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Continuous production method of Grignard reagent

A production method and Grignard reagent technology, applied in the direction of magnesium organic compounds, can solve the problems of Grignard reaction difficulty, easy flushing, etc., and achieve the effects of improving stability, reducing impact, and saving raw materials

Inactive Publication Date: 2017-05-17
江苏创拓新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] According to the above background, the technical problem solved by the present invention is to solve the difficulty of Grignard reverse initiation in the Grignard reagent synthesis process, the safety problems such as quick and easy heating up, improve the stability of control in the Grignard reaction process, and reduce the impact of human factors on the synthesis. The influence of Grignard reagents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Synthesis of continuous n-butylmagnesium bromide Grignard reagent: two kettles (with an effective volume of 50 L) were used for series reaction.

[0034] Continuous Grignard startup: Add 2.53kg of magnesium, 0.6kg of 1-bromobutane, 1L of tetrahydrofuran, and 3L of toluene to the reaction kettles at all levels, stir, raise the temperature to 90°C, and add 100g of dibromoethane to initiate. After the initiation is successful, Controlled at 90°C with a metering pump to add the following three materials 13.1kg of 1-bromobutane, 20L of tetrahydrofuran, and 20L of toluene dropwise in parallel at a uniform speed. Rate > 98%;

[0035] Continuous Grignard reaction operation: use a metering pump to continuously feed into the first-stage reactor, 1-bromobutane 13.1kg / h, toluene 30L / h, tetrahydrofuran 10L / h, and solid feeder to add magnesium 2kg / h; Feed continuously in the reactor, magnesium 0.43kg / h; primary and secondary reaction temperature is controlled at 90°C, reaction resid...

Embodiment 2

[0037] Synthesis of continuous n-butylmagnesium chloride Grignard reagent: three kettles (with an effective volume of 50 L) were used for series reaction.

[0038] Continuous Grignard startup: Add 2.43kg of magnesium, 0.6kg of 1-chlorobutane, 1L of tetrahydrofuran, and 3L of cyclopentyl methyl ether into the reactors at all levels, stir, raise the temperature to 90°C, and add 100g of dibromoethane to initiate. After the initiation is successful, the following three materials are added dropwise in parallel with a metering pump at a constant speed at 90°C: 8.66kg of 1-chlorobutane, 13.3L of tetrahydrofuran, and 26.7L of cyclopentyl methyl ether. Control, the conversion rate of 1-chlorobutane in all levels of reactor > 98%;

[0039] Continuous Grignard reaction operation: use a metering pump to continuously feed into the primary reactor, 1-chlorobutane 9.26kg / h, cyclopentyl methyl ether 26.7L / h, tetrahydrofuran 13.3L / h, magnesium 1.2kg / h ; Continuous feeding in the secondary rea...

Embodiment 3

[0041] Synthesis of continuous 4-fluorophenylmagnesium chloride Grignard reagent: Four kettles (with an effective volume of 50 L) were used for series reaction.

[0042] Continuous Grignard startup: Add 2.43kg of magnesium, 0.6kg of 4-fluorochlorobenzene, 3L of tetrahydrofuran, and 3L of isopropyl ether into the reactors at all levels, stir, raise the temperature to 70°C, add 100g of dibromoethane to initiate, and the initiation is successful Finally, add the following three materials 12.4kg of 4-fluorochlorobenzene, 20L of tetrahydrofuran, and 20L of isopropyl ether in parallel at a constant speed at 70°C with a metering pump. After the addition, keep warm for 5 hours. The conversion rate of reactors at all levels is >98%;

[0043]Continuous Grignard reaction operation: use a metering pump to continuously feed into the primary reactor: 4-fluorochlorobenzene 13kg / h, isopropyl ether 20L / h, tetrahydrofuran 20L / h, magnesium 0.9kg / h; secondary reactor Continuous feeding in the me...

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Abstract

The invention provides a continuous production method of a Grignard reagent, a mode of connecting n kettles in series is adopted, and the Grignard reagent is obtained through continuous Grignard reaction of halide and magnesium, wherein n is greater than or equal to 2; the production method comprises a continuous Grignard starting step and a continuous Grignard reaction operation step. The method effectively solves the problems of triggering and heat dissipating of the Grignard reaction, the potential safety hazards like blanking or explosion caused by the dramatic temperature rise of the Grignard reaction are avoided, meanwhile, the stability of control in the process of the Grignard reaction is improved, and the influences of human factors on the synthesis of the Grignard reagent are reduced.

Description

technical field [0001] The invention belongs to the field of organic chemical industry; in particular, it relates to a continuous production method of Grignard reagents. Background technique [0002] Halogenated hydrocarbon reacts with metal magnesium in anhydrous ether or tetrahydrofuran to generate alkylmagnesium halide RMgX. This organic magnesium compound is called Grignard reagent. Grignard reagent is one of the most important intermediates in the chemical industry, widely used in the synthesis of pharmaceutical intermediates and material intermediates. [0003] Grignard reagents react with compounds such as aldehydes, ketones, carbon dioxide, and epoxides to produce alcohols, aldehydes, acids, alkyl groups, etc. after hydrolysis. This type of reaction is called a Grignard reaction. There are many literatures on the synthesis of various organic compounds using Grignard reactions. At present, the preparation process of Grignard reagents is mostly a batch method, and in...

Claims

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Application Information

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IPC IPC(8): C07F3/02
CPCC07F3/02
Inventor 叶永靳灿辉谭玉东冯代军
Owner 江苏创拓新材料有限公司
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