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Method for preparing tetramethyl ammonium hydrogen carbonate with condensation reaction of pipe type reactor

A tetramethylammonium bicarbonate, tubular reactor technology, which is applied in the preparation of amino compounds by condensation/addition reactions, the preparation of amino compounds, chemical instruments and methods, etc. Stability and other issues, to achieve the effect of stable product quality, simple equipment and high use efficiency

Inactive Publication Date: 2008-12-03
HANGZHOU GREENDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The invention provides a method of using a continuous tubular reactor instead of a batch reactor and cooperating with corresponding processes to synthesize TMAC, which solves the problems of unstable pressure, unstable reaction, and affecting product quality in the synthesis reaction process, and realizes continuous production. Production, increase yield, reduce energy consumption and production costs, etc.

Method used

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  • Method for preparing tetramethyl ammonium hydrogen carbonate with condensation reaction of pipe type reactor
  • Method for preparing tetramethyl ammonium hydrogen carbonate with condensation reaction of pipe type reactor
  • Method for preparing tetramethyl ammonium hydrogen carbonate with condensation reaction of pipe type reactor

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Effect test

Embodiment 1

[0028] The tubular reactor is equipped with a static mixer, with 1000ml of methanol as the solvent, the raw material ratio (molar ratio) DMC:TMA=0.95:1, the reaction temperature is 115°C, and the reaction pressure is 0.5MPa. The continuous reaction time is 130 Minutes, a sample was taken and chromatographically analyzed for the content of dimethyl carbonate, and the conversion rate was 93.4%.

Embodiment 2

[0030] With 1000ml ethanol as solvent, in raw material proportioning (molar ratio) DMC: TMA=1: 1, reaction temperature is 115 ℃, reaction time is 130 minutes under the condition of reaction pressure 0.5MPa, sampling and chromatographic analysis dimethyl carbonate content, the conversion rate is 90.1%.

Embodiment 3

[0032] With 1000ml of acetone as solvent, in raw material proportioning (molar ratio) DMC: TMA=1: 1, reaction temperature is 105 ℃, reaction time is 175 minutes under the condition of reaction pressure 0.8MPa, sampling and chromatographic analysis dimethyl carbonate content, the conversion rate is 88.1%.

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Abstract

The invention discloses a method for preparing tetramethylammonium hydrogen carbonate through condensation reaction by a tubular reactor. The method comprises the following steps that: raw materials dimethyl carbonate (DMC) and trimethylamine (TMA) are mixed with a solvent for preheating with a mol ratio of 0.5-1.5 to 1, and then the mixture enters into the tubular reactor for condensation reaction so as to prepare the tetramethylammonium hydrogen carbonate; and the solvent after reaction is recovered and recycled. The method adopts continuous tubular reaction, and can effectively solve the problems of periodic kettle-type reaction; a device for implementing the method is simple and compact, has small floor space and high service efficiency, and saves the investment; the safety factor of the device is improved to a large extent; the product quality is stable; the production process is simple and concise; and the consumption and the cost are effectively reduced.

Description

technical field [0001] The invention relates to a method for preparing tetramethylammonium bicarbonate, in particular to a method for preparing tetramethylammonium bicarbonate using a tubular reactor. Background technique [0002] Tetramethyl ammonium hydroxide (TAMH) is the most widely used product in electronic chemicals. It is widely used in the production process of liquid crystal and semiconductor chips as a developer and etchant. [0003] TAMH is usually prepared by ammonium chloride electrolysis. The ammonium chloride electrolysis method is through the electrode reaction of the electrolyte. Usually, the aqueous solution of tetramethylammonium chloride is used as the electrolysis raw material, and the electrolysis is performed with an ion-exchange membrane electrolyzer to obtain TMAH at the cathode. The reaction formula is: [0004] [0005] Jiangxi Institute of Chemical Industry Zhang Zhongmin et al. ("Research on Preparation of Tetramethylammonium Hydroxide by E...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/60C07C209/00
Inventor 姚浩川尹云舰吴素芳谭斌
Owner HANGZHOU GREENDA CHEM
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