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Device and method for continuously synthesizing quaternary ammonium compound of ester

A technology for quaternary ammonium compounds and synthetic esters, which is applied in the field of organic synthesis technology, can solve problems that are not conducive to large-scale industrial production, and achieve the effects of easy automatic control, automatic control, and short residence time

Active Publication Date: 2019-12-20
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process adopts intermittent operation, which is not conducive to large-scale industrial production

Method used

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  • Device and method for continuously synthesizing quaternary ammonium compound of ester

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Embodiment 1

[0029] A device for continuously synthesizing quaternary ammonium compounds of esters, the device comprises a static mixer, a tubular reactor, a reaction liquid receiving tank, and a desolvation tower; the inlet of the tubular reactor is communicated with the outlet of the static mixer through a pipeline, The outlet of the tubular reactor is communicated with the inlet of the reaction liquid receiving tank through the pipeline; the outlet of the reaction liquid receiving tank is communicated with the inlet I of the desolvation tower through the pipeline.

[0030] The middle and lower part of the desolvation tower is also provided with an inlet II.

[0031] The top of the desolvation tower is provided with an outlet II, and the outlet II is connected to the condenser through a pipeline.

[0032] The outlet of the condenser is communicated with the inlet III of the desolvation column through a pipeline.

[0033] A circulating condensation device is provided outside the tubular ...

Embodiment 2

[0040] Adopt the device described in embodiment 1 to continuously synthesize tetraisobutylammonium ethyl sulfate, and its concrete steps are:

[0041] Using diethyl sulfate and triisobutylamine as raw materials and ethanol as solvent, tetraisobutylammonium ethyl sulfate was synthesized. Taking diethyl sulfate as the measurement benchmark, the flow rate of diethyl sulfate is 154g / h, the flow rate of ethanol is 231g / h, and the flow rate of triisobutylamine is 182g / h, and the three enter the static mixer after metering Mixed and then quaternized in a tubular reactor. The pressure of the tubular reactor was 0.2 MPa, the residence time of the reactants in the tubular reactor was 30 min, and the temperature of the tubular reactor was controlled at 50°C.

[0042] After the material comes out of the tubular reactor, it enters the reaction liquid receiving tank, and then is pumped into the middle position of the desolvation tower. The tower pressure is -0.098MPa, the reflux ratio is 1...

Embodiment 3

[0045] Adopt the device described in embodiment 1 to synthesize tetra-n-propyl ammonium methyl carbonate continuously, and its concrete steps are:

[0046]Using dimethyl carbonate and tri-n-propylamine as raw materials and methanol as solvent, tetra-n-propyl ammonium methyl carbonate was synthesized. Taking dimethyl carbonate as the measurement benchmark, the flow rate of dimethyl carbonate is 900g / h, the flow rate of methanol is 1200g / h, and the flow rate of tri-n-propylamine is 143g / h. , and then the quaternization reaction was carried out in a tubular reactor. The pressure of the tubular reactor was 1.0 MPa, the residence time of the reactants in the tubular reactor was 15 min, and the temperature of the tubular reactor was controlled at 60°C.

[0047] After the material comes out of the tubular reactor, it enters the reaction liquid receiving tank, and then enters the middle and upper part of the desolvation tower at a flow rate of 2200g / h, and pure water enters the middl...

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Abstract

The invention belongs to the technical field of organic synthesis processes, and particularly relates to a device and a method for continuously synthesizing a quaternary ammonium compound of ester. According to the invention, the tubular reactor is adopted, so that the continuous reaction is realized; and the separation is continuous by using the rectification technology, and the reaction and theseparation are organically combined, such that the reaction and the separation are continuous at the same time, the production efficiency is improved, the side reactions are reduced, and the reactionconversion rate is increased.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a device and a method for continuously synthesizing quaternary ammonium compounds of esters. Background technique [0002] The quaternary ammonium compound of ester is an important intermediate product for synthesizing quaternary ammonium salts and quaternary ammonium bases and other quaternary ammonium compounds, and has a very wide range of uses. For example, methyl chloroacetate quaternary ammonium salt can be hydrolyzed to synthesize betaine hydrochloride; tetramethylammonium methyl sulfate can be hydrolyzed to synthesize tetramethylamine hydroxide in aqueous sodium hydroxide solution. [0003] The synthesis of quaternary ammonium compounds of esters at present is usually batch synthesis in a tank reactor followed by a solvent removal process. The whole reaction process is discontinuous, and the post-processing is difficult. As reported in p...

Claims

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Application Information

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IPC IPC(8): C07C213/08C07C219/16C07C219/06C07C303/24C07C305/08C07C227/08C07C229/12C07C68/06C07C69/96B01J19/24B01D3/00B01D3/14
CPCC07C213/08C07C303/24C07C227/08C07C68/06B01J19/2415B01D3/009B01D3/14C07C219/16C07C219/06C07C305/08C07C229/12C07C69/96
Inventor 陈琦滕俊峰岳涛王灏王达彤
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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