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Heat-resistant flame-proof phosphorus- and silicon-containing hybrid curing agent for epoxy type electronic polymer material and preparation thereof

A polymer material, epoxy-based technology, applied in the field of polymer materials, can solve the problems of thermal and mechanical properties of epoxy resins, and achieve excellent mechanical properties

Inactive Publication Date: 2008-10-01
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on the principle of the relationship between polymer structure and performance, although phosphorus-containing or silicon-containing epoxy resins have better flame-retardant effects than ordinary epoxy resins, they often reduce the thermal and mechanical properties of epoxy resins.

Method used

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  • Heat-resistant flame-proof phosphorus- and silicon-containing hybrid curing agent for epoxy type electronic polymer material and preparation thereof
  • Heat-resistant flame-proof phosphorus- and silicon-containing hybrid curing agent for epoxy type electronic polymer material and preparation thereof
  • Heat-resistant flame-proof phosphorus- and silicon-containing hybrid curing agent for epoxy type electronic polymer material and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 100g of glycidoxybutyltrimethoxysilane, 20g of diethyl phosphite, 0.6g of dibutyltin dilaurate and 80g of butyl ether solvent into a three-necked flask, and reflux at 50°C for 10h. A hybrid epoxy compound containing silicon and phosphorus is obtained. Then add 20g of anilinomethyltriethoxysilane, add 50g of deionized water dropwise under stirring at 30°C, complete the dropwise addition in 30min, react under reflux for 8h, remove the solvent and small molecules by rotary evaporation to obtain phosphorus-containing silicon Heat-resistant hybrid epoxy curing agent.

[0034] Take 20g of heat-resistant hybrid epoxy resin and 100g of F51 type epoxy resin to compound, and then use 12.15g of triethylenetetramine to cure. The limiting oxygen index of the cured product is 29.2, the tensile strength is 43.4MPa, and the glass transition temperature is 167°C.

Embodiment 2

[0036]Add 100g of glycidoxypropyl dimethoxysilane, 40g of diethyl phosphate, 0.7g of triethylamine catalyst and 120g of toluene solvent into a three-necked flask, and reflux at 60°C for 8h to obtain hybrid epoxy compounds. Then add 40g of anilinomethyltriethoxysilane, add 60g of deionized water dropwise under stirring at 40°C, complete the dropwise addition in 20min, react under reflux for 6h, remove the solvent and small molecules by rotary evaporation to obtain phosphorus-containing silicon Heat-resistant hybrid epoxy curing agent.

[0037] Take 20g of heat-resistant hybrid epoxy resin and 100g of E51 type epoxy resin to compound, and then use 30.47g of diaminodiphenyl sulfone to cure. The limiting oxygen index of the cured product is 28.0, the tensile strength is 45.0MPa, and the glass transition temperature is 185°C.

Embodiment 3

[0039] Add 100g of glycidoxypropyltriethoxysilane, 50g of diethyl phosphite, 0.75g of dibutyltin dilaurate catalyst and 50g of tetrahydrofuran solvent into a three-necked flask, and reflux at 70°C for 5h , to obtain hybrid epoxy compounds containing silicon and phosphorus. Then add 75g of γ-aminopropyltriethoxysilane, add 70g of deionized water dropwise under stirring at 50°C, complete the dropwise addition in 30 minutes, react for 4 hours under reflux, and remove the solvent and small molecules by rotary evaporation to obtain phosphorus-containing Silicone based heat resistant hybrid epoxy curing agent.

[0040] Take 20g of the above-mentioned heat-resistant hybrid epoxy curing agent and compound it with 100g of E44 epoxy resin, and then use 25.12g of diaminodiphenyl sulfone to cure. The limiting oxygen index of the cured product is 27.5, the tensile strength is 44.2MPa, and the glass transition temperature is 178°C.

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Abstract

The invention pertains to the field of polymeric material and relates to an epoxy phosphorus-containing hybridization hardener with heat resistance and flame retardancy for electron polymer material and a preparation method thereof. The phosphorus-containing hybridization hardener is nanometer-sized organic / inorganic hybrid silicone of a hollow enclosed type or a partially enclosed type, wherein, the structure center of the silicone consists of inorganic skeleton Si-O bonds; the external end of the structure center consists of organic groups of organic phosphor or amidogen or imidogen and has a number average molecular weight of 600 to 10000 and the structural formula is as above, wherein, R< / > can be hydrogen, cymene, ethyl, n-propyl, isopropyl or butyl; X is organic containing phosphorus substituent ; Y is organic amino-containing substituent. The samples prepared with epoxy resin hardened by the hardener not only have a very good flame retardant performance, but also maintain good heat resistant and mechanical property, thus meeting the requirements for heat resistance and flame retardancy and mechanical aspects of the epoxy resin used for the electronic substrate material with high performance.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a phosphorus-containing silicon hybrid curing agent for heat-resistant and flame-retardant epoxy-type electronic polymer materials and a preparation method thereof. Background technique [0002] The electronics industry represented by electronic computers and mobile phones is the fastest-growing high-tech industry in the past two decades. The rapid development of the electronics industry has also led to the development of thermosetting resins that are closely related to it. Thermosetting resins are used in all electronics industries. In the field of resin materials, the epoxy resin system is the largest due to its superior performance and low cost, accounting for more than 40%. It is widely used in the manufacture of printed circuit boards and the packaging of semiconductors and electronic devices. A very important polymer material. [0003] With the emergence of adv...

Claims

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Application Information

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IPC IPC(8): C08K5/544C08L63/00
Inventor 刘伟区于丹刘云峰
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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