Continuous hydrogenation method of pyrazine-2-ethyl carboxylate and its application

A technology of ethyl formate and pyrazine, which is applied in the field of continuous hydrogenation of pyrazine-2-ethyl formate, can solve the problems of difficult to control spontaneous combustion of catalyst, large amount of labor in autoclave operation, uncontrollable excessive reduction, etc. Risk of spontaneous combustion, reduced risk of impurity generation, low cost effect

Active Publication Date: 2020-11-06
ASYMCHEM LIFE SCI TIANJIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The main purpose of the present invention is to provide a continuous hydrogenation method of pyrazine-2-ethyl carboxylate and its application to solve the problem of hydrogen and reaction device safety in the existing catalytic hydrogenation reaction process of pyrazine-2-ethyl carboxylate. High performance requirements, high labor and high operation requirements for autoclave operation, catalyst needs to be filtered, difficult to control catalyst spontaneous combustion, long hydrogenation reaction time, low conversion rate and uncontrollable excessive reduction, etc.

Method used

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  • Continuous hydrogenation method of pyrazine-2-ethyl carboxylate and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Dispersion process: disperse ethyl pyrazine-4-carboxylate and hydrogen in collision convection (jet method), the gas-liquid ratio is 1:100, and form a gas-liquid mixture containing small droplets with a particle size of 50nm to 50μm , as the reaction raw material.

[0042] Continuous reaction: Pack 5% Ru / C catalyst in the reaction column. Alumina microspheres (1mm) are used at both ends, the mass of the middle catalyst is 28.38g, the filling height is 300mm, the filling diameter is 19.2mm, and the particle size of the catalyst is 1mm. It is used as the catalytic hydrogenation device 40 (fixed bed reactor).

[0043] The above-mentioned reaction raw materials are continuously passed into the above-mentioned catalytic hydrogenation device 40 (fixed-bed reactor) for catalytic hydrogenation reaction to obtain ethyl piperazine-4-carboxylate, wherein the catalytic hydrogenation device 40 (fixed-bed reactor) is controlled in two stages. temperature, and along the material flow...

Embodiment 2

[0045] Dispersion process: disperse ethyl pyrazine-4-carboxylate and hydrogen in collision convection (jet method), the gas-liquid ratio is 1:100, and form a gas-liquid mixture containing small droplets with a particle size of 50nm to 50μm , as the reaction raw material.

[0046] Continuous reaction: Pack 5% Ru / C catalyst in the reaction column. Alumina microspheres (1mm) are used at both ends, the mass of the middle catalyst is 28.38g, the filling height is 300mm, the filling diameter is 19.2mm, and the particle size of the catalyst is 1mm. It is used as the catalytic hydrogenation device 40 (fixed bed reactor).

[0047] The above-mentioned reaction raw materials are continuously passed into the above-mentioned catalytic hydrogenation device 40 (fixed-bed reactor) for catalytic hydrogenation reaction to obtain ethyl piperazine-4-carboxylate, wherein the catalytic hydrogenation device 40 (fixed-bed reactor) is controlled in two stages. temperature, and along the material flow...

Embodiment 3

[0049] Dispersion process: Disperse ethyl pyrazine-4-carboxylate and hydrogen gas by means of collision convection (jet flow method), with a gas-liquid ratio of 1:100, to form a gas-liquid mixture containing small droplets with a particle size of 50nm to 50μm. as a reaction material.

[0050] Continuous reaction: Pack 5% Ru / C catalyst in the reaction column. Alumina microspheres (1mm) are used at both ends, the mass of the middle catalyst is 28.38g, the filling height is 300mm, the filling diameter is 19.2mm, and the particle size of the catalyst is 1mm. It is used as the catalytic hydrogenation device 40 (fixed bed reactor).

[0051] The above-mentioned reaction raw materials are continuously passed into the above-mentioned catalytic hydrogenation device 40 (fixed-bed reactor) for catalytic hydrogenation reaction to obtain ethyl piperazine-4-carboxylate, wherein the catalytic hydrogenation device 40 (fixed-bed reactor) is controlled in two stages. temperature, and along the ...

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Abstract

The invention provides a continuous hydrogenation method of pyrazine-2-ethyl formate. The continuous hydrogenation method comprises: dispersing a mixture of pyrazine-2-ethyl formate and hydrogen to form a gas-liquid mixture containing small droplets of 50 nm to 5 mm as a reaction raw material; feeding the reaction raw material into a fixed-bed reactor continuously Catalytic hydrogenation is carried out in the reactor, and piperazine-2-ethyl formate is continuously discharged, and the fixed-bed reactor is divided into at least two temperature control sections along the flow direction of the material, and the temperature of the latter temperature control section is lower than The temperature of the previous temperature control section. The above-mentioned forced dispersion process can enable the reaction raw materials to perform high-performance mass transfer in the catalytic hydrogenation reaction process, improve the sufficient reaction degree of the reaction raw materials, and shorten the reaction time. Along the flow direction of the material, the fixed bed reactor is subjected to a segmented temperature control section, which can effectively remove the heat accumulation and control the reaction state in the reactor, and improve the yield, purity and product performance stability of the target product.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a continuous hydrogenation method of ethyl pyrazine-2-carboxylate and its application. Background technique [0002] Ethyl pyrazine-2-carboxylate is a white or light yellow solid. The existing hydrogenation process of ethyl pyrazine-2-carboxylate is carried out in a catalytic hydrogenation reduction reactor, and the whole process is a batch reaction. And the above catalytic hydrogenation reaction process has high safety requirements for hydrogen and reaction equipment, high labor and high operation requirements for autoclave operation, catalyst needs to be filtered, it is difficult to control catalyst spontaneous combustion, long hydrogenation reaction time, low conversion rate and excessive reduction cannot be controlled and product issues. [0003] In view of the existence of the above problems, the application provides a continuous hydrogenation method for ethyl pyrazine-2-c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/04
CPCC07D241/04
Inventor 洪浩洪亮陶建胡忠张岩朱建林王波辉戴瑞智王俊强
Owner ASYMCHEM LIFE SCI TIANJIN
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