Preparation method of hydroxamic acid or hydroxamic acid salt

A technology of hydroxamic acid salt and hydroxamic acid, which is applied in the direction of organic chemistry, can solve the problems of low reaction efficiency, unfavorable industrial production of hydroxamic acid and its salt, and long reaction time, and achieves the simple operation of the method, Effects of low cost and shortened response time

Active Publication Date: 2014-07-16
岳阳中科华昂精细化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] At present, there is a large amount of wastewater to be treated in the preparation of hydroxamic acid and its salts in alkaline aqueous media, while the existing organic solvent media for the preparation of hydroxamic acids and their salts has low reaction efficiency and long reaction time, which is not conducive to Industrial Production of Hydroxamic Acid and Its Salts

Method used

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  • Preparation method of hydroxamic acid or hydroxamic acid salt
  • Preparation method of hydroxamic acid or hydroxamic acid salt
  • Preparation method of hydroxamic acid or hydroxamic acid salt

Examples

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Embodiment 1

[0040] Synthesis of Benzyl Hydroxamic Acid:

[0041] Add 21g of sodium hydroxide in batches (4g, 4g, 4g, 4g, 5g) into a reaction flask containing 19.2g of hydroxylamine hydrochloride and 150mL of methanol, keep the feed temperature no more than 30°C, after all the sodium hydroxide is added, Then pour 50mL of methanol into the reaction flask, let sodium hydroxide and hydroxylamine hydrochloride react for another 10min, then add 34g of methyl benzoate dropwise into the reaction flask within 30 minutes, then raise the temperature to 50°C, and react for 4 hours. After the reaction, the temperature of the reaction mixture was lowered to below 5°C, and then 7 mL of concentrated sulfuric acid was slowly added to the reaction flask while keeping the addition temperature below 5°C. After the concentrated sulfuric acid was added dropwise, the filtrate was distilled under reduced pressure to remove the methanol solvent to obtain the benzoic hydroxamic acid product. Based on the detection...

Embodiment 2

[0043] Synthesis of salicylhydroxamic acid:

[0044] Replace 34g methyl benzoate with 38g methyl salicylate, carry out hydroximation reaction and prepare salicylic hydroxamic acid at 55 ℃ by the similar technique of embodiment 1, detect based on ferric ion, the yield of salicylic hydroxamic acid is 96%.

Embodiment 3

[0046] Synthesis of Octyl Hydroxamic Acid:

[0047] Using 40g of methyl octanoate instead of 34g of methyl benzoate, octyl hydroxamic acid was prepared by a process similar to that of Example 1. Based on the detection of ferric ions, the yield of octyl hydroxamic acid was 97%.

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Abstract

The invention discloses a preparation method of hydroxamic acid or hydroxamic acid salt. The method comprises the steps of adding alkaline into a methanol solution of a hydroxylamine salt under a stirring condition, then, adding organic carboxylic acid methyl ester to react, distilling to recover methanol after the reaction is ended to obtain a product hydroxamic acid salt; or cooling a reaction system after the reaction is ended, adding concentrated sulfuric acid into the reaction system, and distilling to recover methanol to obtain hydroxamic acid. The method can be used for greatly increasing the yield of hydroxamic acid or hydroxamic acid salt; methanol as a solvent can be recycled, so that wastewater is prevented from being generated; in addition, the preparation method is wild in reaction condition and beneficial to industrial production.

Description

technical field [0001] The invention relates to a preparation method of hydroxamic acid or hydroxamate, belonging to the field of synthesis of flotation collectors. Background technique [0002] Hydroxamic acids and their salts are known flotation collectors for froth flotation of oxide minerals. Former Soviet researchers have found multiple uses of this class of hydroxamic acids, such as described in Pradip and Fuerstenau's "mineral flotation using hydroxamic acid (ester) flotation collectors", reagents in the mineral industry (Reagents in the Minerals Industry), Ed. M. J. Jones and R. Oblatt, Inst. Min. Met., London, 1984, pp. 161-168, a literature review summarizing the flotation applications of hydroxamic acids. Hydroxamic acid is used in the flotation of metals or minerals, such as fluorspar, wolframite, wolframite, cassiterite, muscovite, phosphatite, hematite, pyrolusite, rhodoxene, chrysocolla, malachite Stone, barite, calcite and rare earths. Hydroxamic acids are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/10C07C259/06
Inventor 刘广义张惠丽钟宏刘胜赵刚肖静晶
Owner 岳阳中科华昂精细化工科技有限公司
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