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Method for preparing hydroximic acid derivatives by solid state process

A technology for preparing hydroxamic acid and solid-state method, which is applied in the field of preparation of hydroxamic acid derivatives by solid-state method, can solve problems such as wastewater discharge and industrial discharge problems, and achieve easy control of the reaction, short synthesis process, and strong chelation Effect

Active Publication Date: 2018-12-04
HUNAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, whether water or alcohol is used as a solvent, the use of the above-mentioned solvent method will cause wastewater discharge problems, which requires a large amount of post-treatment, and will also cause industrial discharge problems.

Method used

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  • Method for preparing hydroximic acid derivatives by solid state process
  • Method for preparing hydroximic acid derivatives by solid state process
  • Method for preparing hydroximic acid derivatives by solid state process

Examples

Experimental program
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Embodiment 1

[0029] Preparation of benzohydroxamic acid

[0030] Control the temperature of the reactor to be room temperature, add 13.60 parts of methyl benzoate and 6.95 parts of hydroxylamine hydrochloride to the reactor with a purity of 99%, add and then add 8.00 parts of sodium hydroxide to the above-mentioned reactor, grind or ball mill, and react 5 After ~30 minutes, the obtained solid is sodium benzohydroxamic acid. After drying, the detection purity was 75.6% (the impurity was sodium chloride), the yield was 95%, and the product was confirmed as the target product by mass spectrometry.

Embodiment 2

[0032] Preparation of n-octyl hydroxamic acid

[0033] Control the temperature of the reactor to be room temperature, add 17.22 parts of ethyl n-octanoate and 8.2 parts of hydroxylamine sulfate into the reactor with a purity of 99%, add and then add 11.2 parts of potassium hydroxide into the above-mentioned reactor, grind or ball mill, and react 5 After ~30 minutes, the obtained solid is sodium octylhydroxamate. After drying, the detection purity was 71% (the impurity was potassium chloride), and the yield was 96%. The product was confirmed as the target product by mass spectrometry.

Embodiment 3

[0035] Preparation of n-decyl hydroxamic acid

[0036] Control the temperature of the reactor to be room temperature, add 21.42 parts of isopropyl n-decanoate and 6.40 parts of hydroxylamine carbonate to the reactor with a purity of 99%, add and then add 8.00 parts of potassium hydroxide to the above-mentioned reactor, grind or ball mill, After reacting for 5-30 minutes, the obtained solid is potassium n-decylhydroxamate. After drying, the detection purity was 74.6% (the impurity was potassium chloride), the yield was 95%, and the product was confirmed as the target product by mass spectrometry.

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Abstract

The invention discloses a method for preparing hydroxamic acid derivatives by a solid state process. The method comprises the following steps: mixing an ester, hydroxylamine and an alkali substance, performing solid-state grinding or ball milling, and carrying out a reaction to obtain the hydroxamic acid derivatives. The method of the invention has the advantages of mild reaction conditions, highyield, low cost, easiness in operation, short production cycle, no solvent, no emission, greenness and environmental protection, and can meet industrial production.

Description

technical field [0001] The invention belongs to the field of synthesis of metal ore flotation collectors, in particular to a method for preparing hydroxamic acid derivatives by a solid-state method. Background technique [0002] Hydroxamic acid, also known as hydroxamic acid, hydroxamic acid, acyl hydroxylamine. Hydroxamic acid is an important class of metal complexing agents, which has attracted great research interest due to its special structure and corresponding physical and chemical properties. The ability of hydroxamic acid to chelate metal ions (Fe, Zn, W, Ca, Cu, Cr, Co, Mn, etc.) has been widely studied in the fields of biology, medicine and chemical industry. Hydroxamic acid has been widely used as a chelating collector for mineral flotation, such as benzohydroxamic acid and octyl hydroxamic acid have been used as iron ore, copper ore, tin ore, tungsten ore, rare earth ore, etc. Flotation collector for oxide ore. [0003] At present, the commonly used synthetic ...

Claims

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Application Information

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IPC IPC(8): C07C259/10C07C259/06
CPCC07C259/06C07C259/10
Inventor 邓兰青黄志强唐昱黄颖周媛静任倩
Owner HUNAN UNIV OF CHINESE MEDICINE