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Preparation method of 3-aminopropanol

A technology of aminopropanol and hydroxypropionitrile, which is applied in the preparation of aminohydroxyl compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of harsh reaction conditions, dangerous raw materials, low yield, etc., and achieve low production costs , high conversion rate and low energy consumption

Active Publication Date: 2019-03-12
昆山市祥和精细化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing high-purity methods have disadvantages such as dangerous raw materials, low yields, and harsh reaction conditions.

Method used

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  • Preparation method of 3-aminopropanol
  • Preparation method of 3-aminopropanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method for 3-aminopropanol, comprising the following steps:

[0022] Inhale the nickel catalyst and silver nitrate into the high-pressure reduction kettle through a vacuum pump, then inhale methanol and 3-hydroxypropionitrile, close the vacuum valve, open the vent valve, replace the air in the kettle with nitrogen, at least three times, 0.2MPa each time and slowly exhaust Vent, close the vent valve and vent valve after the replacement, open the ammonia valve, start stirring, open the jacket cooling water, and feed liquid ammonia; stop stirring after the ammonia is passed, close the ammonia valve, open the hydrogen valve, and replace the hydrogen three times Exclude residual nitrogen, 0.2MPa each time and slowly exhaust and vent. After the replacement, close the valve and then start stirring and open the steam valve to raise the temperature to 45°C and start feeding hydrogen. Keep the pressure in the kettle at 3MPa. The jacket and inner coil of the reduction...

Embodiment 2

[0028] A preparation method for 3-aminopropanol, comprising the following steps:

[0029] Inhale the nickel catalyst and silver nitrate into the high-pressure reduction kettle through a vacuum pump, then inhale methanol and 3-hydroxypropionitrile, close the vacuum valve, open the vent valve, replace the air in the kettle with nitrogen, at least three times, 0.2MPa each time and slowly exhaust Vent, close the vent valve and vent valve after the replacement, open the ammonia valve, start stirring, open the jacket cooling water, and feed liquid ammonia; stop stirring after the ammonia is passed, close the ammonia valve, open the hydrogen valve, and replace the hydrogen three times Exclude residual nitrogen, 0.2MPa each time and slowly exhaust and vent. After the replacement, close the valve and then start stirring and open the steam valve to raise the temperature to 45°C and start feeding hydrogen. Keep the pressure in the kettle at 3MPa. The jacket and inner coil of the reduction...

Embodiment 3

[0035] A preparation method for 3-aminopropanol, comprising the following steps:

[0036] Inhale the nickel catalyst and silver nitrate into the high-pressure reduction kettle through a vacuum pump, then inhale methanol and 3-hydroxypropionitrile, close the vacuum valve, open the vent valve, replace the air in the kettle with nitrogen, at least three times, 0.2MPa each time and slowly exhaust Vent, close the vent valve and vent valve after the replacement, open the ammonia valve, start stirring, open the jacket cooling water, and feed liquid ammonia; stop stirring after the ammonia is passed, close the ammonia valve, open the hydrogen valve, and replace the hydrogen three times Exclude residual nitrogen, 0.2MPa each time and slowly exhaust and vent. After the replacement, close the valve and then start stirring and open the steam valve to raise the temperature to 45°C and start feeding hydrogen. Keep the pressure in the kettle at 3MPa. The jacket and inner coil of the reduction...

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Abstract

The invention provides a preparation method of 3-aminopropanol, which is high in conversion rate. The invention adopts the following technical scheme: adding 3-hydroxypropionitrile into a reactor witha nickel catalyst and silver nitrate, and then adding an amine reagent under nitrogen; then introducing hydrogen into the reactor, stirring for reducing reaction, and performing precipitation and distillation to prepare the 3-aminopropanol. The raw materials are high in utilization rate; the separation process is simple and clear; the energy consumption is low; the production cost of a product islow; and the solvent and the catalyst can be recycled for use.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 3-aminopropanol. Background technique [0002] 3-Aminopropanol is a commonly used drug intermediate for the synthesis of cyclophosphamide, propodin and other drugs. The conventional method is obtained by catalytic hydrogenation of β-hydroxypropionitrile, adding β-hydroxypropionitrile, Rainy nickel, ethanol, and ammonia into an autoclave for reaction, and the resulting 3-aminopropanol has a purity of more than 88% and a yield close to 60% %. 3-Aminopropanol is an important raw material for the production of cosmetics, pharmaceuticals and crop protection compositions, so the quality and purity requirements are very high. The existing high-purity methods have disadvantages such as dangerous raw materials, low yields, and harsh reaction conditions. Contents of the invention [0003] The invention provides a new preparation method of ...

Claims

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Application Information

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IPC IPC(8): C07C215/08C07C213/02C07C213/10
CPCC07C213/02C07C213/10C07C215/08Y02P20/584
Inventor 王阿祥
Owner 昆山市祥和精细化工厂
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