CN101450994B - Method for preparing cyanate ester resin prepolymer - Google Patents
Method for preparing cyanate ester resin prepolymer Download PDFInfo
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- CN101450994B CN101450994B CN2007101905237A CN200710190523A CN101450994B CN 101450994 B CN101450994 B CN 101450994B CN 2007101905237 A CN2007101905237 A CN 2007101905237A CN 200710190523 A CN200710190523 A CN 200710190523A CN 101450994 B CN101450994 B CN 101450994B
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- ester resin
- cyanate ester
- bisphenol
- prepolymer
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Abstract
The invention relates to a method for preparing a cyanate ester resin prepolymer and relates to preparation of the cyanate ester resin prepolymer. Bisphenol A-type cyanate ester resin is taken as a raw material and the method comprises the following steps: 1, the solid-state bisphenol A-type cyanate ester resin is put into a prepolymerization reactor, is heated to a temperature of between 140 and150 DEG C, is kept at the temperature for 15 to 20 hours; meanwhile, the mixture is stirred till refractive index is between 1.580 and 1.585; and viscosity is controlled between 350 and 750mpa.s/25 DEG C; 2, the solution prepared in the step one is cooled and is continuously stirred in the cooling period; and 3, when the cooling temperature is between 75 and 85 DEG C, the solution is kept at the temperature; butanone accounting for 20 to 30 percent of weight of the bisphenol A-type cyanate ester resin is added into the solution, is continuously stirred; and when the solution is even, the solution is cooled to a temperature of between 20 and 25 DEG C and is evenly stirred in the cooling period to prepare the cyanate ester resin prepolymer. The cyanate ester resin prepolymer prepared through the method has certain molecular weight, certain viscosity and good fluidity; and the appearance of the prepolymer shows salmon pink liquid. The chemical property and quality standard of the prepolymer are equivalent to solid cyanate ester resin. The method has low processing cost.
Description
Technical field
The present invention relates to a kind of preparation method of cyanate ester resin prepolymer, relate in particular to the preparation method of the good cyanate ester resin prepolymer of a kind of resistance to elevated temperatures.
Background technology
Cyanate ester resin is a kind of novel high-performance thermosetting resin that development in recent years is got up.It has excellent dielectric properties, resistance toheat and mechanical property, is the important foundation material of industries such as aerospace, electronics and information communication, at military, civil area very wide application prospect is arranged all.Cyanate is most widely used in the printed-wiring board (PWB) manufacturing of civil area at present.Developed country end of the eighties such as external U.S., day with regard to development and production be the high-performance printed circuit board of resin matrix with the cyanate, satisfying high frequency microwave (more than the 1GHz) request signal transmission, but this resin and utilisation technology thereof are restricted export; Even allow to introduce, also can supplementary condition and cost an arm and a leg.And the present domestic low and middle-grade printed circuit board of can only producing substantially, lacking high-quality reisn base material is its major cause.
Gel time (the Tgel) 〉=10min (150 ℃) of its pre-polymerization degree control of present cyanate ester resin prepolymer can not adapt to the requirement of some sector applications.
Summary of the invention
The present invention is directed to above problem, provide that a kind of preparation cost is low, the preparation method of the more rational cyanate ester resin prepolymer of gellifying property.
Technical scheme of the present invention is to be raw material with the bisphenol A cyanate ester resin, according to the following steps preparation:
1), solid-state bisphenol A cyanate ester resin is inserted in the prepolymerization reactor, heat, be incubated 15～20 hours, stir therebetween to 140～150 ℃, to refractive index be 1.580～1.585, controlling its viscosity is 350～750mPas/25 ℃;
2), will go up step and make thing cooling, cooling period does not stop to stir;
3), keep this temperature during cooling temperature to 75～85 ℃, add the butanone of bisphenol A cyanate ester resin weight 20～30%, continue to stir, evenly after, cool off again until being cooled to 20～25 ℃, cooling period still evenly stirs again, makes cyanate ester resin prepolymer.
Described butanone weight is 25% of bisphenol A cyanate ester resin weight.
The cyanate ester resin prepolymer that the present invention makes is for having certain molecular weight, necessarily viscosity, and good fluidity, and its outward appearance is shallow clear look liquid, viscosity 350～750mPas (20～25 ℃), gel time (Tgel) 〉=20min (200 ℃).Its chemical property and quality standard are equal to the solid cyanate ester resin.The demand that tooling cost of the present invention is low, physicals adapts to some special industries.In addition, preparation method of the present invention also is applicable to the preparation of Bisphenol F type, tetramethyl-Bisphenol F type, bis-phenol M type cyanate ester resin prepolymer.
Embodiment
Embodiment 1
The present invention is raw material with the bisphenol A cyanate ester resin, according to the following steps preparation:
1), solid-state bisphenol A cyanate ester resin is inserted in the prepolymerization reactor, heat, be incubated 20 hours, stir therebetween to 140 ℃, to refractive index be 1.580, controlling its viscosity is 350mPas/25 ℃;
2), will go up step and make thing cooling, cooling period does not stop to stir;
3), keep this temperature during cooling temperature to 75 ℃, add the butanone of bisphenol A cyanate ester resin weight 20%, continue to stir, evenly after, cool off again until being cooled to 25 ℃, cooling period still evenly stirs again, makes cyanate ester resin prepolymer.
