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Flame-retardant block copolymer containing nitrogen and phosphorus and preparation method thereof

A technology of block copolymers and polymer chains, which is applied in the field of polymer halogen-free flame retardants, can solve the problems of restricting the widespread use of halogen-containing flame retardants, achieve improved compatibility and flame retardancy, and mild reaction conditions Effect

Active Publication Date: 2015-01-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, studies have found that brominated flame retardants will produce toxic substances such as brominated dibenzodioxins when burned, which limits the widespread use of halogenated flame retardants

Method used

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  • Flame-retardant block copolymer containing nitrogen and phosphorus and preparation method thereof
  • Flame-retardant block copolymer containing nitrogen and phosphorus and preparation method thereof
  • Flame-retardant block copolymer containing nitrogen and phosphorus and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) PMOEP 80 Synthesis of Macromolecular Chain Transfer Agents

[0029] Dissolve MOEP (0.9125g, 4mmol), CDB (13.62mg, 0.05mmol) and AIBN (1.64mg, 0.01mmol) in 5ml of anhydrous methanol, after continuous freeze-thaw degassing for 3 to 5 times, under the protection of argon Polymerize at 65°C. After 24 hours of reaction, stop the reaction by quenching with liquid nitrogen. Use 15 times the volume, that is, 90ml of ethanol as the precipitant, and repeat the precipitation twice to obtain the product PMOEP. 80 .

[0030] (2) PMOEP 80 -b-PDMAEMA 100 Synthesis of diblocks

[0031] will PMOEP 80 (0.3g, 0.03mmol), DMAEMA (0.6027ml, 3mmol), AIBN (1mg, 0.006mmol) were dissolved in 3ml of anhydrous methanol, after continuous freeze-thaw degassing for 3 to 5 times, under the protection of argon at 65°C Polymerization, after 24 hours of reaction, it was quenched with liquid nitrogen to stop the reaction, and ethanol was used as the precipitating agent for repeated precipitation...

Embodiment 2

[0033] (1) PMOEP 60 Synthesis of Macromolecular Chain Transfer Agents

[0034] Dissolve MOEP (0.6844g, 3mmol), CDB (13.62mg, 0.05mmol) and AIBN (1.64mg, 0.01mmol) in 4.5ml of anhydrous methanol. Polymerization at 65°C, after 24 hours of reaction, quenched with liquid nitrogen to stop the reaction, 15 times the volume, that is, 80ml of ethanol as the precipitant, and repeated precipitation twice to obtain the product PMOEP 60 .

[0035] (2) PMOEP 60 -b-PDMAEMA 100 Synthesis of diblocks

[0036] will PMOEP 60 (0.225g, 0.0225mmol), DMAEMA (0.6027ml, 3mmol), AIBN (1mg, 0.006mmol) were dissolved in 3ml of anhydrous methanol, after continuous freeze-thaw degassing for 3 to 5 times, under argon protection at 65°C Polymerization, after 24 hours of reaction, it was quenched with liquid nitrogen to stop the reaction, and ethanol was used as the precipitating agent for repeated precipitation twice to obtain the product PMOEP 60 -b-PDMAEMA100 .

Embodiment 3

[0038] (1) PMOEP 80 Synthesis of Macromolecular Chain Transfer Agents

[0039] Dissolve MOEP (0.9125g, 4mmol), CDB (13.62mg, 0.05mmol) and AIBN (1.64mg, 0.01mmol) in 4.5ml of anhydrous methanol. Polymerization at 65°C, after 24 hours of reaction, quenched with liquid nitrogen to stop the reaction, 15 times the volume, that is, 80ml of ethanol as the precipitant, and repeated precipitation twice to obtain the product PMOEP 80 .

[0040] (2) PMOEP 80 -b-PDMAEMA 80 Synthesis of diblocks

[0041] will PMOEP 80 (0.3g, 0.03mmol), DMAEMA (0.4822ml, 2.4mmol), AIBN (1mg, 0.006mmol) were dissolved in 3ml of anhydrous methanol, after continuous freeze-thaw degassing for 3 to 5 times, under the protection of argon at 65 Polymerization at ℃, after 24 hours of reaction, it was quenched with liquid nitrogen to stop the reaction, and ethanol was used as the precipitating agent for repeated precipitation twice to obtain the product PMOEP 80 -b-PDMAEMA 80 .

[0042] Obtained target pho...

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Abstract

The invention discloses a flame-retardant block copolymer containing nitrogen and phosphorus and a preparation method thereof and relates to a block copolymer. The flame-retardant block copolymer containing nitrogen and phosphorus is PMOEPm-b-PDMAEMAn. The preparation method comprises the steps of dissolving 2-hydroxyethyl methacrylate phosphate, cumyl dithiobenzoate and azobisisobutyronitrile in a solvent, carrying out freeze thawing and degassing until unfreezing is realized and no bubbles come out, carrying out polymerization reaction under the protection of inert gas, quenching with liquid nitrogen to stop the reaction, precipitating and drying to obtain a product which is a PMOEPm macromolecular chain transfer agent; dissolving the PMOEPm macromolecular chain transfer agent, dimethylaminoethyl methacrylate and azobisisobutyronitrile in the solvent, carrying out freeze thawing and degassing, carrying out polymerization reaction under the protection of inert gas, quenching with liquid nitrogen to stop the reaction and repeatedly precipitating with ethanol used as a precipitant to obtain the target product, namely, flame-retardant block copolymer containing nitrogen and phosphorus (PMOEPm-b-PDMAEMAn). The flame-retardant block copolymer containing nitrogen and phosphorus can be used in preparation of halogen-free flame retardant and self-assemble micelles.

Description

technical field [0001] The invention belongs to the field of polymer halogen-free flame retardancy, and relates to a block copolymer, in particular to a phosphorus-nitrogen-containing flame-retardant block copolymer with flame-retardant function and a preparation method thereof. Background technique [0002] Traditional halogenated flame retardants, especially bromine-containing flame retardants, have good flame retardant effects and have been widely used. However, studies have found that bromine-containing flame retardants will produce toxic substances such as brominated dibenzodioxins when burned, which limits the widespread use of halogen-containing flame retardants. Therefore, the establishment of a new type of efficient, halogen-free, non-toxic flame retardant system has become a new direction of flame retardant scientific research. [0003] The traditional condensed phase halogen-free flame retardant system is related to the three elements of P, N, and Si. They can ef...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08L53/00A61K47/32
Inventor 戴李宗叶华立袁丛辉李远源陈显明刘诚罗伟昂何凯斌许一婷刘新瑜
Owner XIAMEN UNIV
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