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Organic silicon fibre retardant containing phosphorus and epoxy radical and its preparation method

A silicone and flame retardant technology, applied in the field of flame retardants, can solve the problems of thermal and mechanical properties of epoxy resins, and achieve high glass transition temperature and good flame retardant performance

Inactive Publication Date: 2006-01-25
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

Although phosphorus-containing or silicon-containing epoxy resins have better flame retardant effects than ordinary epoxy resins, at the same time the thermal and mechanical properties of epoxy resins are reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]100g of methyl hydrogen-containing silicone oil (hydrogen content of 0.1%) and 1g of allyl glycidyl ether were added to a three-necked flask, and under nitrogen protection, 2.02g of chloroplatinic acid / iso Propanol solution (the mass fraction of chloroplatinic acid is 0.5%), the dropwise addition is completed in 40 minutes, and after 3 hours of reaction, epoxy silicon oil is obtained, and then 1.0 g of diethyl phosphate is added, at 150 ° C and in the presence of a mixed solvent of xylene and ethanol Under the conditions of reflux for 5h, cooling to remove the solvent to obtain phosphorus and epoxy-containing organosilicon flame retardant.

[0025] Take 1 / 10 of the above flame retardant and compound it with 100g of F51 epoxy resin, and then use 25.4g of DDM to cure. The limiting oxygen index of the cured product is 21.2, and the impact strength is 11.0KJ / m 2 , the glass transition temperature is 164°C.

Embodiment 2

[0027] 100g of methyl hydrogen-containing silicone oil (hydrogen content of 0.32%), 20g of allyl glycidyl ether and 2.1g of vinyl trimethoxysilane (CH 2 =CHSi(OCH 3 ) 3 ) into a three-necked flask, under the protection of nitrogen, 2.44g of chloroplatinic acid / isopropanol solution (the mass fraction of chloroplatinic acid is 0.5%) was added dropwise under stirring at 80°C, and the addition was completed in 45 minutes. After 3 hours of reaction, the obtained Epoxy silicone oil, then add 10.2g of phosphorous acid, reflux at 150°C for 5h in the presence of a mixed solvent of ethanol and chloroform, and cool to remove the solvent to obtain a silicone flame retardant containing phosphorus and epoxy groups.

[0028] Take 1 / 10 of the above flame retardant and compound with 100g of common epoxy resin F51, and then use 25.7g of DDM to cure. The limiting oxygen index of the cured product is 23.3, and the impact strength is 11.3KJ / m 2 , the glass transition temperature is 167°C.

Embodiment 3

[0030] 100g of methyl hydrogen-containing silicone oil (hydrogen content of 0.54%), 38g of allyl glycidyl ether and 6g of γ-methacryloxypropyl triethoxysilane (CH 2 =CCH 3 CO 2 CH 2 CH 2 CH 2 Si(OC 2 h 5 ) 3 ) into a three-necked flask, and under nitrogen protection, 2.86g of chloroplatinic acid / isopropanol solution (the mass fraction of chloroplatinic acid is 0.5%) was added dropwise at 85°C with stirring, and the addition was completed in 50 minutes. After 3 hours of reaction, the obtained Epoxy silicone oil, then add 26.2g of phosphoric acid, reflux reaction at 150°C in the presence of a mixed solvent of ethanol and chloroform for 5 hours, and cool to remove the solvent to obtain a silicone flame retardant containing phosphorus and epoxy groups.

[0031] Take 1 / 10 of the above-mentioned flame retardant and compound it with 100g of common epoxy resin E51, and then use 25.6g of DDM to cure it. The limiting oxygen index of the cured product is 24.1, and the impact stre...

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Abstract

The invention relates to organic silicon fire retardant containing phosphor and epoxy radical. It is made up of 100 portions methyl containing hydrogen silicone oil, 1-150 portions allylglycidyl ether, 0-50 portions end reaction contained double organic silane coupler and 1-200 portions active material containing phosphor after compounding. The invention also relates to the manufacturing method of taking polyaddition reaction of methyl containing hydrogen silicone oil, allylglycidyl ether, and end reaction contained double organic silane coupler, and compounding with phosphor contained active material. The condensate compounded by the invention and common epoxy resin the limiting oxygen index would reach 23-29, and vitrifying transforming temperature would reach 168-185degree centigrade.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus- and epoxy-containing organosilicon flame retardant, and also to a preparation method of the organosilicon flame retardant. Background technique [0002] Epoxy resin is an important thermosetting resin, which has excellent mechanical properties, mechanical properties, electrical properties, chemical properties, adhesive properties and easy molding and processing, so it is widely used in coatings, adhesives, electronic appliances and advanced In the matrix of composite materials, in recent years, its application has been extended to electronic and electrical packaging materials such as semiconductor packaging materials, fiber reinforced materials, laminates, copper foil, and integrated circuits. This requires that the epoxy resin materials used not only have high toughness, heat resistance, and chemical resistance, but also have excellent flame retardancy and electrical properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/00C08L63/00C08K5/524
Inventor 刘伟区侯孟华
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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