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Inflaming retarding segmented copolymer containing phosphorus and silicon and preparation method thereof

A technology of block copolymers and polymer chains, applied in the field of phosphorus-containing silicon flame-retardant block copolymers and its preparation, can solve problems such as secondary hazards and large amounts of hydrogen halide gas, achieve mild reaction conditions, and improve compatibility The effect of resistance and flame retardancy

Active Publication Date: 2014-12-17
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Halogen-containing flame retardants have excellent flame-retardant effects and have been widely used as flame-retardant materials. Halogen-containing flame-retardant materials will produce a large amount of smoke and toxic corrosive hydrogen halide gas during the flame-retardant process, causing secondary hazards.

Method used

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  • Inflaming retarding segmented copolymer containing phosphorus and silicon and preparation method thereof
  • Inflaming retarding segmented copolymer containing phosphorus and silicon and preparation method thereof
  • Inflaming retarding segmented copolymer containing phosphorus and silicon and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Synthesis of HEDOPO monomer

[0034] First DOPO (4.32g, 0.02mol) and carbon tetrachloride (3.692g, 0.024mol) were mixed, added to 20ml of dichloromethane solvent and stirred with a magnet, and hydroxyethyl methacrylate (3.1234g, 0.024mol ) and triethylamine salt (2.4272g, 0.024mol) solution were mixed and added to the former, and ice-bathed, reacted at room temperature for 24 hours after a period of time, filtered, washed with NaOH solution for 3 times, and then washed with deionized water 2 times to get HEDOPO monomer.

[0035] 2)PHEDOPO 100 Synthesis of Macromolecular Chain Transfer Agents

[0036] Dissolve HEDOPO (1.376g, 4mmol), CDB (0.0109g, 0.04mmol) and AIBN (0.00164g, 0.01mmol) in 5mL of tetrachloroethane, and after continuous freeze-thaw degassing for 5 times, under argon protection, Polymerize at 65°C. After 24 hours of reaction, quench with liquid nitrogen to stop the reaction. Use 15 times the volume of 90mL ethanol as the precipitating agent to repeat...

Embodiment 2

[0040] 1) Synthesis of HEDOPO monomer

[0041] First DOPO (2.16g, 0.01mol) and carbon tetrachloride (2.3076g, 0.015mol) were mixed, added to 10ml of dichloromethane solvent and stirred with a magnet, and hydroxyethyl methacrylate (1.9521g, 0.015mol ) and triethylamine salt (1.5179g, 0.015mol) solution were mixed and added to the former, ice-bathed, reacted at room temperature for 24 hours after a period of time, filtered, washed with NaOH solution for 3 times, and then washed with deionized water for 2 times, to obtain HEDOPO monomer.

[0042] 2)PHEDOPO 50 Synthesis of Macromolecular Chain Transfer Agents

[0043]Dissolve HEDOPO (1.376g, 4mmol), CDB (0.0218g, 0.08mmol) and AIBN (0.00328g, 0.02mmol) in 5mL of tetrachloroethane, and after continuous freeze-thaw degassing for 5 times, under argon protection, Polymerize at 65°C. After 24 hours of reaction, quench with liquid nitrogen to stop the reaction. Use 15 times the volume of 90mL ethanol as the precipitating agent to rep...

Embodiment 3

[0047] 1) Synthesis of HEDOPO monomer

[0048] First DOPO (2.16g, 0.01mol) and carbon tetrachloride (1.3014g, 0.01mol) were mixed, added to 10ml of dichloromethane solvent and magnetically stirred and mixed, and hydroxyethyl methacrylate (1.5384g, 0.01mol ) and triethylamine salt (1.0119g, 0.01mol) solution were mixed and added to the former, and ice-bathed, reacted at room temperature for 24 hours after a period of time, filtered, washed with NaOH solution for 3 times, and then washed with deionized water for 2 times, to obtain HEDOPO monomer.

[0049] 2)PHEDOPO 80 Synthesis of Macromolecular Chain Transfer Agents

[0050] HEDOPO (2.752g, 8mmol), CDB (0.0272g, 0.1mmol) and AIBN (0.00328g, 0.02mmol) were dissolved in 5mL of tetrachloroethane, and after continuous freeze-thaw degassing for 5 times, under the protection of argon, the Polymerize at 65°C. After 24 hours of reaction, quench with liquid nitrogen to stop the reaction. Use 15 times the volume of 90mL ethanol as the...

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Abstract

An inflaming retarding segmented copolymer containing phosphorus and silicon and a preparation method thereof relate to the segmented copolymer. The preparation method includes mixing 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide and carbon tetrachloride and adding the mixture into a solvent to obtain a mixture A; mixing methyl-hydroxyethyl acrylate and a triethylamine salt solution, adding the mixture into the mixture A, conducting filtering after reaction and conducting washing to obtain HEDOPO; dissolving the HEDOPO, dithio-benzoic acid-cumyl-ester and AIBN into the solvent, conducting freeze thawing degasification post polymerization reaction, stopping reaction through liquid nitrogen sudden cooling and conducting sedimentation to obtain a PHEDOPO macromolecule chain transfer agent; dissolving the PHEDOPO macromolecule chain transfer agent, 3-(isobutene-acyl-oxygen)-propyl-trimethoxy silane and the AIBN into tetrachloroethane, conducting continuous freeze thawing degasification post polymerization reaction, stopping the reaction through liquid nitrogen sudden cooling and conducting sedimentation through a precipitant to obtain the product the inflaming retarding segmented copolymer containing phosphorus and silicon.

Description

technical field [0001] The invention relates to a block copolymer, in particular to a phosphorus-containing silicon flame-retardant block copolymer with flame-retardant function and a preparation method thereof. Background technique [0002] Halogen-containing flame retardants have excellent flame-retardant effects and have been widely used as flame-retardant materials. Halogen-containing flame-retardant materials will produce a large amount of smoke and toxic corrosive hydrogen halide gas during the flame-retardant process, causing secondary hazards. The World Health Organization (WHO) and many national environmental protection departments have banned the use of halogen-containing flame retardants, and new halogen-free flame retardants have become new products that meet the development trend of international standards. 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 resear...

Claims

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Application Information

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IPC IPC(8): C08F230/02C08F230/08C07F9/6574C08F293/00
Inventor 许一婷陈显明戴李宗叶华立陈国荣李聪曹莹李奇罗伟昂何凯斌刘新瑜
Owner XIAMEN UNIV
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