Carboxylic ester oximationmethod

A carboxylate, oximation reaction technology, applied in directions such as organic chemistry, can solve problems such as unfavorable industrial production of hydroxamic acid or its salt, high energy consumption, long time, etc., and achieves simplified industrial production process, short time and cost low effect

Active Publication Date: 2019-10-22
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

[0008] However, there is a large amount of waste water to be treated in the preparation of (hydro)hydroxamic acid or its salts in alkaline aqueous medium, while the preparation of (hydro)hydroxamic acid or its salts in organic solvent media requires the recovery of a large amount of organic solvents and high energy consumption , for a long time, these are unfavorable for the industrialized production of (hydro)xamic acid or its salt

Method used

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  • Carboxylic ester oximationmethod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The synthesis of benzoyl (different) sodium hydroxamate:

[0062] 21g sodium hydroxide is added in batches (6g, 5g, 4g, 3g, 3g) in the reactor that 19.2g hydroxylamine hydrochloride and 34g methyl benzoate are housed, fully mix, and keep feed temperature not exceeding 40 ℃, wait After all the sodium hydroxide was added, the temperature was raised to 50° C., and the reaction was carried out for 4 hours. After the reaction, the sodium benzoic acid (hydro)hydroxamate product was obtained. Based on the color reaction of ferric ions, the yield of sodium benzoic acid (hydro)hydroxamate was 98.6%.

Embodiment 2

[0064] Synthesis of Benzene (iso)hydroxamic acid:

[0065] 21g sodium hydroxide is added in batches (6g, 5g, 4g, 3g, 3g) in the reactor that 19.2g hydroxylamine hydrochloride and 34g methyl benzoate are housed, fully mix, and keep feed temperature not exceeding 40 ℃, wait After all the sodium hydroxide was added, the temperature was raised to 50° C., and the reaction was carried out for 4 hours. With sufficient mixing, the temperature of the reaction mixture was lowered below 10°C, and then 7mL of concentrated sulfuric acid was slowly added to the reactor while keeping the feed temperature below 10°C to obtain the benzyl (hydro)hydroxamic acid product based on ferric iron Ion chromogenic detection showed that the yield of benzoic acid (hydro)xamic acid was 98.3%.

Embodiment 3

[0067] Synthesis of Sodium Salicyl (iso)hydroxamic acid:

[0068] Compared with Example 1, the difference is only that, with 38g methyl salicylate instead of 34g methyl benzoate, the hydroximation reaction is carried out at 55° C. to prepare sodium salicylic (iso)hydroxamic acid by the similar technique of embodiment 1 , based on the detection of ferric ions, the yield of sodium salicyl (iso)hydroxamic acid was 98.3%.

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Abstract

The invention discloses method for preparing(iso)hydroxamic acid salt or (iso)hydroxamic acid. The method for preparing (iso)hydroxamic acid salt or (iso)hydroxamic acidcomprises the steps that analkali, a hydroxylamine salt, and an organic carboxylic acid ester are directly subjected to hybrid reaction without an extra solvent, and thusan (iso) hydroxamic acid salt product is obtained; and or after the reaction is completed, a reaction system is cooled, an acid is added to the reaction system to obtain (iso)hydroxamic acid.According to themethod for preparing (iso)hydroxamic acid salt or (iso)hydroxamic acid,the (iso)hydroxamic acid salt or the (iso)hydroxamic acidcan be obtainedwith near atomic economy without additional organic solvents or water being added, environment-friendly effectis achieved, simpleness and efficiency are achieved, and industrial production is advantageous.

Description

technical field [0001] The invention belongs to the field of smelting agent synthesis, and in particular relates to a method for preparing (hydro)hydroxamate or (hydro)hydroxamic acid by using carboxylic acid ester through oximation reaction. Background technique [0002] (Hydro)hydroxamic acid and its salts are widely used in flotation collectors and metallurgical extractants. Researchers in the former Soviet Union discovered a variety of beneficiation and smelting uses of this type of (hydro)hydroxamic acid; Pradip and Fuerstenau's "Mineral Flotation Using (Hydro) Hydroxamic Acid (Ester) Flotation Collectors", "Mineral Flotation 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, pho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C259/06C07C259/08C07C259/10
CPCC07C259/06C07C259/08C07C259/10
Inventor 刘广义
Owner 岳阳中科华昂精细化工科技有限公司
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