Liquid-liquid homogeneous method for synthesizing polyaryl ether by using continuous flow micro-channel reactor

A technology of microchannel reactor and channel reactor, which is applied in the field of liquid-liquid homogeneous method, can solve the problems of failing to realize large-scale production of all-water medium, etc.

Active Publication Date: 2019-08-23
常州中英新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Essentially, the synthesis of polyphenylene ether is also achieved through the oxidative condensation polymerization of 2,6-dimethylphenol. However, there has been no preparation of polyphenylene ether or polyarylether in all-aqueous medium using a continuous flow microchannel reactor. Research work reports, but failed to realize the industrialized large-scale production of the all-aqueous medium method

Method used

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  • Liquid-liquid homogeneous method for synthesizing polyaryl ether by using continuous flow micro-channel reactor
  • Liquid-liquid homogeneous method for synthesizing polyaryl ether by using continuous flow micro-channel reactor
  • Liquid-liquid homogeneous method for synthesizing polyaryl ether by using continuous flow micro-channel reactor

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Embodiment 1

[0028] Embodiment 1: as attached figure 1 ,2 and attached image 3 As shown, configure 4wt% 2,6,-dimethylphenol sodium hydroxide aqueous solution, the pH value is controlled at 11, and add 0.75wt% sodium lauryl sulfate, stir slowly; then add 20wt% hydrogen peroxide 1.2wt% copper-ethylenediaminetetraacetic acid complex, stir evenly; inject 2,6,-dimethylphenol aqueous sodium hydroxide solution and hydrogen peroxide into the straight line of Corning high-throughput microchannel reactor through a metering pump The channel module is preheated, and the preheating temperature is set to 35°C, and the preheating residence time is 30s; the flux of the sodium hydroxide aqueous solution of 2,6,-dimethylphenol in the straight channel module is controlled at 3mL / min, and 2,6,-Dimethylphenol and H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.2. The preheated 2,6,-dimethylphenol sodium hydroxide aqueous solution and hydrogen peroxide directly enter the reaction module co...

Embodiment 2

[0029] Embodiment 2: as attached figure 1 , 2 and attached image 3 As shown, configure 4wt% 2-methyl-6-bromophenol aqueous sodium hydroxide solution, the pH value is controlled at 11, and add 0.75wt% sodium lauryl sulfate, stir slowly; then add 1.2wt% copper-ethylenediaminetetraacetic acid complex, stir evenly; inject 2-methyl-6-bromophenol aqueous sodium hydroxide solution and hydrogen peroxide into the straight line of Corning high-throughput microchannel reactor through metering pump The channel module is preheated, the preheating temperature is set to 45°C, and the preheating residence time is 40s; the flux of the sodium hydroxide aqueous solution of 2-methyl-6-bromophenol in the straight channel module is controlled at 3mL / min, and 2-Methyl-6-bromophenol and H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.2. The preheated 2-methyl-6-bromophenol aqueous sodium hydroxide solution and hydrogen peroxide directly enter the reaction module composed of 10 ...

Embodiment 3

[0030] Embodiment 3: as attached figure 1 , 2 and attached image 3 As shown, configure 8wt% 2,6,-dimethylphenol sodium hydroxide aqueous solution, the pH value is controlled at 11, and add 1.25wt% sodium lauryl sulfate, stir slowly; then add to 30wt% hydrogen peroxide 1.5wt% copper-ethylenediaminetetraacetic acid complex, stir evenly; inject 2,6,-dimethylphenol aqueous sodium hydroxide solution and hydrogen peroxide into the straight line of Corning high-throughput microchannel reactor through a metering pump The channel module is preheated, and the preheating temperature is set to 45°C, and the preheating residence time is 40s; the flux of the sodium hydroxide aqueous solution of 2,6,-dimethylphenol in the straight channel module is controlled at 2mL / min, and 2,6,-Dimethylphenol and H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.2. The preheated 2,6,-dimethylphenol sodium hydroxide aqueous solution and hydrogen peroxide directly enter the reaction modu...

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Abstract

The invention belongs to the field of polymer synthesis, and in particular relates to a liquid-liquid homogeneous method for synthesizing polyaryl ether by using a continuous flow micro-channel reactor. According to the method, an alkaline aqueous solution of a phenol derivative and an aqueous solution of an oxidant are respectively injected into DC-type micro-channel reactors by using metering pumps for preheating, and then are directly introduced into enhancing mixed-type continuous flow micro-channel reactors, a polyaryl ether solution is obtained by a liquid-liquid homogeneous reaction, and a final product polyaryl ether is obtained by filtering, washing and drying. The operation is simple, the polymerization process is safe, controllable and green, the yield is high, the molecular weight distribution is relatively narrow, the production efficiency is high, and the continuous industrial mass production can be realized.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a liquid-liquid homogeneous method for synthesizing polyarylether by using a continuous flow microchannel reactor. Background technique [0002] The continuous flow microchannel reactor is a small reaction system, and its pipe size is much smaller than that of conventional reactors. The miniaturization of the reaction channel can significantly increase the contact area between the channel and the heat exchange medium, and improve the heat exchange efficiency. The extremely strong turbulent flow process in the microchannel can make the mass transfer effect increase exponentially. In addition, the continuous flow microchannel reactor can realize multi-step continuous reaction, and can be directly scaled up to achieve mass production without pilot test, with high safety, controllable production process and high reaction selectivity. [0003] At present, the co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/44
CPCC08G65/44
Inventor 俞卫忠顾书春俞丞冯凯
Owner 常州中英新材料有限公司
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