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Novel synthetic process of bromized polyphenyl ether

A technology of brominated polyphenylene ether and synthesis process, which is applied in the field of new brominated polyphenylene ether synthesis technology, can solve problems such as unsatisfactory performance, and achieve the effects of good flame retardant performance, improved mechanical performance and good flame retardant efficiency

Active Publication Date: 2016-12-21
WEIFANG XINYANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although decabromodiphenyl ether is widely used, its mechanical performance is unsatisfactory in the current application of resin products, and it is increasingly unable to meet people's needs. Excellent polyphenylene ether products need to be developed urgently

Method used

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  • Novel synthetic process of bromized polyphenyl ether
  • Novel synthetic process of bromized polyphenyl ether
  • Novel synthetic process of bromized polyphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A novel brominated polyphenylene ether synthesis process, comprising the following steps:

[0020] (1) Polymerization: use 1000 g methanol as a solvent, put 331 g of solid tribromophenol (TBP) and 54 g of solid sodium methoxide into it, and add 1.6 g-10 g of benzoyl peroxide (BPO) after complete dissolution As a catalyst, the temperature was raised to 65 °C and refluxed for 4 h, then cooled to below 30 °C, suction filtered, rinsed with methanol, and dried to obtain crude poly[2,6-dibromo-1,4-]polyphenylene ether (POBP). .

[0021] In the above polymerization reaction, 2,4,6-tribromophenol (TBP) is used as a raw material, firstly, a sodium salt is formed with a strong base, and then a polycondensation reaction is carried out under the catalysis of an oxidant. The raw material sodium methoxide is obtained by reacting sodium metal in methanol.

[0022] (2) Recrystallization: after weighing the crude POBP obtained in step (1), dissolve it into tetrahydrofuran with 3 times...

Embodiment 2

[0025] Different from embodiment 1, a kind of novel brominated polyphenylene ether synthesis process, comprises the following steps:

[0026] (1) Polymerization: use 1000 g methanol as a solvent, put 331 g of solid tribromophenol (TBP) and 27 g of solid sodium methoxide into it, and add 1.6 g to 10 g of benzoyl peroxide (BPO) after complete dissolution. As a catalyst, the temperature was raised to 65 °C and refluxed for 4 h, then cooled to below 30 °C, suction filtered, rinsed with methanol, and dried to obtain crude poly[2,6-dibromo-1,4-]polyphenylene ether (POBP). .

[0027] In the above polymerization reaction, 2,4,6-tribromophenol (TBP) is used as a raw material, firstly, a sodium salt is formed with a strong base, and then a polycondensation reaction is carried out under the catalysis of an oxidant. The raw material sodium methoxide is obtained by reacting sodium metal in methanol.

[0028] (2) Recrystallization: after weighing the crude POBP obtained in step (1), disso...

Embodiment 3

[0031] Different from embodiment 1, a kind of novel brominated polyphenylene ether synthesis process, comprises the following steps:

[0032] (1) Polymerization: use 1000 g methanol as a solvent, put 331 g solid tribromophenol (TBP) and 108 g solid sodium methoxide into it, and add 1.6 g-10 g benzoyl peroxide (BPO) after complete dissolution As a catalyst, the temperature was raised to 65 °C and refluxed for 4 h, then cooled to below 30 °C, suction filtered, rinsed with methanol, and dried to obtain crude poly[2,6-dibromo-1,4-]polyphenylene ether (POBP). .

[0033] In the above polymerization reaction, 2,4,6-tribromophenol (TBP) is used as a raw material, firstly, a sodium salt is formed with a strong base, and then a polycondensation reaction is carried out under the catalysis of an oxidant. The raw material sodium methoxide is obtained by reacting sodium metal in methanol.

[0034] (2) Recrystallization: after weighing the crude POBP obtained in step (1), dissolve it into ...

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Abstract

The invention discloses a novel synthetic process of bromized polyphenyl ether. The novel synthetic process comprises the following steps of (1) polymerization: putting solid tribromophenol and solid sodium methylate with the molar ratio of 1 to (0.5 to 2) into methanol, adding a catalyst, rising the temperature to 65 DEG C, carrying out backflow reaction for 4 hours, cooling for suction filtration, leaching with the methanol, and drying to obtain a POBP crude product; (2) recrystallization: weighing the POBP crude product prepared in the step (1), dissolving into tetrahydrofuran with the weight three times of that of the POBP crude product, stirring at normal temperature till the POBP crude product is completely dissolved, starting electromagnetic stirring, quickly dripping into the methanol with the weight equal to that of the tetrahydrofuran, then continuously stirring for 1 hour, carrying out suction filtration and drying for spare use; (3) bromization: taking and dissolving POBP in dichloroethane with the weight three times of that of the POBP, dripping excessive bromine at the temperature of 20-30 DEG C, rising the temperature to 75 DEG C, reacting for 4 hours, cooling to 30 DEG C, adjusting PH, carrying out suction filtration, leaching, secondary suction filtration and drying to obtain the product. The novel synthetic process disclosed by the invention has the advantages that after bromized polyphenyl ether is used, the flame retardance and the mechanical property of a resin product can be obviously enhanced, and all detection indexes of the resin product are obviously more excellent, so that the bromized polyphenyl ether can be used as a great substitute product of decabromodiphenyl ether.

Description

technical field [0001] The invention belongs to the field of compound preparation, in particular to a novel brominated polyphenylene ether synthesis process. Background technique [0002] Polyphenylene ether is a high-strength engineering plastic developed in the 1960s. Its chemical name is poly-2,6-dimethyl-1,4-phenylene ether, abbreviated as PPO (Polyphenylene Oxide). thing. PPO has excellent physical and chemical properties, it is non-toxic, transparent, has low relative density, and has excellent mechanical strength, stress relaxation resistance, creep resistance, heat resistance, water resistance and water vapor resistance. [0003] Brominated polyphenylene ether (BPPO), as the brominated product of polyphenylene ether, has been widely used due to its excellent thermal stability, heat resistance and mechanical properties. Among them, decabromodiphenyl ether is a kind of high-efficiency broad-spectrum additive flame retardant. It is a traditional variety with mature pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/38C08G65/48
CPCC08G65/38C08G65/485
Inventor 丁加中王振良
Owner WEIFANG XINYANG CHEM CO LTD
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