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Silicon-phosphor-containing heat-stable hybridized epoxide resin and the preparing method and application thereof

A technology of epoxy resin and phosphorous silicon, which is applied in electrical components, circuits, circuit substrate materials, etc., can solve the problems of the reduction of thermal and mechanical properties of epoxy resin, and achieve excellent heat resistance and mechanical properties, good flame retardancy performance, the effect of improving the flame retardant effect

Inactive Publication Date: 2009-11-18
海南中科翔新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although phosphorus-containing or silicon-containing epoxy resins have a better flame-retardant effect than ordinary epoxy resins, at the same time, the limitations of molecular design and other conditions reduce the thermal and mechanical properties of epoxy resins.

Method used

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  • Silicon-phosphor-containing heat-stable hybridized epoxide resin and the preparing method and application thereof
  • Silicon-phosphor-containing heat-stable hybridized epoxide resin and the preparing method and application thereof
  • Silicon-phosphor-containing heat-stable hybridized epoxide resin and the preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] With the glycidoxybutyl trimethoxysilane of 100g, 0.2g catalyst dibutyl tin laurate (the consumption of catalyst is 0.2% of the glycidoxybutyl trimethoxysilane quality) and 90g butyl ether solvent Add it into a three-necked flask, add 25g of deionized water dropwise under stirring at 60°C, and drop it in 30 minutes. After reacting at 60°C for 6 hours, a silicon-containing hybrid epoxy resin is obtained, and then add 25.7g of diethyl phosphate , Reflux at 150°C for 5 hours, and cool to remove the solvent butyl ether and the by-product methanol to obtain 94.0 g of phosphorus-containing silicon heat-resistant hybrid epoxy resin with a number average molecular weight of 1779.

[0037] Take 30g of the above-mentioned phosphorus-containing silicon heat-resistant hybrid epoxy resin and compound it with 100g of F51 epoxy resin, and then use 19.4g of triethylenetetramine to cure (the specific process conditions are the same as those in the specification, the same below). The lim...

Embodiment 2

[0039] With the glycidoxypropyl methyldimethoxysilane of 100g, 0.01g catalyst triethylamine (the consumption of catalyst is 0.01% of glycidoxypropylmethyldimethoxysilane quality), 60g toluene and Add 60g of benzene mixed solvent into a three-necked flask, add 40g of deionized water dropwise under stirring at 120°C, and finish adding dropwise in 40 minutes. After reacting at 120°C for 2 hours, a silicon-containing epoxy resin is obtained, and then add DOPO19. 6g, reflux reaction at 100°C for 10h, and cooling to remove the solvent toluene, benzene and by-product methanol to obtain 92.6g of phosphorus-containing silicon heat-resistant hybrid epoxy resin with a number average molecular weight of 954.

[0040] Take 20g of the above-mentioned phosphorus-containing silicon heat-resistant hybrid epoxy resin and compound it with 100g of E51 type epoxy resin, and then use 58.4g of polyamide to cure it. The limiting oxygen index of the cured product is 28.0, the tensile strength is 55MPa...

Embodiment 3

[0042] With the glycidoxypropyl methyl diisopropoxysilane of 100g, 0.001g catalyst hydrochloric acid (the consumption of catalyst is 0.001% of glycidoxypropyl methyl diisopropoxysilane quality) and 50g tetrahydrofuran solvent Add it into a three-necked flask, add 10g of deionized water dropwise under stirring at 50°C, and drop it in 60 minutes. After reacting at 50°C for 8 hours, a silicon-containing epoxy resin is obtained, and then add 10g of phosphoric acid and dimethyl phosphate 16.4 g, reflux at 130°C for 5 hours, and cool to remove the solvent tetrahydrofuran and the by-product isopropanol to obtain 74.1 g of phosphorus-containing silicon heat-resistant hybrid epoxy resin with a number average molecular weight of 569.

[0043] Take 25g of the above-mentioned phosphorus-containing silicon heat-resistant hybrid epoxy resin and compound it with 100g of E44 type epoxy resin, and then use 28.5g of diaminodiphenyl sulfone to cure. The limiting oxygen index of the cured product...

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Abstract

The invention discloses a phosphorus-containing silicon heat-resistant hybrid epoxy resin and its preparation method and application. The epoxy resin is prepared according to the following method: in parts by weight, 100 parts of epoxy polyalkylsilane , 50 to 120 parts of organic solvent, mixed with a catalyst accounting for 0.001% to 0.5% of the mass of epoxy polyalkylsilane, and 10 to 40 parts of deionized water were added dropwise to the above mixed solution at 50 to 120 ° C. ~120°C hydrolysis and reflux for 2~8 hours, then add 1~100 parts of phosphorus-containing active substances, and react at 100~160°C for 3~10 hours, remove the organic solvent used for the reaction, and obtain phosphorus-containing silicon heat-resistant hybrid epoxy Resin; its number average molecular weight is 500-6000. After the phosphorus-containing silicon heat-resistant hybrid epoxy resin is cured alone or combined with ordinary epoxy resin, it has excellent mechanical properties, flame retardancy and heat resistance, the tensile strength can reach 43-94Mpa, and the limiting oxygen index can reach 23-38, the glass transition temperature reaches 165-187°C, and can be widely used as a high-performance matrix material for the electronics industry.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a phosphorus-containing silicon heat-resistant hybrid epoxy resin and its preparation method and application. 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 advanced electronic technology, the improvement of heat-resistant and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14C08G59/68H01L23/29H05K1/03
Inventor 刘伟区侯孟华苏倩倩
Owner 海南中科翔新材料科技有限公司
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