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Method for preparing electronic-grade N-methylformamide at low temperature

A technology of methyl formamide and low temperature conditions, which is applied in the field of preparation of electronic grade N-methyl formamide, which can solve the problems of increased heating conditions, equipment corrosion, excessive metal ion content, increased safety of pressure vessels, and production costs. , to achieve the effect of being suitable for large-scale industrial use, extremely fast reaction speed and easy separation

Active Publication Date: 2021-03-26
WUHAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Pressure vessels increase safety issues and production costs in the production process, and heating conditions increase the corrosion of equipment during the reaction process, which can easily lead to excessive metal ion content in the product

Method used

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  • Method for preparing electronic-grade N-methylformamide at low temperature
  • Method for preparing electronic-grade N-methylformamide at low temperature
  • Method for preparing electronic-grade N-methylformamide at low temperature

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Experimental program
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Embodiment Construction

[0025] The specific implementation of the method for preparing electronic-grade N-methylformamide under low temperature conditions involved in the present invention will be described in detail below in conjunction with the accompanying drawings.

[0026]

[0027] Add 30mL of methyl formate to a 100mL glass beaker, add a stirring magnet, put it in a cold trap, cool to -30°C, and then pass 12L of methylamine gas (normal temperature and pressure) into it, and the methylamine gas immediately Liquefied into methylamine liquid, and mixed with methyl formate in the liquid phase to quickly react to generate N-methylformyl and methanol; and then distilled to remove methanol to obtain pure N-methylformamide.

[0028]

[0029] Such as figure 1 and 2 As shown, under the condition of -30°C, the online infrared spectrometer was used to monitor the reaction of methyl formate and methylamine. Will not affect the progress of the reaction.

[0030] In addition, since both methyl formate...

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Abstract

The invention provides a method for preparing electronic-grade N-methylformamide under a saturated low-temperature condition. The method is characterized in that under the normal-pressure low-temperature condition, liquid methyl formate reacts with liquid methylamine with the same mass as the liquid methyl formate to obtain the product N-methylformamide. The whole reaction process is carried out under the low-temperature condition, a high-temperature and high-pressure reaction device is not needed, impurities introduced by corrosion can be reduced as much as possible, and the possibility of introducing the impurities by the reaction device is reduced to the greatest extent, so that the electronic-grade N-methylformamide with extremely high purity can be obtained; and since the reaction iscarried out at normal pressure and low temperature, reaction conditions are easy to control, potential safety hazards are extremely small, and the method is very suitable for large-scale industrialization.

Description

technical field [0001] The invention belongs to the field of synthetic chemistry, and in particular relates to a method for preparing electronic-grade N-methylformamide under low temperature conditions. Background technique [0002] N-methylformamide is an important chemical raw material, which can be used in the synthesis of medicines, pesticides, artificial leather, etc., and is also widely used as a solvent. Especially with the development of the electronics industry, N-methylformamide has been widely used as a cleaning agent in recent years, and its demand is increasing, and ultra-high-purity electronic semiconductor grade N-methylformamide is required. [0003] Although the preparation method of N-methylformamide has been reported, such as by reacting methyl formate and methylamine, the preparation of ultra-high-purity electronic semiconductor-grade N-methylformamide still faces great challenges. The core problem is It is to reduce the content of metal ions in it. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/03
CPCC07C231/02C07C233/03
Inventor 雷爱文张恒崔德文万建龙
Owner WUHAN UNIV
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