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A kind of continuous synthesis method of diazoacetate

A technology of diazoacetate and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of high ammonia nitrogen and high salt-containing wastewater discharge, low biochemical efficiency of wastewater, difficult biochemical treatment and other problems, and achieve the effect of high yield

Active Publication Date: 2021-11-09
JIANGSU YOUTH CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis yield of diazoacetate is only about 90%, and a large amount of high-ammonia nitrogen and high-salt wastewater is discharged, and the biochemical efficiency of wastewater is low, making it difficult to biochemically treat

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  • A kind of continuous synthesis method of diazoacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A pyrethroid intermediate diazoacetate continuous synthesis clean production methods:

[0028] (1) A 75kg hydrochloride aqueous solution (sodium glycine methyl ester hydrochloride and 0.1M acetic acid / acetate buffer solution preparation, pH value was adjusted to 4.3, wherein the salt of glycine methyl ester hydrochloride mass fraction of 35%), aqueous sodium 45kg (mass fraction of sodium nitrite 35%), placed in a chloroform solvent with 70kg diazotization synthesis reactor, in which the glycine methyl ester hydrochloride aqueous hydrochloric acid and aqueous sodium salt sodium nitrite in a molar ratio of 1: 1.09; synthesis of a diazotized at 12 ℃, 4H reaction; an overflow to a secondary synthesis product diazotized diazonium synthesis reactor, the 8 ℃ carried out under two diazotization synthesis, the reaction time is 4H; two diazotized synthesis product overflows into a settling tank for standing layered reservoir to the lower tank diazonium night, the aqueous layer was ...

Embodiment 2

[0032](1) The 8kg hydrochloride aqueous solution (sodium glycine ethyl ester hydrochloride and 0.1M acetic acid / acetate buffer solution preparation, pH value was adjusted to 4.2 with glycine ethyl ester hydrochloride salt mass fraction of 40%), aqueous sodium 45kg (mass fraction of sodium nitrite 45%), 1,2-dichloroethane solvent together into a diazonium 45kg synthesis reactor, in which the aqueous hydrochloric acid salt of glycine ethyl ester hydrochloride the molar ratio of salt to an aqueous solution of sodium nitrite is 1: 1.28; synthesis of a diazotized at 5 ℃, 2H reaction; an overflow to a secondary diazotized synthesis product in the synthesis reactor diazotization carried out at 5 ℃ two diazotization synthesis, the reaction time is 2H; two diazotized synthesis product overflows into a settling tank for standing layered reservoir to the lower tank diazonium night, the aqueous layer underflow flow to the extraction vessel; 1,2-dichloroethane was added 60kg extractant to th...

Embodiment 3

[0035] (1) A 80kg hydrochloride solution (0.1M glycine ethyl ester hydrochloride and formic acid / sodium formate buffer solution preparation, pH value was adjusted to 4.3, wherein the salt of glycine ethyl ester hydrochloride mass fraction of 40%), 40kg an aqueous solution of sodium (mass fraction of sodium nitrite 50%), into the synthesis reactor together with a diazotized 60kg solvent such as dichloromethane, in which aqueous hydrochloric acid ethyl ester hydrochloride salt with aqueous sodium glycine alkylene molar ratio of nitrous acid is 1: 1.26; diazotized at a 3 ℃ synthesis, the reaction IH; an overflow to a secondary synthesis product diazotized diazonium synthesis pot, and at 3 ℃ two diazotization synthesis, the reaction time is 3H; two diazotized synthesis product overflows into a settling tank for standing layered reservoir to the lower tank diazonium night, the aqueous layer was extracted kettle to overflow; to 60kg kettle was added and extracted with dichloromethane ...

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Abstract

The invention discloses a continuous synthesis method of diazoacetate, in which glycine ester hydrochloride aqueous solution, sodium nitrite aqueous solution, and organic solvent are subjected to two-stage diazotization synthesis reaction, the product is separated and separated, and the oil layer is deweighted Nitrogen liquid low level tank, water layer to the extraction tank; add extractant to the extraction tank for extraction and continue to stand for stratification, the water layer goes to the acidification reflux tank, and the oil layer goes to the diazo liquid low level tank to combine to obtain a diazoacetate solution . The water layer in the acidification reflux kettle is subjected to acidification reflux, cooling, resin adsorption, negative pressure simple steaming, dehydration and concentration, and centrifugation to obtain the sodium chloride wet base and centrifuged mother liquor. The centrifuged mother liquor is returned to the acidification reflux kettle for use mechanically. The wet base is dried to obtain industrial grade sodium chloride. The method of the invention enables the reaction to be fully carried out so as to obtain a high yield, and at the same time, the high-salt wastewater produced by the reaction is treated to recover sodium chloride; and the continuous production of the whole process is tested. Realize clean production without waste water, waste gas and waste residue discharge.

Description

Technical field [0001] The present invention relates to a continuous synthesis diazoacetate clean production method, particularly relates to a cleaning method for producing an important intermediate for the production of a pyrethroid diazoacetate synthetic, belonging to the technical field of chemical synthesis. Background technique [0002] Diazo carbonyl compound as the carbene precursor is a class of highly active reagents, under the catalysis of a transition metal compound or a Lewis acid, cycloaddition reaction of many reactions may occur, and an etherification reaction of the carbon-hydrogen bond insertion and the like. For the synthesis of many types of organic compounds. Diazoacetate cycloaddition reactions with olefins have been used in industrial production cyclopropanecarboxylic acid ester. Because of the potential instability and the explosive diazoacetate, such compounds required by the current system. Diazotization reaction impurities accompanying side reactions oft...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C245/18
Inventor 周其奎何红军汪国庆解春满杨凡吴桂生杨磊
Owner JIANGSU YOUTH CHEM
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