Continuous synthesis method of diazoacetate

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

Active Publication Date: 2019-05-21
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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  • Continuous synthesis method of diazoacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A clean production method for continuous synthesis of pyrethroid intermediate diazoacetate:

[0028] (1) 75kg hydrochloride aqueous solution (glycine methyl ester hydrochloride and 0.1M acetic acid / sodium acetate buffer solution is prepared, the pH value is adjusted to 4.3, wherein the mass fraction of glycine methyl ester hydrochloride is 35%), 45kg sodium nitrite aqueous solution (sodium nitrite mass fraction is 35%), 70kg solvent chloroform is put into the first-level diazotization synthesis kettle together, wherein, the glycine methyl ester hydrochloride in the hydrochloride aqueous solution and the sodium nitrite aqueous solution The molar ratio of sodium nitrite in the solution is 1:1.09; the primary diazotization synthesis is carried out at 12°C, and the reaction is 4h; the primary diazotization synthesis product overflows into the secondary diazotization synthesis kettle, The secondary diazotization synthesis is carried out under the lower pressure, and the reac...

Embodiment 2

[0032](1) 8kg aqueous hydrochloride solution (formed from ethyl glycine hydrochloride and 0.1M acetic acid / sodium acetate buffer solution, the pH value is adjusted to 4.2, wherein the mass fraction of ethyl glycine hydrochloride is 40%), 45kg of sodium nitrite aqueous solution (sodium nitrite mass fraction is 45%), 45kg of solvent 1,2-ethylene dichloride are put into the primary diazotization synthesis kettle together, wherein, glycine ethyl ester hydrochloride in hydrochloride aqueous solution The molar ratio of salt to nitrous acid in the sodium nitrite aqueous solution is 1:1.28; the primary diazotization synthesis is carried out at 5°C, and the reaction is 2h; the primary diazotization synthesis product overflows into the secondary diazotization synthesis kettle , carry out two-stage diazotization synthesis at 5°C, and the reaction time is 2 hours; the secondary diazotization synthesis product overflows into the first-stage settling tank for static stratification, the oil l...

Embodiment 3

[0035] (1) 80kg hydrochloride aqueous solution (prepared from formic acid / sodium formate buffer solution of glycine ethyl ester hydrochloride and 0.1M, the pH value is adjusted to 4.3, wherein the mass fraction of glycine ethyl ester hydrochloride is 40%), 40kg Sodium nitrite aqueous solution (sodium nitrite mass fraction is 50%), 60kg solvent dichloromethane is put into one-stage diazotization synthesis kettle together, wherein, glycine ethyl ester hydrochloride in the hydrochloride aqueous solution and sodium nitrite aqueous solution The molar ratio of nitrous acid is 1:1.26; the primary diazotization synthesis is carried out at 3°C, and the reaction is 1h; Two-stage diazotization synthesis, the reaction time is 3h; the secondary diazotization synthesis product overflows into the first-stage settling tank for static stratification, the oil layer goes to the low-level tank for diazotization, and the water layer overflows to the extraction kettle; Add 60kg of extractant dichlo...

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Abstract

The invention discloses a continuous synthesis method of diazoacetate. The method comprises the following steps: performing a two-stage diazotization synthesis reaction on glycine ester hydrochlorideaqueous solution, sodium nitrite aqueous solution and an organic solvent, performing still standing on a product for layering, enabling an oil layer to enter a diazonium liquid low tank and enabling awater layer to enter an extraction kettle; and adding an extraction agent into the extraction kettle for extraction, continuously performing still standing for layering, enabling a water layer to enter an acidification backflow kettle, enabling an oil layer to enter the diazonium liquid low tank for combination, so as to obtain diazoacetate solution. Acidification backflow, cooling, resin adsorption, negative pressure steaming, dehydration, concentration and centrifugation are performed on the water layer in the acidification backflow kettle, so as to obtain a sodium chloride wet basis and centrifugal mother liquid; the centrifugal mother liquid flows back to the acidification backflow kettle for use; meanwhile, high salt waste water generated by reaction is treated for recycling sodium chloride; and in addition, continuous production of the whole process is achieved, and clean production without discharge of waste water, waste gas and waste residues is achieved.

Description

technical field [0001] The invention relates to a continuous clean production method for synthesizing diazoacetate, in particular to a clean production method for synthesizing important intermediate diazoacetate in the production of pyrethroids, and belongs to the technical field of chemical synthesis. Background technique [0002] Diazocarbonyl compounds, as carbene precursors, are highly reactive reagents. Under the catalysis of transition metal compounds or Lewis acids, many reactions such as cycloaddition reactions, etherification reactions, and insertion of carbon-hydrogen bonds can occur. For the synthesis of many types of organic compounds. The cycloaddition reaction of diazoacetate with alkenes has been used in the industrial production of cyclopropane carboxylates. Due to the potential instability and explosiveness of diazoacetates, these compounds need to be prepared and used immediately. The impurities produced by the side reactions of the diazotization reaction...

Claims

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Application Information

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Patent Type & Authority Applications(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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