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Liquid-liquid heterogeneous method for synthesizing polyarylether by utilizing continuous flow micro-channel reactor

A micro-channel reactor and channel reactor technology, applied in the field of liquid-liquid heterogeneous method

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

However, there has been no research report on the preparation of polyphenylene ether or polyarylether by using a continuous flow microchannel reactor.

Method used

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  • Liquid-liquid heterogeneous method for synthesizing polyarylether by utilizing continuous flow micro-channel reactor
  • Liquid-liquid heterogeneous method for synthesizing polyarylether by utilizing continuous flow micro-channel reactor
  • Liquid-liquid heterogeneous method for synthesizing polyarylether by utilizing continuous flow micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: as attached figure 1 , 2 and attached image 3 As shown, 0.37g CuBr, 5.24g N,N-di-n-butylamine, 1.51g pyridine and 0.036g trioctylmethylammonium chloride were dissolved in 100g toluene solution, followed by adding 80g 50wt% 2,6- The dimethylphenol / toluene solution was quickly stirred evenly to obtain the reaction solution A. The reaction solution A and 20wt% hydrogen peroxide were pumped into the straight channel module of the Corning high-throughput microchannel reactor through a metering pump for preheating. The preheating temperature was set to 35°C and the preheating residence time was 30s; The flux in the channel module is controlled at 4mL / min, the 2,6-dimethylphenol in the reaction solution A and the H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.2. The preheated reaction solution A and 20wt% hydrogen peroxide were directly connected to the heart-shaped channel module of the Corning high-throughput microchannel reactor for mix...

Embodiment 2

[0030] Embodiment 2: as attached figure 1 , 2 and attached image 3 As shown, 0.38g CuBr, 5.32g N,N-di-n-butylamine, 1.50g pyridine and 0.051g trioctylmethylammonium chloride were dissolved in 100g toluene solution, followed by adding 80g 74wt% 2,3, 6-trimethylphenol / toluene solution and stirred rapidly to obtain reaction solution A. The reaction solution A and 30wt% hydrogen peroxide were pumped into the straight channel module of the Corning high-throughput microchannel reactor through the metering pump for preheating. The preheating temperature was set at 40°C and the preheating residence time was 30s; The flux in the channel module is controlled at 3.5mL / min, and the 2,3,6-trimethylphenol in the reaction solution A and the H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.3. The preheated reaction solution A and 30wt% hydrogen peroxide were directly connected to the heart-shaped channel module of the Corning high-throughput microchannel reactor for mixe...

Embodiment 3

[0031] Embodiment 3: as attached figure 1 , 2 and attached image 3 As shown, 0.40g CuBr, 5.68g N,N-di-n-butylamine, 1.62g pyridine and 0.073g trioctylmethylammonium chloride were dissolved in 100g toluene solution, followed by adding 80g 78wt% 2,6- The dimethylphenol / toluene solution was quickly stirred evenly to obtain the reaction solution A. The reaction solution A and 30wt% hydrogen peroxide were pumped into the straight channel module of Corning high-throughput microchannel reactor through the metering pump for preheating. The preheating temperature was set at 45°C and the preheating residence time was 40s; The flux in the channel module is controlled at 3.5mL / min, the 2,6-dimethylphenol in the reaction solution A and the H in hydrogen peroxide 2 o 2 The molar ratio between them is 1:1.3. The preheated reaction solution A and 30wt% hydrogen peroxide were directly connected to the heart-shaped channel module of Corning high-throughput microchannel reactor for mixed r...

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Abstract

The invention belongs to the field of polymer synthesis and in particular relates to a liquid-liquid heterogeneous method for synthesizing polyarylether by utilizing a continuous flow micro-channel reactor. The method disclosed by the invention comprises the following steps: taking an organic solution of phenol derivatives and hydrogen peroxide as raw materials, taking a metal salt-amine complex as a catalyst, introducing the various raw materials and the catalyst into a direct-flow type micro-channel reactor by a metering pump for preheating, directly introducing the materials into an enhanced mixing type continuous flow micro-channel reactor, and carrying out a liquid-liquid heterogeneous reaction to prepare a polyarylether solution; and finally, performing separating out-precipitating,filtering, washing and drying so as to obtain the final product polyarylether. The method disclosed by the invention is simple in operation, safe and controllable in polymerization process, high in yield, narrow in molecular weight distribution and high in production efficiency, and can realize large-scale continuous industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a liquid-liquid heterogeneous 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, especially for heterogeneous reactions, the mass transfer enhancement effect is more obvious. 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 saf...

Claims

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Application Information

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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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