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Production process of high-quality trimethyl orthoacetate

A technology of trimethyl orthoacetate and production process, applied in the field of chemical industry, can solve the problems of great influence on the reaction process, unfavorable production cost, high toxicity, etc., achieves stable and reliable product quality and yield, increases stability, and is widely applicable sexual effect

Inactive Publication Date: 2017-05-24
QINGDAO SENMEIKE CHEM TECH CO LTD
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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

[0015] Put 512.5Kg of acetonitrile, 440Kg of methanol, and 1750Kg of solvent trimethylbenzene into a 5000L enamel reactor, turn on the stirring and freezing brine, cool the contents of the reactor to 0-5°C, and start to pass 502Kg of hydrogen chloride gas, usually about 10-12 hours, when the ventilation is about to end, adjust the frozen brine valve appropriately, the reaction temperature gradually rises to 20-25 ℃ and start the heat preservation, the heat preservation reaction is 8 hours, the salt formation reaction is over, and the ethyleneimine methyl ether hydrochloride is obtained. body. Under the condition of stirring and freezing brine, add 600Kg of methanol to the ethyleneimine methyl ether hydrochloride intermediate, cool the reaction solution to 0-5℃, and add 15-20% ammonia methanol solution dropwise between 0-5℃ , To the pH value of the reaction solution between 5-6, and then according to the amount of methanol used in the ammonia methanol, make up the amount of meth...

Embodiment 2

[0017] Put 512.5Kg of acetonitrile, 440Kg of methanol, and 1800Kg of solvent trimethylbenzene into a 5000L enamel reaction kettle, turn on the stirring and freezing brine, cool the contents of the reaction kettle to 0-5°C, and start to pass hydrogen chloride gas 525Kg, usually about 10-12 hours, when the ventilation is about to end, adjust the frozen brine valve appropriately, the reaction temperature gradually rises to 20-25 ℃ and start the heat preservation, the heat preservation reaction is 8 hours, the salt formation reaction is over, and the ethyleneimine methyl ether hydrochloride is obtained. body. Under the condition of stirring and freezing brine, add 600Kg of methanol to the ethyleneimine methyl ether hydrochloride intermediate, cool the reaction solution to 0-5℃, and add 15-20% ammonia methanol solution dropwise between 0-5℃ , To the pH value of the reaction solution between 5-6. At this time, according to the amount of methanol used in the ammonia methanol, make up ...

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PUM

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Abstract

The invention discloses a production process of high-quality trimethyl orthoacetate. The production process comprises the following steps: performing salification reaction on acetonitrile, methanol and chlorine hydride in the presence of a solvent unsym-trimethyl benzene, so as to obtain ethyleneimine methyl ether hydrochloride; then adding the ethyleneimine methyl ether hydrochloride into a methanol solution; dropwise adding an aminomethanol solution to regulate a pH value, performing alcoholysis reaction to obtain a trimethyl orthoacetate crude product; filtering out solid ammonium chloride, and recycling the solid ammonium chloride; adsorbing filtrate by use of strong-basicity macroporous ion-exchange resin so as to remove chloridion; and finally performing continuous rectification, thereby obtaining a trimethyl orthoacetate product with content greater than 999.5% and yield greater than 85%. The production process is simple in process, the product is stable and reliable, and the used unsym-trimethyl benzene solvent is low in toxicity and safe to use.

Description

Technical field [0001] The invention relates to the field of chemical engineering, in particular to a process for producing high-quality trimethyl orthoacetate. Background technique [0002] Trimethyl orthoacetate is a colorless liquid with a special odor. 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 pharmaceutical intermediates; in the agricultural field, it is Intermediate raw materials for the synthesis of cypermethrin, kungfu pyrethroid and other pyrethroids. [0003] At present, the commonly reported production processes of trimethyl orthoacetate are all using acetonitrile, anhydrous methanol and dry hydrogen chloride as raw materials. Under the action of a solvent, a salt-forming reaction is carried out to produce ethyleneimine formamidine hydrochloride, which is then added Methanol is used for alcoholysis to prepare t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/60C07C43/32
CPCC07C41/60C07C249/04
Inventor 李春梅
Owner QINGDAO SENMEIKE CHEM TECH CO LTD
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