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Production technique of high-quality trimethyl orthoacetate

A technology of trimethyl orthoacetate and production process, applied in the field of production technology of high-quality trimethyl orthoacetate, can solve the problems of affecting the purity of trimethyl orthoacetate, having a great influence on the reaction process, unfavorable production costs and the like, and achieving The product quality and yield are stable and reliable, widely applicable, and the effect of improving safety

Inactive Publication Date: 2013-02-13
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the choice of solvent has a great influence on the reaction process. Commonly used solvents with low boiling points in industry, such as n-hexane and carbon tetrachloride, are highly toxic and used in large amounts, which is not conducive to saving production costs.
Simultaneously, the residue of chloride ion has influenced the purity of trimethyl orthoacetate in the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 512.5Kg of acetonitrile, 440Kg of methanol, and 1750Kg of solvent mesitylene into a 5000L enamel reaction kettle, start stirring and freezing brine, cool the materials in the reaction kettle to 0-5°C, and start feeding 502Kg of hydrogen chloride gas, usually about After 10-12 hours, when the ventilation is about to end, properly adjust the valve for entering the frozen brine, and gradually raise the reaction temperature to 20-25°C and start to keep warm, keep warm for 8 hours, and the salt-forming reaction ends, and the intermediate ethyleneimine methyl ether hydrochloride is obtained body.

[0020] Under the conditions of stirring and freezing brine, add 600Kg methanol to the intermediate of ethyleneimine methyl ether hydrochloride, cool the reaction solution to 0-5°C, and add 15-20% ammonia-methanol solution dropwise at 0-5°C , until the pH value of the reaction solution is between 5-6, then according to the amount of methanol used in ammonia methanol, make up the...

Embodiment 2

[0023] Put 512.5Kg of acetonitrile, 440Kg of methanol, and 1800Kg of solvent mesitylene into a 5000L enamel reaction kettle, start stirring and freezing brine, cool the materials in the reaction kettle to 0-5°C, and start feeding 525Kg of hydrogen chloride gas, usually about After 10-12 hours, when the ventilation is about to end, properly adjust the valve for entering the frozen brine, and the reaction temperature gradually rises to 20-25°C to start heat preservation. After 8 hours of heat preservation reaction, the salt-forming reaction is completed, and the intermediate ethyleneimine methyl ether hydrochloride is obtained. body.

[0024] Under the condition of stirring and freezing brine, add 600Kg methanol to the intermediate of ethyleneimine methyl ether hydrochloride, cool the reaction solution to 0-5°C, and add 15-20% ammonia-methanol solution dropwise at 0-5°C , to the pH value of the reaction solution between 5-6, at this time, then according to the amount of methanol...

Embodiment 3 comparative Embodiment 1

[0026] Embodiment 3 comparative example 1: solvent is n-hexane

[0027] With the step described in embodiment 1, difference is to adopt 1400Kg solvent normal hexane to replace above-mentioned 1750Kg solvent mesitylene, the result is: yellow ammonium chloride 730Kg, content: 97.0%, final trimethyl orthoacetate product: 1125Kg, Content: 99.3%, yield: 75%.

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PUM

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Abstract

The invention discloses a production technique of high-quality trimethyl orthoacetate, which comprises the following steps: in the presence of solvent unsym-trimethyl benzene, carrying out salification reaction on acetonitrile, methanol and chlorine hydride to prepare ethyleneimine methyl ether hydrochloride; putting the ethyleneimine methyl ether hydrochloride in a methanol solution, and dropwisely adding an ammonia methanol solution to regulate the pH value; carrying out alcoholysis reaction to obtain a trimethyl orthoacetate crude product; filtering to remove and recycle solid ammonium chloride; adsorbing the filtrate with a strongly alkaline macroporous ion-exchange resin to remove chlorine ions; and finally, carrying out continuous rectification to obtain the trimethyl orthoacetate product of which the content is greater than 99.5% and the yield is greater than 85%. The invention has the advantages of simple technique and high product stability and reliability; and since the used unsym-trimethyl benzene solvent has low toxicity, the trimethyl orthoacetate is safe to use.

Description

technical field [0001] The invention relates to a production process of high-quality trimethyl orthoacetate. Background technique [0002] Trimethyl orthoacetate is a colorless liquid with a special smell. It is mainly used as a chemical intermediate for the production of medicines and pesticides. In the pharmaceutical industry, it is mainly used to synthesize vitamin B1, vitamin A1, sulfadiazine and other drug intermediates; in the agricultural field it is It is an intermediate raw material for the synthesis of pyrethroids such as cypermethrin and kungfuthrin. [0003] The production process of trimethyl orthoacetate that is often reported at present is to use acetonitrile, anhydrous methanol and dry hydrogen chloride as raw materials. Under the action of solvent, a salt-forming reaction is carried out to generate ethyleneimine formamidine hydrochloride. Carry out alcoholysis reaction with methanol to prepare trimethyl orthoacetate. Among them, the choice of solvent has a...

Claims

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Application Information

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IPC IPC(8): C07C43/32C07C41/60C01C1/16
Inventor 周甦谭建平金标
Owner NANTONG TENDENCI CHEM
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