Production process of medicinal raw material sodium methoxide

A production process, the technology of sodium methoxide, is applied in the field of production process of sodium methoxide, a medical raw material, which can solve the problems of insufficient utilization of raw materials, high energy consumption of methanol recovery, and easy residue of metal sodium, so as to achieve reasonable design and improve Utilization rate, the effect of simple method

Active Publication Date: 2021-01-22
安徽金邦医药化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction is not complete, the product often contains sodium hydroxide impurity, and sodium hydroxide often has side effects when participating in the pharmaceutical synthesis reaction. It can decompose the ester in the reactant and the product, so the sodium hydroxide in the sodium methoxide will be controlled at a relatively low level. Low range, and the products produced by the alkaline process are often difficult to meet this requirement, which is the main bottleneck restricting the production of the alkaline process
In addition, the removal of water and the recovery of methanol consume a lot of energy, which is also the disadvantage of alkaline production
[0003] At present, it is more convenient to adopt the sodium method to prepare sodium methylate, but the purity of sodium methylate prepared by the sodium method needs to be further improved, and the metal sodium in the process is easy to remain, and other raw materials cannot be fully utilized.

Method used

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  • Production process of medicinal raw material sodium methoxide
  • Production process of medicinal raw material sodium methoxide

Examples

Experimental program
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Effect test

Embodiment 1

[0023] A production process of medicinal raw material sodium methylate, comprising the following steps:

[0024] Step S1: In the reaction kettle, according to the solid-to-liquid mass ratio of 1:10, add molten sodium metal, slowly add the condensed methanol liquid into the reaction kettle under stirring conditions, and continuously feed into the reaction solution in the reaction kettle Nitrogen;

[0025] Step S2: Under normal pressure at 80°C, metal sodium and methanol liquid were reacted for 3 hours, and after the reaction was complete, a mixed solution of sodium methanolate was obtained;

[0026] Step S3: heat-filter the sodium methanolate mixed solution obtained in step S2 to obtain the filter residue and the target solution, the filter residue enters the next process, the target solution is distilled and dried under negative pressure to obtain sodium methoxide, and the discharged methanol gas is condensed and then enters the reaction kettle again continue to react;

[00...

Embodiment 2

[0029] A production process of medicinal raw material sodium methylate, comprising the following steps:

[0030] Step S1: In the reaction kettle, according to the solid-to-liquid mass ratio of 1:11, add molten sodium metal, slowly add the condensed methanol liquid into the reaction kettle under stirring conditions, and continuously feed into the reaction solution in the reaction kettle Nitrogen;

[0031] Step S2: Under normal pressure at 85°C, the metal sodium and methanol liquid were reacted for 2.5 hours. After the reaction was complete, a mixed solution of sodium methanolate was obtained;

[0032] Step S3: heat-filter the sodium methanolate mixed solution obtained in step S2 to obtain the filter residue and the target solution, the filter residue enters the next process, the target solution is distilled and dried under negative pressure to obtain sodium methoxide, and the discharged methanol gas is condensed and then enters the reaction kettle again continue to react;

[...

Embodiment 3

[0035] A production process of medicinal raw material sodium methylate, comprising the following steps:

[0036] Step S1: In the reaction kettle, according to the solid-liquid mass ratio of 1:12, add powdered sodium metal with a particle size of 500nm, slowly add the condensed methanol liquid into the reaction kettle under stirring conditions, and add to the reaction kettle. Continuously inject argon into the liquid;

[0037] Step S2: Under normal pressure at 90°C, metal sodium and methanol liquid were reacted for 2 hours, and after complete reaction, a mixed solution of sodium methanolate was obtained;

[0038] Step S3: heat-filter the sodium methanolate mixed solution obtained in step S2 to obtain the filter residue and the target solution, the filter residue enters the next process, the target solution is distilled and dried under negative pressure to obtain sodium methoxide, and the discharged methanol gas is condensed and then enters the reaction kettle again continue to...

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Abstract

The invention relates to a production process of a medicinal raw material sodium methoxide, which comprises the following steps: proportionally adding metal sodium into a reaction kettle, slowly adding condensed methanol liquid into the reaction kettle while stirring, and continuously introducing inert gas into the reaction kettle; reacting metallic sodium with methanol liquid for 2-3 hours undernormal pressure, and thoroughly reacting to obtain a sodium methoxide mixed solution; performing heat preservation and filtration on the sodium methoxide mixed solution obtained in the step S2, obtaining filter residues and a target solution, enabling the filter residues to enter the next procedure, obtaining sodium methoxide after the target solution is subjected to negative-pressure distillationand drying, and condensing exhausted methanol gas for entering the reaction kettle again for continuous reaction. According to the method, the raw material sodium metal is prepared into molten or nanoscale powder, so that the sodium metal and methanol are fully mixed, the reaction between the sodium metal and methanol is more sufficient, the reaction speed is increased, and the reaction efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of sodium methoxide preparation, in particular to a production technique of medicinal raw material sodium methoxide. Background technique [0002] Sodium methoxide is the most basic sodium alkoxide. It is mainly used as a raw material for the synthesis of medicines and pesticides. It can also be used as a catalyst and analytical reagent for the production of edible oil and biodiesel. It has a good market prospect. At present, the domestic production methods of sodium methoxide mainly include alkali method and metal sodium method, both of which have been industrialized on a large scale. The metal sodium method refers to the direct reaction of metal sodium with alcohol to produce sodium alkoxide and hydrogen. This method has simple process, high product purity and low equipment investment. But the production process is extremely unsafe, and metal sodium is expensive. Alkali method refers to the reaction of s...

Claims

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Application Information

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IPC IPC(8): C07C29/70C07C29/76C07C31/30C07C31/04C01B3/50
CPCC07C29/70C07C29/76C01B3/50C07C31/30C07C31/04
Inventor 余奋玉周章凯衡永刚
Owner 安徽金邦医药化工有限公司
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