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Halogen-free flame-retardant prepolymer and prepreg and laminated board made from same

A prepreg and prepolymer technology, which is applied in the fields of integrated circuit packaging, electronic materials, high-frequency, high-speed and high-density interconnection, can solve the problems of failing to reach UL94V-0 level, high flame retardant effect, low phosphorus content, etc., and achieve Excellent moisture and heat resistance and heat resistance and low thermal expansion coefficient, excellent moisture and heat resistance and heat resistance, the effect of low thermal expansion coefficient

Active Publication Date: 2013-09-18
SHENGYI TECH SUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are mainly two methods to solve the halogen-free flame retardancy of cyanate resin and its system: (1) Adding inorganic fillers directly into the resin matrix, such as aluminum hydroxide, magnesium hydroxide and other inorganic compounds containing crystal water; Although this method can improve the flame retardancy of the cyanate ester resin system to a certain extent, due to its low flame retardancy efficiency, a large amount of filling is required to reach the UL94V-0 level, and there is a problem of interfacial bonding, so it deteriorates Mechanical properties of cyanate resin; (2) Intrinsic flame retardancy, that is, the introduction of flame retardant groups on the skeleton of cyanate resin; Effectiveness and main direction of cyanate resin
For example, Japanese patent (publication number: 2003-128785) uses 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (referred to as DOPO-HQ ) into the cyanate resin skeleton, however, due to the low phosphorus content in the synthesized product (maximum 1.5%), it cannot reach the UL94V-0 level, and in order to achieve the UL94V-0 level, it is necessary to add phosphorus-containing epoxy resin and Epoxy resins with intrinsic flame retardancy (such as biphenyl resins), which in turn lead to the deterioration of the excellent performance of cyanate ester resins

Method used

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  • Halogen-free flame-retardant prepolymer and prepreg and laminated board made from same
  • Halogen-free flame-retardant prepolymer and prepreg and laminated board made from same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 160g of bisphenol A dicyanate resin monomer, 20g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (hereinafter referred to as DOPO), 10-(2,5-di Hydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (hereinafter referred to as DOPO-HQ) 18g and 10-(2,5-dicarboxypropyl)-9,10 - Put 2 g of dihydro-9-oxo-10-phosphaphenanthrene-10-oxide (hereinafter referred to as DDP) into the reaction bottle, slowly heat it to 140°C in an oil bath, and keep stirring for 6 hours , and cooled to room temperature after the reaction was complete.

Embodiment 2

[0029] Take 130g of tetramethylbisphenol F cyanate resin monomer, 40g of DOPO, 20g of DOPO-HQ and 10g of DDP into the reaction bottle, slowly heat to 130°C with an oil bath, and keep stirring for 12 hours. After the reaction is completed Cool to room temperature.

Embodiment 3

[0031] Take 150g of bisphenol A dicyanate resin monomer, 30g of DOPO, 14g of DOPO-HQ and 6g of DDP into the reaction bottle, slowly heat up to 120°C with an oil bath, and keep stirring for 12 hours. After the reaction is completed, cool to room temperature.

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Abstract

The invention discloses a halogen-free flame-retardant prepolymer which is prepared according to a method comprising the following steps of: heating a phosphorus-containing mixture and a cyanate resin monomer to 100-150 DEG C; reacting for 2-12 hours under the condition of keeping stirring; and cooling to room temperature to obtain the halogen-free flame-retardant prepolymer. The phosphorus-containing mixture: the cyanate resin monomer is equal to (15-65):(20-80) in parts by weight; the phosphorus-containing mixture comprises DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), DOPO-HQ (10-(2,5-dihydroxyphenyl)-9,10-dihydro-9-xa-10-phosphaphenanthrene-10-oxide) and DDP(10-(2,5-dicarboxylpropyl)9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide); and the weight ratio of DOPO to DOPO-HQ to DDP is (20-85): (15-65): (0-20). The novel halogen-free flame-retardant prepolymer disclosed by the invention has good technology capability and can realize the halogen-free flame retardance, achieve excellent wet-heat resistance and heat resistance and low heat expansion coefficient and meet the requirements of a base material of a high-property printed wiring board.

Description

technical field [0001] The invention belongs to the technical field of electronic materials, and relates to a halogen-free flame-retardant prepolymer and a prepreg and a laminate made of the same, which can be applied to the fields of integrated circuit packaging, high-frequency, high-speed and high-density interconnection, and the like. Background technique [0002] As one of the high-performance resin matrices, cyanate resin is widely used in aerospace, aviation and other fields due to its excellent dielectric properties, heat resistance, high glass transition temperature and low water absorption. . However, the current disadvantage of cyanate ester resin is its poor flame retardancy (UL94V-2 grade), and when it is used in electronics and other fields, its flame retardancy must meet the requirements of UL94V-0 grade. Therefore, it is necessary to improve the flame retardancy of cyanate resins. [0003] In recent years, due to strict laws, regulations and environmental pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08G79/04B32B27/04B32B15/08B32B37/06B32B37/10
Inventor 谌香秀季立富戴善凯肖升高崔春梅顾嫒娟粱国正
Owner SHENGYI TECH SUZHOU