Embodiment 2
The present invention is raw material with the bisphenol A cyanate ester resin, according to the following steps preparation:
1), solid-state bisphenol A cyanate ester resin is inserted in the prepolymerization reactor, heat, be incubated 18 hours, stir therebetween to 145 ℃, to refractive index be 1.583, controlling its viscosity is 550mPas/25 ℃;
2), will go up step and make thing cooling, cooling period does not stop to stir;
3), keep this temperature during cooling temperature to 80 ℃, preferably add the butanone of bisphenol A cyanate ester resin weight 25%, continue to stir, evenly after, cool off again until being cooled to 23 ℃, cooling period still evenly stirs again, makes cyanate ester resin prepolymer.
Embodiment 3
The present invention is raw material with the bisphenol A cyanate ester resin, according to the following steps preparation:
1), solid-state bisphenol A cyanate ester resin is inserted in the prepolymerization reactor, heat, be incubated 15 hours, stir therebetween to 150 ℃, to refractive index be 1.585, controlling its viscosity is 750mpPs/25 ℃;
2), will go up step and make thing cooling, cooling period does not stop to stir;
3), keep this temperature during cooling temperature to 85 ℃, preferably add the butanone of bisphenol A cyanate ester resin weight 30%, continue to stir, evenly after, cool off again until being cooled to 20 ℃, cooling period still evenly stirs again, makes cyanate ester resin prepolymer.
Claims (2)
1. the preparation method of a cyanate ester resin prepolymer is a raw material with the bisphenol A cyanate ester resin, it is characterized in that, according to the following steps preparation:
1), solid-state bisphenol A cyanate ester resin is inserted in the prepolymerization reactor, heat, be incubated 15～20 hours, stir therebetween to 140～150 ℃, to refractive index be 1.580～1.585, controlling its viscosity is 350～750mPas/25 ℃;
2), will go up step and make thing cooling, cooling period does not stop to stir;
3), keep this temperature during cooling temperature to 75～85 ℃, add the butanone of bisphenol A cyanate ester resin weight 20～30%, continue to stir, evenly after, cool off again until being cooled to 20～25 ℃, cooling period still evenly stirs again, makes cyanate ester resin prepolymer.
2. the preparation method of a kind of cyanate ester resin prepolymer according to claim 1 is characterized in that, described butanone weight is 25% of bisphenol A cyanate ester resin weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101905237A CN101450994B (en) | 2007-11-30 | 2007-11-30 | Method for preparing cyanate ester resin prepolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101905237A CN101450994B (en) | 2007-11-30 | 2007-11-30 | Method for preparing cyanate ester resin prepolymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101450994A CN101450994A (en) | 2009-06-10 |
| CN101450994B true CN101450994B (en) | 2011-02-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2007101905237A Expired - Fee Related CN101450994B (en) | 2007-11-30 | 2007-11-30 | Method for preparing cyanate ester resin prepolymer |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199289B (en) * | 2011-04-08 | 2013-01-02 | 扬州天启化学股份有限公司 | Method for preparing tetramethyl bisphenol F type cyanate resin prepolymer |
| CN103145983B (en) * | 2012-06-27 | 2014-10-29 | 天门赋通新材料有限公司 | Preparation method of bisphenol A type cyanate ester resin prepolymer |
| CN102993438B (en) * | 2012-09-20 | 2014-12-24 | 苏州生益科技有限公司 | Bisphenol A-type cyanate ester resin prepolymer and preparation method thereof |
| CN106810691B (en) * | 2015-11-30 | 2019-08-09 | 航天特种材料及工艺技术研究所 | A method of control cyanate ester resin system rheological property |
| TWI798734B (en) * | 2021-06-30 | 2023-04-11 | 南亞塑膠工業股份有限公司 | Thermosetting resin material, prepreg, and metal substrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312887A (en) * | 1992-12-09 | 1994-05-17 | International Business Machines Corporation | Dicyanate prepolymers, use and preparation thereof |
| CN1629137A (en) * | 2003-12-19 | 2005-06-22 | 上虞市盛达生物化工有限公司 | Method for preparing bisphenol A cyanate |
| CN1861374A (en) * | 2005-05-10 | 2006-11-15 | 西北工业大学 | Mehtod for preparing composite material contg. nano-silicon dioxide, polyurethane and cyanate resin |
-
2007
- 2007-11-30 CN CN2007101905237A patent/CN101450994B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312887A (en) * | 1992-12-09 | 1994-05-17 | International Business Machines Corporation | Dicyanate prepolymers, use and preparation thereof |
| CN1629137A (en) * | 2003-12-19 | 2005-06-22 | 上虞市盛达生物化工有限公司 | Method for preparing bisphenol A cyanate |
| CN1861374A (en) * | 2005-05-10 | 2006-11-15 | 西北工业大学 | Mehtod for preparing composite material contg. nano-silicon dioxide, polyurethane and cyanate resin |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2000-191776A 2000.07.11 |
| 王汝敏，陈立新，张双存，杨黎."双酚A二氰酸酯树脂的固化特性研究".《玻璃钢学会第十五届全国玻璃钢/复合材料学术年会论文集》.2003,61-67. |
| 王汝敏,陈立新,张双存,杨黎."双酚A二氰酸酯树脂的固化特性研究".《玻璃钢学会第十五届全国玻璃钢/复合材料学术年会论文集》.2003,61-67. * |
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| CN101450994A (en) | 2009-06-10 |
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