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Prepn process of acetohydroxamic acid

A technology for the preparation of acetohydroxamic acid, which is applied in the chemical industry to achieve the effect of promoting development

Inactive Publication Date: 2002-12-11
FUSHIDA AGRI SCI & TECH SHAANXI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no public technical report on the production of acetohydroxamic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1, Firstly, hydroxylamine hydrochloride NH 2 OH.HCL and methyl acetate CH 3 COOCH 3 Mix according to the weight ratio of 1:1.1 and place it in a stainless steel reaction kettle with a stirrer and a reflux condenser. The stirring kettle is required to be sealed, and the stirring speed is 1000 rpm; then solid NaOH (containing less than 0.1% of NaCl) is added as a catalyst to To neutralize the hydrochloric acid brought in by hydroxylamine hydrochloride, add solid NaOH in an amount of 90% of the amount of hydrochloric acid brought in by hydroxylamine hydrochloride; then add 80% methanol with the same volume as methyl acetate as a solvent to the reaction vessel; The reaction temperature is controlled at 30℃ and the pressure is controlled at -0.05Mpa, then the synthesis reaction can occur: , Get acetohydroxamic acid.

Embodiment 2

[0012] Example 2, Firstly, hydroxylamine hydrochloride NH 2 OH.HCL and methyl acetate CH 3 COOCH 3 Mix according to the weight ratio of 1:1.2 and place it in a glass-lined reactor with a stirrer and a reflux condenser. The stirrer is required to be sealed, and the stirring speed is 10000rpm; then solid KOH (the amount of KCl is less than 0.1%) is added as a catalyst to To neutralize the hydrochloric acid brought in by hydroxylamine hydrochloride, add solid KOH in an amount of 20% of the amount of hydrochloric acid brought in by hydroxylamine hydrochloride; then add 90% ethanol with the same volume as methyl acetate as a solvent to the reaction vessel; The reaction temperature is controlled at 60℃ and the pressure is controlled at -0.01Mpa, then the synthesis reaction can occur: , Get acetohydroxamic acid.

Embodiment 3

[0013] Example 3, first add hydroxylamine hydrochloride NH 2 OH.HCL and methyl acetate CH 3 COOCH 3 Mix according to the weight ratio of 1:1.3 and place it in a stainless steel reactor with a stirrer and a reflux condenser. The stirrer is required to be sealed, and the stirring speed is 3000 rpm; then solid NaOH (containing less than 0.1% of NaCl) is added as a catalyst to To neutralize the hydrochloric acid brought in by hydroxylamine hydrochloride, add solid NaOH in an amount of 50% of the amount of hydrochloric acid brought in by hydroxylamine hydrochloride; then add 82% methanol with the same volume as methyl acetate as a solvent to the reaction vessel; The reaction temperature is controlled at 50℃ and the pressure is controlled at -0.04Mpa, then the synthesis reaction can occur: , Get acetohydroxamic acid.

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PUM

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Abstract

During the preparation of acetohydroxamic acid, hydroxylamine chloride and methyl acetate are first mixed in a reactor, and solid alkali catalyst to neutralize hydrochloric acid carried by hdyroxylamine chloride and alcohol in the same volume as methyl acetate as solvent are then added, so that a synthetic reaction is effected to produce acetohydroxamic acid. The artificially prepared acetohydroxamic acid has a purity has high as 80% and may be re-compounded into 5% product suitable for use as feed additive. The product may find its wide use in stockbreeding, agriculture, medicine and environment protection.

Description

1. Technical Field [0001] The invention belongs to a preparation process in the chemical field, and particularly relates to a preparation process of acetohydroxamic acid. 2. Background technology [0002] Acetohydroxamic acid is used as a fungicide in medicine, as a urease inhibitor for ruminants in animal husbandry, as a deodorant in environmental protection, and as a long-term fertilizer additive in agriculture. Due to the wide range of uses of acetohydroxamic acid, the demand is great, but the above-mentioned acetohydroxamic acid all appear as a mixture. There is no published technical report on the production of acetohydroxamic acid. Oxime is the reaction product of aldehyde and hydroxylamine, hydroxamic acid is prepared by the reaction of carboxylic acid ester and hydroxylamine, and acetohydroxamic acid is brought into acetyl group. Third, the content of the invention [0003] The purpose of the present invention is to provide a preparation process of acetohydroxamic acid. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/06
Inventor 马新华孔宪铭
Owner FUSHIDA AGRI SCI & TECH SHAANXI
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