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A kind of phosphorus-containing poss flame-retardant bismaleimide resin and preparation method thereof

A technology of bismaleimide resin and bismaleimide, which is applied in the field of bismaleimide resin and its preparation, can solve the problems of reduced mechanical properties, poor compatibility and the like, and achieves the promotion of dense carbon layer. The formation of , improve compatibility, improve the effect of flame retardant performance

Inactive Publication Date: 2017-05-24
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, adding filler-type flame retardants is the main means to improve the flame retardant performance of the resin matrix, but most of the flame retardants have poor compatibility with the resin matrix, resulting in a significant decrease in the mechanical properties of the resin while improving the flame retardant performance.

Method used

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  • A kind of phosphorus-containing poss flame-retardant bismaleimide resin and preparation method thereof
  • A kind of phosphorus-containing poss flame-retardant bismaleimide resin and preparation method thereof
  • A kind of phosphorus-containing poss flame-retardant bismaleimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1: Add 0.001mol of chloropropyl POSS, 0.006mol of O,O-bis(4-(hydroxy)phenyl)phenylphosphonate, and 0.7mol of N,N-dimethylformamide into a three-necked flask. After dissolution, add 0.02mol triethylamine, 0.002mol KI, and react for 8 hours at 80°C in a water bath. After the reaction is completed, the solvent is evaporated and washed with dilute hydrochloric acid and distilled water. After recrystallization, poly(bis(4-hydroxy Phenyl) phenyl phosphonate) substituted chloropropyl silsesquioxane.

[0031] Step 2: According to the mass, weigh 100 parts of diphenylmethane type bismaleimide and 60 parts of diallyl bisphenol A into a beaker, heat and melt at 120~150℃, stir evenly, add 10 parts Multi-(bis(4-hydroxyphenyl)phenylphosphonate) substituted chloropropyl silsesquioxane, after stirring evenly, pour it into a mold preheated at 130°C for more than 30 minutes, and put it in 140~160 In a vacuum box at ℃, after deaeration, put it in a blast drying box for stage heating an...

Embodiment 2

[0033] Step 1: Add 0.001mol of chloropropyl POSS, 0.010mol of O,O-bis(4-(hydroxy)phenyl)phenylphosphonate, and 1.0mol of N,N-dimethylformamide into a three-necked flask. After dissolution, add 0.02mol triethylamine, 0.004mol KI, and react at 80℃ in a water bath for 6 hours. After the reaction is completed, the solvent is evaporated and washed with dilute hydrochloric acid and distilled water respectively. After recrystallization, poly(bis(4-hydroxy Phenyl) phenyl phosphonate) substituted chloropropyl silsesquioxane.

[0034] Step 2: Same as implementation example 1.

Embodiment 3

[0036] Step 1: Same as implementation example 1.

[0037] Step 2: According to the mass, weigh 100 parts of diphenylmethane type bismaleimide and 75 parts of diallyl bisphenol A into a beaker, heat and melt at 120~150℃, stir evenly, add 5 parts Multi-(bis(4-hydroxyphenyl)phenylphosphonate) substituted chloropropyl silsesquioxane, after stirring evenly, pour it into a mold preheated at 130°C for more than 30 minutes, and put it in 140~160 In a vacuum box at ℃, after deaeration, put it in a blast drying box for stage heating and curing. The curing process is 180℃ / 2h+200℃ / 2h+220℃ / 2h, cooling, demoulding, and then at 250℃ It is obtained after 4h.

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Abstract

The invention provides a phosphorus-containing POSS (polyhedral oligomeric silsesquioxane) flame-retardant bismaleimide resin and a preparation method thereof. The resin is composed of the following components in parts by mass: 100 parts of diphenylmethane bismaleimide, 50-100 parts of diallyl bisphenol A and 1-20 parts of poly(di(4-hydroxyphenyl)phenylphosphate) substituted chloropropyl silsesquioxane. Under the synergistic effects of the phosphorus and silicon in the poly(di(4-hydroxyphenyl)phenylphosphate) substituted chloropropyl silsesquioxane, the poly(di(4-hydroxyphenyl)phenylphosphate) substituted chloropropyl silsesquioxane can inhibit the combustion of the resin and promote the formation of the compact carbon layer, so that the resin generates a small amount of smoke and does not generate any toxic gas or corrosive gas in the combustion process and conforms to the environmental requirements. The poly(di(4-hydroxyphenyl)phenylphosphate) substituted chloropropyl silsesquioxane can react with the bismaleimide resin, and has favorable compatibility with the resin. Thus, the prepared bismaleimide resin system has the advantages of excellent mechanical properties, high flame retardancy and high temperature resistance, and can be used as an ablation-resistant material.

Description

Technical field [0001] The invention belongs to the field of advanced composite material science and technology, in particular to a bismaleimide resin and a preparation method thereof. Background technique [0002] Bismaleimide resin is a kind of high-performance thermosetting resin matrix with active double bonds, which is widely used in transportation, aerospace, mechanical and electronic fields. With the wide application of polymer materials in various fields, people have higher and higher requirements for their flame retardancy and self-extinguishing properties. Therefore, the research and development of flame retardant modification of bismaleimide is of great significance. At present, adding filler-type flame retardants is the main method to improve the flame retardant performance of the resin matrix, but most flame retardants have poor compatibility with the resin matrix, resulting in improved flame retardant properties of the resin while greatly reducing the mechanical pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L79/08C08K5/549C08G73/12
CPCC08G73/12C08K5/549C08L2201/02C08L2201/08C08L79/085
Inventor 颜红侠李松陈争艳汤成
Owner NORTHWESTERN POLYTECHNICAL UNIV