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A kind of phosphorus-containing silicon block copolymer and preparation method thereof

A technology of block copolymer and polymerization reaction, which is applied in the field of phosphorus-containing silicon block copolymer and its preparation, can solve the problems such as the limitation of the use of halogen-containing flame retardants, and achieves improved thermal properties and flame retardancy, and mild reaction conditions. Effect

Active Publication Date: 2016-06-01
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Although traditional halogen-containing flame retardants, especially bromine-containing flame retardants, have been proven to have good flame-retardant effects and have been widely used, studies have found that brominated dibenzodioxins, polybrominated dibenzofurans, etc. are toxic when burned. Substances that restrict the use of halogenated flame retardants

Method used

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  • A kind of phosphorus-containing silicon block copolymer and preparation method thereof
  • A kind of phosphorus-containing silicon block copolymer and preparation method thereof
  • A kind of phosphorus-containing silicon block copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) PMAiBuPOSS 18 Synthesis of Macromolecular Chain Transfer Agents

[0026] MAiBuPOSS (4.7315g, 5mmol), CDB (68.0mg, 0.25mmol) and AIBN (8.2mg, 0.05mmol) were dissolved in 3.5ml of toluene, and after continuous freezing and thawing and degassing for 3 to 5 times, they were placed under the protection of argon in Polymerize at 65°C. After 48 hours of reaction, the reaction is quenched with liquid nitrogen to stop the reaction. Methanol / ethyl acetate=7 / 1 is used as the precipitating agent, and the product is obtained by repeated precipitation for 3 times.

[0027] (2) PMAiBuPOSS 18 -b-PGMA 190 Synthesis of diblocks

[0028] PMAiBuPOSS 18 (2.572g), GMA (3.96ml), AIBN (3mL tetrahydrofuran solution with a concentration of 0.005mmol / ml AIBN) dissolved in 6ml tetrahydrofuran, after continuous freeze-thaw degassing for 3 to 5 times, polymerize at 65°C under the protection of argon , After 24 hours of reaction, the reaction was quenched with liquid nitrogen to stop the rea...

Embodiment 2～5

[0034] Steps (1) and (2) are the same as in Example 1. By changing step (3) PMAiBuPOSS m -b-PGMA n Phosphorus-silicon block copolymers with different ratios of P and Si were synthesized with the molar ratio of DOPO.

[0035] Table 1

[0036] Example

[0037] By changing step (3) PMAiBuPOSS m -b-PGMA n The phosphorus-containing silicon block copolymers with different P and Si ratios were synthesized with the molar ratio of DOPO, and the results are shown in Table 1.

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Abstract

The invention discloses a block copolymer containing phosphorus and silicon and a preparation method of the block copolymer, and relates to a block copolymer. Methacryloxy propyl hepta-isobutyl POSS and glycidyl methacrylate are taken as monomers to synthesize two block copolymers through reversible addition fragmentation chain transfer and free radical polymerization, then 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is grafted onto the two block copolymers through ring-opening reaction to form the block copolymer containing phosphorus and silicon. The DOPO with polyhedral oligomeric silsesquioxanes and an excellent flame retardant property is input into a macromolecular chain through chemical bonds to achieve the purpose of synergistic flame retardancy. The reaction conditions are mild; the content of the phosphorus and silicon can be regulated by controlling the rate of charge; the thermal property and flame retardancy of matrix resin are significantly improved.

Description

technical field [0001] The invention relates to a block copolymer, especially a phosphorus-containing silicon block copolymer with flame-retardant function and a preparation method thereof. Background technique [0002] Although traditional halogen-containing flame retardants, especially bromine-containing flame retardants, have been proven to have good flame-retardant effects and have been widely used, studies have found that brominated dibenzodioxins, polybrominated dibenzofurans, etc. are toxic when burned. Substances that restrict the use of halogenated flame retardants. Establishing a new type of halogen-free and non-toxic flame retardant system has become a new direction for the development of flame retardant science research. [0003] It is well known that the two elements of phosphorus and silicon have a synergistic flame retardant effect. When phosphorus-containing silicon flame retardant is used, at high temperature, phosphorus element promotes the formation of c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F8/40
Inventor 戴李宗邱武辉袁丛辉罗伟昂许一婷曾碧榕曹莹何凯斌刘新瑜
Owner XIAMEN UNIV