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Synthesis process of methoxypropylamine

A technology of methoxypropylamine and synthesis process, which is applied in the preparation of amino hydroxyl compounds, the preparation of organic compounds, organic chemistry, etc., can solve the problems of low conversion rate of reaction results, high operation difficulty, low selectivity, etc., and achieve the benefit of large Scale production control, good selectivity, and simple process

Pending Publication Date: 2021-10-29
山东汉鸿新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthetic method of existing methoxypropylamine, with 3-methoxypropanol as raw material, with Cu-Co / Al2O3-diatomaceous earth is catalyst, under certain pressure, temperature condition, 3-methoxypropanol Nitrile is fed into the preheater and mixed with alkali metal hydroxide and hydrogen for preheating and vaporization, and then enters the fixed bed reactor for reaction. After the reaction, the material is condensed and cooled, and the gas and liquid are separated. 3-Methoxypropylamine is extracted as a product, and the system material Recycling, but the technical equipment of the above-mentioned synthesis method is relatively complicated, the operation is difficult, and the conversion rate of the reaction result is low, and the selectivity is low

Method used

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  • Synthesis process of methoxypropylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0019] A kind of synthetic method of 3-methoxypropylamine, take 3-methoxypropionitrile as raw material catalytic hydrogenation:

[0020] Put 400g 3-methoxypropionitrile, 20g ethanol, 12g modified carrier nickel catalyst into a 1000ml autoclave; The pressure was stirred and reacted at 2.8MPa for 2h. After the reaction was completed, the reaction was cooled to room temperature, and then the still liquid was filtered and rectified under normal pressure (collecting fractions at 110-160°C) to obtain 354.09g of colorless and transparent 3-methoxypropylamine. The conversion rate of the raw material obtained after the reaction was analyzed by gas chromatography was 97.0%, and the product yield was 94.52%.

Embodiment example 2～ Embodiment example 6

[0022] The amount of the catalyst used in Example 1 is adjusted, and the rest of the conditions are the same as in Example 1. The conversion rate and total yield of raw materials are shown in the table below.

[0023] implementation 1 2 3 4 5 6 Catalyst addition amount / g 12 0.4 4 20 40 60 Raw material conversion rate / % 97 95.2 96.21 97.23 97.15 97.02 Product yield / % 94.52 92.11 91.68 95.43 95.11 95.86

Embodiment example 7～ Embodiment example 10

[0025] The temperature and pressure conditions in the implementation case 1 are adjusted, and the remaining conditions are equal to the implementation case 1, and the obtained raw material conversion rate and total yield are shown in the following table.

[0026] Implementation case serial number 1 7 8 9 10 temperature / ℃ 90 60 130 90 90 Pressure / MPa 2.80 2.80 2.80 2.00 3.00 Raw material conversion rate / % 97 95.56 97.73 95.11 97.13 Product yield / % 94.52 92.83 94.44 92.55 94.87

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Abstract

The invention discloses a synthesis process of methoxypropylamine. The synthesis process is characterized by comprising the following steps of: (1) taking 3-methoxypropionitrile as a raw material, putting the 3-methoxypropionitrile, a solvent, a modifier and a catalyst into an autoclave, and modifying the catalyst; and (2) at a specific temperature, introducing methylamine / alkali metal hydroxide into the autoclave in vacuum, then introducing hydrogen, heating to a certain temperature, maintaining the pressure intensity at 2-3 MPa, and carrying out a stirring reaction for 2 h to obtain a stirred solution, after the reaction is finished, cooling the autoclave to room temperature, then filtering the stirred solution in the autoclave, and rectifying at normal pressure after filtering to obtain colorless and transparent 3-methoxypropylamine. According to the method, the 3-methoxypropionitrile is used as the raw material and is subjected to catalytic hydrogenation, Compared with the prior art, the method is simple in technological process, high in conversion rate and good in selectivity.

Description

technical field [0001] The present invention relates to the technical field of synthesis of methoxypropylamine, and more specifically relates to a synthesis process of methoxypropylamine. Background technique [0002] The synthetic method of existing methoxypropylamine, with 3-methoxypropanol as raw material, with Cu-Co / Al2O3-diatomaceous earth is catalyst, under certain pressure, temperature condition, 3-methoxypropanol Nitrile is fed into the preheater and mixed with alkali metal hydroxide and hydrogen for preheating and vaporization, and then enters the fixed bed reactor for reaction. After the reaction, the material is condensed and cooled, and the gas and liquid are separated. 3-Methoxypropylamine is extracted as a product, and the system material Recycling, but the technical equipment of the above synthesis method is relatively complicated, the operation is difficult, and the conversion rate of the reaction result is low, and the selectivity is low. Contents of the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/08C07C213/02C07C213/10
CPCC07C213/02C07C213/10C07C217/08
Inventor 刘涛李福同庞宝阳张娟
Owner 山东汉鸿新材料科技有限公司
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