Method for synthesizing paraphthaloyl chloride (TPC) through continuous flow in micro-channel reactor

A technology of terephthaloyl chloride and microchannel reactor, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, preparation of organic compounds, etc., can solve the problem of dark catalyst color, increase process steps, and recovery rate Low-level problems, to achieve the effect of low catalyst consumption, high reaction efficiency and stable catalyst

Active Publication Date: 2017-05-10
JIANGSU RUISHENG ADVANCED MATERIAL TECH CO LTD +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Disclosed in CN1054062A with TPA, PCl 3 , Cl 2 Synthesize TPC as a raw material, the reaction time is as long as 20 hours, PCl 3 High consumption, great corrosion to equipment, low product purity, need multiple vacuum distillation, low product yield; TPA and thionyl chloride are used as raw materials in CN104402709A, thionyl chloride is not only a reactant but also a solvent, and chlorination Thionoxide decompression distillation is difficult to remove, and it is easy to have a side reaction with TPC in the rectification process, which produces impurities and affects product quality; in CN101935276A, it is also a synthetic method of thionyl chloride, but it is difficult to recycle with quaternary ammonium salt as a catalyst, increasing Solid waste amount and product cost; CN10180527A discloses that TPA and solid Sanguang are used as raw materials, dichloroethane is used as solvent, and batch reaction is carried out. The utilization rate of solid light is low, the consumption of catalyst is large,

Method used

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  • Method for synthesizing paraphthaloyl chloride (TPC) through continuous flow in micro-channel reactor
  • Method for synthesizing paraphthaloyl chloride (TPC) through continuous flow in micro-channel reactor
  • Method for synthesizing paraphthaloyl chloride (TPC) through continuous flow in micro-channel reactor

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Experimental program
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Effect test

Embodiment 1

[0035] 1. Raw material preparation: Weigh 2000g of TPC, put it into a 2000ml four-neck bottle, heat and melt it in an oil bath at 90°C, then add 500g of TPA (screened with 200 mesh in advance), 10g of DMF, stir and mix to form a uniform slurry Standby; phosgene is connected to the microreactor through the pipeline through the mass flow meter, one-way valve, safety valve, etc. for standby.

[0036] 2. In the heart-shaped microchannel made of special glass, follow the steps below: (1) TPA slurry enters the microchannel reactor through the heat preservation slurry pump, opens the phosgene valve, and enters the microchannel reactor through the mass flow meter ; (2) Continuous flow microchannel reactor is adopted in the reaction process, raw material TPA homogeneous slurry and phosgene are mixed in the reactor according to the ratio, and the reaction is controlled at 100 ℃ by heat exchanger; (3) By adjusting the slurry pump Frequency and flow meter opening control the mol ratio of ...

Embodiment 2

[0038]1. Raw material preparation: Weigh 2000g of TPC, put it into a 2000ml four-neck bottle, heat and melt it in an oil bath at 90°C, then add 500g of TPA (screened with 200 mesh in advance), 5g of DMF, stir and mix to form a uniform slurry Standby; phosgene is connected to the microreactor through the pipeline through the mass flow meter, one-way valve, safety valve, etc. for standby.

[0039] 2. In the heart-shaped microchannel made of special glass, follow the steps below: (1) TPA slurry enters the microchannel reactor through the heat preservation slurry pump, opens the phosgene valve, and enters the microchannel reactor through the mass flow meter ; (2) Continuous flow microchannel reactor is adopted in the reaction process, raw material TPA homogeneous slurry and phosgene are mixed in the reactor according to the ratio, and the reaction is controlled at 120 ℃ by heat exchanger; (3) By adjusting the slurry pump Frequency and flow meter opening control the mol ratio of TP...

Embodiment 3

[0041] 1. Raw material preparation: Weigh 2000g of TPC, put it into a 2000ml four-neck bottle, heat and melt it in an oil bath at 90°C, then add 500g of TPA (screened with 200 mesh in advance), 5g of DMF, stir and mix to form a uniform slurry Standby; phosgene is connected to the microreactor through the pipeline through the mass flow meter, one-way valve, safety valve, etc. for standby.

[0042] 2. In the heart-shaped microchannel made of special glass, follow the steps below: (1) TPA slurry enters the microchannel reactor through the heat preservation slurry pump, opens the phosgene valve, and enters the microchannel reactor through the mass flow meter ; (2) Continuous flow microchannel reactor is adopted in the reaction process, raw material TPA homogeneous slurry and phosgene are mixed in the reactor according to the ratio, and the reaction is controlled at 120 ℃ by heat exchanger; (3) By adjusting the slurry pump Frequency and flow meter opening control the mol ratio of T...

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Abstract

The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing paraphthaloyl chloride through continuous flow in a micro-channel reactor by taking phthalic acid and phosgene/triphosgene as raw materials. The invention aims to provide a micro-channel continuous flow reaction manner for performing terephthalic acid chlorination so as to synthesize paraphthaloyl chloride. Compared with the existing process, the process disclosed by the invention has the characteristics of being accurate in control of reaction conditions, high in phosgene/triphosgene utilization rate, low in catalyst usage, high in TPA (terephthalic acid) conversion ratio with reaction time of decades of seconds, high in TPC yield and the like.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for continuously synthesizing terephthaloyl dichloride in a microchannel reactor using terephthalic acid and phosgene / triphosgene as raw materials. Background technique [0002] Terephthaloyl chloride (TPC) is a white solid or colorless needle-like crystal, mainly used as polyparaphenylene terephthalamide (abbreviated as para-aramid fiber, 1414 or PPTA) and polysulfone fiber Polymerization monomer, in addition, it has certain applications as a modifier of high polymers, intermediates in pesticides and pharmaceutical industries, etc., and has broad prospects for development and utilization. [0003] The development of TPC in China mainly depends on the development of aramid fiber 1414. Since the production of aramid fiber has high requirements on the purity of TPC products, it needs to meet the requirements of purity>99.9%, monoacyl chloride (TMC)...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C63/30
CPCC07C51/60C07C63/30B01J19/0093B01J31/0245
Inventor 徐林王怡明邵波丁克鸿严绘卞辰超赵慧王玉霜
Owner JIANGSU RUISHENG ADVANCED MATERIAL TECH CO LTD
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