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Method and device for synthesizing tetramethylammonium bicarbonate by microchannel reactor

A technology of tetramethylammonium bicarbonate and microchannel reactor, which is applied in the synthesis of tetramethylammonium bicarbonate, using a microchannel reactor to synthesize tetramethylammonium bicarbonate, can solve the problem of incomplete safety, Improve cost and floor area, corrosion of electrolysis device, etc., to achieve the effect of facilitating production expansion and efficiency increase, reducing the number of operators, and expanding production capacity

Pending Publication Date: 2022-06-07
CANGZHOU SUNHEAT CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Tetramethylammonium hydroxide can be prepared by electrolysis of tetramethylammonium chloride, but chloride ions are corrosive to the electrolysis device, and electrolysis produces toxic chlorine gas
[0012] 1. The reaction is an exothermic reaction, and the accumulation of materials in the reactor of the prior art scheme is relatively large, which does not completely solve the safety problem;
[0013] 2. The existing technical solutions all have the problem of long reaction residence time;
[0014] 3. A longer residence time will inevitably lead to a larger reactor volume, which increases the cost and floor area, which is not conducive to increasing production capacity

Method used

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  • Method and device for synthesizing tetramethylammonium bicarbonate by microchannel reactor
  • Method and device for synthesizing tetramethylammonium bicarbonate by microchannel reactor

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Experimental program
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Embodiment 1

[0049] The tetramethylammonium bicarbonate was synthesized through a microchannel reactor, and the raw material ratio was dimethyl carbonate and trimethylamine molar ratio = 1:1.05. The reaction pressure of the 316 stainless steel microchannel reactor was 3MPa, and the reaction temperature was 160°C. The residence time of the material in the microchannel reactor was 5 min, and the conversion rate of dimethyl carbonate was 99.0% by sampling analysis at the outlet of the reactor. The pressure of the first falling film evaporator was 0.11 MPa, and the evaporation temperature was 100°C. The pressure of the second falling film evaporator was normal pressure, and the evaporation temperature was 100°C. The pressure of the rectification tower is 0.09MPa, and the rectification temperature is 100℃. Sampling and analyzing the content of the product tetramethylammonium bicarbonate, the yield of tetramethylammonium bicarbonate was 97.3%.

Embodiment 2

[0051] The tetramethylammonium bicarbonate was synthesized through a microchannel reactor, and the raw material ratio was dimethyl carbonate and trimethylamine molar ratio = 1:1.02. The reaction pressure of the 316 stainless steel microchannel reactor was 4MPa, and the reaction temperature was 180°C. The residence time of the material in the microchannel reactor was 5 min, and the conversion rate of dimethyl carbonate was 98.8% by sampling analysis at the outlet of the reactor. The pressure of the first falling film evaporator was 0.15MPa, and the evaporation temperature was 110°C. The pressure of the second falling film evaporator was normal pressure, and the evaporation temperature was 110°C. The pressure of the rectification tower is 0.1MPa, and the rectification temperature is 110℃. Sampling and analyzing the content of the product tetramethylammonium bicarbonate, the yield of tetramethylammonium bicarbonate was 96.5%.

Embodiment 3

[0053] The tetramethylammonium bicarbonate was synthesized through a microchannel reactor, and the raw material ratio was dimethyl carbonate and trimethylamine molar ratio = 1:1.02. The reaction pressure of the 316 stainless steel microchannel reactor was 4MPa, and the reaction temperature was 180°C. The residence time of the material in the microchannel reactor was 3 minutes, and the conversion rate of dimethyl carbonate was 98.2% by sampling and analyzing the outlet of the reactor. The pressure of the first falling film evaporator was 0.12MPa, and the evaporation temperature was 110°C. The pressure of the second falling film evaporator was normal pressure, and the evaporation temperature was 110°C. The pressure of the rectification tower is 0.11MPa, and the rectification temperature is 110℃. Sampling and analyzing the content of the product tetramethylammonium bicarbonate, the yield of tetramethylammonium bicarbonate was 96.2%.

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Abstract

The invention provides a method and a device for synthesizing tetramethylammonium bicarbonate by a micro-channel reactor, which are characterized in that a micro-channel reactor module is heated to a preset temperature by a heat exchange medium, and raw materials of dimethyl carbonate and trimethylamine and a solvent methanol are pumped into the reactor by a metering pump for continuous reaction. The material discharged from the micro-channel reactor enters a first falling film evaporator after being subjected to flash evaporation, and part of the solvent and unconverted raw materials are recycled through the first falling film evaporator. Materials discharged from the bottom of the first falling-film evaporator and pure water are mixed through a static mixer to generate hydrolysis reaction and enter a second falling-film evaporator to separate part of methanol and water. And feeding the material discharged from the bottom of the second falling film evaporator into a rectifying tower to further separate methanol, and extracting a refined product from a tower kettle. The reaction safety can be effectively improved, the reaction time is shortened, the reactant conversion rate is improved, the equipment occupied area is small, the power consumption is low, the investment is saved, continuous production can be realized, and the product quality is stable.

Description

technical field [0001] The invention relates to a method for synthesizing tetramethyl ammonium bicarbonate, in particular to a method for synthesizing tetramethyl ammonium bicarbonate using a microchannel reactor, and belongs to the field of fine chemicals. Background technique [0002] Tetramethylammonium hydroxide (TMAH) is an organic base with the strongest alkalinity. TMAH is used as developer and etchant in liquid crystal and semiconductor chip industries. [0003] Tetramethylammonium hydroxide can be prepared by electrolysis of tetramethylammonium chloride, but chloride ions are corrosive to electrolysis devices, and electrolysis produces toxic chlorine gas. Tetramethylammonium hydroxide is prepared by electrolysis with tetramethylammonium bicarbonate as the raw material, and the anode produces carbon dioxide, which avoids the generation of toxic gas and reduces the corrosiveness to the equipment at the same time. [0004] Tetramethylammonium bicarbonate can be synthe...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/00B01J19/00
CPCC07C209/00B01J19/0093C07C211/63Y02P20/141
Inventor 刘颂军孙炜贾成林王亮高猛热甫开提江·木合塔尔张明慧冯亚楠
Owner CANGZHOU SUNHEAT CHEM
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