphenol A type epoxy resin 55 ~ 78 parts, polyoxypropylene diamine 32 ~ 56 parts, ammonium phosphate copper 14 ~ 30 parts, talcum powder 5 ~ 18 parts, wilkinite 5 ~ 12 parts, dioctyl tin 4 ~ 10 parts, sodium laurylsulfonate 3 ~ 8 parts, zinc borate 3 ~ 12 parts, 3 ~ 12 parts, xylogen and coupling agent 0.5 ~ 1 part.
4. a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to claim 1, it is characterized in that, described component is counted by weight: bisphenol f type epoxy resin 60 parts, bisphenol A type epoxy resin 72 parts, polyoxypropylene diamine 45 parts, ammonium phosphate copper 18 parts, talcum powder 7 parts, wilkinite 7 parts, dioctyl tin 5 parts, sodium laurylsulfonate 4 parts, zinc borate 6 parts, 7 parts, xylogen and coupling agent 0.6 part.
5. a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to claim 1, it is characterized in that, described coupling agent is KH-550 or KH-570.
6. a preparation method for a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to any one of claim 1 ~ 5, it is characterized in that, preparation process is as follows:
(1) each component is weighed according to certainweight number;
(2) sodium laurylsulfonate in component, zinc borate and xylogen are added in reactor, be warming up to 80 DEG C ~ 120 DEG C, be uniformly mixed 30min ~ 80min;
(3) remaining component is added in reactor, continues stirring 2 ~ 10h.
7. the preparation method of a kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin according to claim 6, it is characterized in that, described step is warming up to 90 DEG C in (2), is uniformly mixed 50min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615526.5A CN105237950B (en) | 2015-09-24 | 2015-09-24 | A kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510615526.5A CN105237950B (en) | 2015-09-24 | 2015-09-24 | A kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin and preparation method thereof |
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| Publication Number | Publication Date |
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| CN105237950A true CN105237950A (en) | 2016-01-13 |
| CN105237950B CN105237950B (en) | 2017-11-28 |
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| CN201510615526.5A Expired - Fee Related CN105237950B (en) | 2015-09-24 | 2015-09-24 | A kind of copper-clad plate environment friendly halogen-free fireproof epoxy resin and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111424294A (en) * | 2020-05-15 | 2020-07-17 | 惠州联合铜箔电子材料有限公司 | Production process of reverse copper foil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979437A (en) * | 2010-11-16 | 2011-02-23 | 莱芜金鼎电子材料有限公司 | Phosphorus-nitrogen composite expanded composition and preparation method and application thereof |
| CN103435973A (en) * | 2013-09-06 | 2013-12-11 | 苏州生益科技有限公司 | Halogen-free epoxy resin composition as well as prepreg and laminate made from same |
| CN104194271A (en) * | 2014-08-29 | 2014-12-10 | 天津德高化成新材料股份有限公司 | Dielectric composite material for fingerprint sensor induction layer and preparation method thereof |
| CN104449516A (en) * | 2014-12-06 | 2015-03-25 | 赵冯 | Epoxy adhesive |
-
2015
- 2015-09-24 CN CN201510615526.5A patent/CN105237950B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101979437A (en) * | 2010-11-16 | 2011-02-23 | 莱芜金鼎电子材料有限公司 | Phosphorus-nitrogen composite expanded composition and preparation method and application thereof |
| CN103435973A (en) * | 2013-09-06 | 2013-12-11 | 苏州生益科技有限公司 | Halogen-free epoxy resin composition as well as prepreg and laminate made from same |
| CN104194271A (en) * | 2014-08-29 | 2014-12-10 | 天津德高化成新材料股份有限公司 | Dielectric composite material for fingerprint sensor induction layer and preparation method thereof |
| CN104449516A (en) * | 2014-12-06 | 2015-03-25 | 赵冯 | Epoxy adhesive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111424294A (en) * | 2020-05-15 | 2020-07-17 | 惠州联合铜箔电子材料有限公司 | Production process of reverse copper foil |
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| Publication number | Publication date |
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| CN105237950B (en) | 2017-11-28 |
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