Method for preparing vinyl magnesium chloride

A technology of vinyl magnesium chloride and vinyl chloride, applied in the direction of magnesium organic compounds, etc., can solve the problems of slow solvent absorption rate, low vinyl chloride concentration, hidden dangers in production safety, etc., achieve accurate yield and concentration, and improve concentration and yield. , the effect of increasing solubility

Active Publication Date: 2017-11-24
安徽伟祥新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since vinyl chloride has little solubility in tetrahydrofuran or ether at normal temperature or 0°C and normal pressure, and the rate of absorption by the solvent is also very slow, most of the vinyl chloride gas is released from the reaction system before it can be dissolved and absorbed. The concentration of vinyl chloride in the solvent is very low, the reaction speed is very slow, and the reaction often terminates halfway, which brings great hidden dangers to safe production.

Method used

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  • Method for preparing vinyl magnesium chloride
  • Method for preparing vinyl magnesium chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: prepare vinylmagnesium chloride according to the following specific steps

[0023] (1) Treatment of magnesium chips: take a certain amount of magnesium chips, act for several minutes with a 5% hydrochloric acid solution with a mass concentration, remove the acid solution by suction filtration, wash with water, ethanol, tetrahydrofuran successively, drain and put in a desiccator for subsequent use;

[0024] (2) Check whether there is peroxide in tetrahydrofuran: mix tetrahydrofuran reagent with an equal volume of 2% KI solution, add a few drops of 5% dilute hydrochloric acid and shake together, if the starch solution can turn purple or blue , that is, to prove the presence of peroxide; to remove peroxide is to add a certain amount of tetrahydrofuran and tetrahydrofuran equal volume of FeSO with a mass concentration of 20% in the separatory funnel 4 Solution, after vigorous shaking, the solution will be divided into two layers, the upper layer is the organic...

Embodiment 2

[0028] Embodiment 2: prepare vinylmagnesium chloride according to the following specific steps

[0029](1) Treatment of magnesium chips: take a certain amount of magnesium chips, act for several minutes with a 5% hydrochloric acid solution with a mass concentration, remove the acid solution by suction filtration, wash with water, ethanol, tetrahydrofuran successively, drain and put in a desiccator for subsequent use;

[0030] (2) Check whether there is peroxide in tetrahydrofuran: mix tetrahydrofuran reagent with an equal volume of 2% KI solution, add a few drops of 5% dilute hydrochloric acid and shake together, if the starch solution can turn purple or blue , that is, to prove the presence of peroxide; to remove peroxide is to add a certain amount of tetrahydrofuran and tetrahydrofuran equal volume of FeSO with a mass concentration of 20% in the separatory funnel 4 Solution, after vigorous shaking, the solution will be divided into two layers, the upper layer is the organic ...

Embodiment 3

[0034] Embodiment 3: prepare vinylmagnesium chloride according to the following specific steps

[0035] (1) Treatment of magnesium chips: take a certain amount of magnesium chips, act for several minutes with a 5% hydrochloric acid solution with a mass concentration, remove the acid solution by suction filtration, wash with water, ethanol, tetrahydrofuran successively, drain and put in a desiccator for subsequent use;

[0036] (2) Check whether there is peroxide in tetrahydrofuran: mix tetrahydrofuran reagent with an equal volume of 2% KI solution, add a few drops of 5% dilute hydrochloric acid and shake together, if the starch solution can turn purple or blue , that is, to prove the presence of peroxide; to remove peroxide is to add a certain amount of tetrahydrofuran and tetrahydrofuran equal volume of FeSO with a mass concentration of 20% in the separatory funnel 4 Solution, after vigorous shaking, the solution will be divided into two layers, the upper layer is the organic...

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Abstract

The invention discloses a method for preparing vinyl magnesium chloride. The method comprises the following steps: by taking vinyl chloride and magnesium as raw materials, and taking anhydrous tetrahydrofuran as a solvent, carrying out a Grignard reaction in a pressure-resistant thick-walled glass reactor; after reaction is ended, filtering unreacted magnesium chips so as to obtain a dark-brown solution, namely a Grignard reagent; and performing titrimetric analysis on a small amount of solution, and calculating the concentration and yield of the produced Grignard reagent according to analytical data. According to the method disclosed by the invention, the yield is 70-75%, and the concentration is 1.5mol/l. According to the method disclosed by the invention, the Grignard reaction is carried out between vinyl chloride gases packaged in a steel cylinder and the magnesium chips in anhydrous tetrahydrofuran so as to prepare the vinyl magnesium chloride of a certain concentration, the method is simple, by-products are less and are easily removed, and the product has extremely high industrialization value.

Description

technical field [0001] The invention relates to pharmaceutical and chemical intermediates, in particular to a preparation method of vinylmagnesium chloride. Background technique [0002] At present, industrial-grade vinyl magnesium chloride solutions are generally synthesized by using vinyl chloride and magnesium strips as raw materials, tetrahydrofuran or ether as solvents, and using Grignard reaction. Most of the synthesis techniques adopted are to continuously pass vinyl chloride gas into tetrahydrofuran or ether containing magnesium strips or magnesium powder at normal temperature or about 0°C and normal pressure for reaction. Since vinyl chloride has little solubility in tetrahydrofuran or ether at normal temperature or 0°C and normal pressure, and the rate of absorption by the solvent is also very slow, most of the vinyl chloride gas is released from the reaction system before it can be dissolved and absorbed. Cause the concentration of vinyl chloride in the solvent t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/02
CPCC07F3/02
Inventor 唐鹏飞彭本军张杰张君刘琦胡振东
Owner 安徽伟祥新材料有限公司
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