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Process for prepn. of dialkyl formanmide

A technology of dialkylformamide and a manufacturing method, which is applied to the preparation of carboxylic acid amides, organic chemical methods, chemical instruments and methods, etc., can solve the problems of difficulty in controlling reaction temperature, accumulation of crystalline by-products, etc. Control becomes difficult, stable continuous production for a long time, and the effect of suppressing accumulation of crystalline by-products

Active Publication Date: 2004-08-11
MITSUBISHI CHEM CORP
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  • Abstract
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Problems solved by technology

[0007] The present invention provides a method for synthesizing dialkylformamide from a mixed gas containing carbon monoxide obtained from gasification of coal or partial oxidation of heavy oil and dialkylamine using alkali metal alkoxide as a catalyst in the presence of alcohol In this method, it solves the defects that crystalline by-products accumulate over time and the control of the reaction temperature becomes difficult, and it is possible to perform continuous operation stably over a long period of time

Method used

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  • Process for prepn. of dialkyl formanmide

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Embodiment 1

[0029] exist figure 1 In this process, the mixed gas obtained by gasification of coal was purified and adjusted to 40% by volume of carbon monoxide, 58.9% by volume of hydrogen, 1.0% by volume of nitrogen, and 0.1% by volume of oxygen. Supply the mixed gas 2800Nm from the lower part of the reaction tower 3 / hr(Nm 3 / hr is the gas flow rate based on 0°C and 101.3kPa, and the carbon monoxide flow rate based on mass is 1400kg / hr), and 2600kg / hr of dimethylamine containing 200mg of water relative to 1kg of dimethylamine, 260kg / hr of methanol, and 24 56 kg / hr of a methanol solution of sodium methoxide in mass % was reacted at a pressure of 2.0 MPa and a temperature of 115°C. The molar ratio of oxygen / sodium methoxide at this time was 0.5. The reaction product is extracted from the top of the reaction tower as a liquid, and the inert gas is extracted from the top of the tower. The dimethylformamide in the reaction product was 4010 kg / hr, and the conversion rate of dimethylamine ...

Embodiment 2

[0031] exist figure 1 In this process, the mixed gas obtained by gasification of coal was purified and adjusted to 40% by volume of carbon monoxide, 58.7% by volume of hydrogen, 1.0% by volume of nitrogen, and 0.3% by volume of oxygen. Supply the mixed gas 2800Nm from the lower part of the reaction tower 3 / hr(Nm 3 / hr is the gas flow rate based on 0°C and 101.3kPa, and the carbon monoxide flow rate based on mass is 1400kg / hr), and 2600kg / hr of dimethylamine containing 200mg of water relative to 1kg of dimethylamine, 260kg / hr of methanol, and 24 The mass % methanol solution of sodium methoxide was 84 kg / hr, and the reaction was carried out at a pressure of 2.0 MPa and a temperature of 115°C. The molar ratio of oxygen / sodium methoxide at this time was 1.0. The reaction product is extracted from the top of the reaction tower as a liquid, and the inert gas is extracted from the top of the tower. The dimethylformamide in the reaction product was 4010 kg / hr, and the conversion ra...

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Abstract

Provided is a method for producing a dialkylformamide suppressing the accumulation of crystalline by-products with time and free from the problem of conventional process comprising the difficult control of the reaction temperature and enabling stable continuous production over a long period. A dialkylformamide is produced from a dialkylamine and carbon monoxide by using an alkali metal alcoholate as a catalyst. The reaction is carried out at an oxygen concentration of <=0.5 vol.% in the mixed raw material gas and an oxygen molar ratio of <=2 in the mixed gas based on the alkali metal alcoholate.

Description

technical field [0001] The present invention relates to a method for producing dialkylformamides from dialkylamines and carbon monoxide using alkali metal alkoxides as catalysts. More specifically, it relates to the use of alkali metal alkoxides as catalysts to synthesize dialkylformamides by reacting a mixed gas containing carbon monoxide and dialkylamines in the presence of alcohol. Background technique [0002] As a representative aprotic polar solvent, dialkylformamide is an important compound widely used in the fiber industry, organic synthesis industry, and the like. [0003] Conventionally, it is well known to use an alkali metal salt of alcohol such as sodium methoxide as a catalyst when dialkylformamide is synthesized from carbon monoxide and dialkylamine under pressure. [0004] In the publication No. 52-45688 of the Japanese Patent Publication, it is described that using an alkali metal salt as a catalyst, in the method for synthesizing a dialkyl formamide from a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/10C07B61/00C07C233/03C07C233/05
Inventor 星野学宗藤明生丹羽洁信兼子功
Owner MITSUBISHI CHEM CORP
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