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Preparation method of xanthic acid alkyl hydroxamic acid ester

A technology of xanthate alkyl hydroxamate and xanthate, which is applied in the field of preparation of xanthate alkyl hydroxamate, can solve the problem that it is difficult to extract copper sulfide and copper oxide at the same time, the cost of medicine is high, and the Oxidized ore collectors are few and other problems, so as to achieve the effect of easy operation, efficient recovery and quality improvement

Pending Publication Date: 2021-10-08
YUNNAN COPPER CO LTD
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Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of preparation method of xanthate alkyl hydroxamate, to solve the problem of conventional collection in the existing mixed copper ore flotation Collectors are often sulfide ore collectors, and oxide ore collectors are less, and the cost of the reagents is high, so it is difficult to extract copper sulfide and copper oxide from mixed ores at the same time

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  • Preparation method of xanthic acid alkyl hydroxamic acid ester
  • Preparation method of xanthic acid alkyl hydroxamic acid ester

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preparation example Construction

[0025] The invention provides a kind of preparation method of xanthate alkylhydroxamate, it comprises the following steps:

[0026] Step (1): Put the xanthate in a beaker, add distilled water or absolute ethanol, and heat in a water bath under stirring conditions to quickly and completely dissolve the xanthate;

[0027] Step (2): Add a certain amount of carbonic acid and concentrated sulfuric acid to the dissolved xanthate solution to dehydrate the xanthate and carbonic acid to generate a medicament. The reaction formula is as follows:

[0028] Among them, R is selected from C 1 -C 5 Alkyl groups, such as methyl, ethyl, propyl, butyl, isobutyl, pentyl, isopentyl, neopentyl.

[0029] When adding a certain amount of oxalic acid and concentrated sulfuric acid to the dissolved xanthate solution. , make xanthate and oxalic acid undergo dehydration reaction to generate medicament, and its reaction formula is as follows:

[0030] Among them, R is selected from C 1 -C 5 Alky...

Embodiment 1

[0052] Put 172.12g of sodium butylxanthate into a 500ml beaker, add 150ml of distilled water, heat and dissolve in a water bath for 40min at a magnetic stirring speed of 250r / min, and a temperature of 60°C to obtain a sodium butylxanthate solution. Then dropwise the concentrated sulfuric acid of 25.62ml (concentration is 98%) and the oxalic acid of 90g in the solution with the speed of 2 drops / second, maintain reaction temperature to be 105 ℃, react 18h under the condition that magnetic stirrer stirring speed is 250r / min . The product after the reaction was transferred to a separatory funnel and left to stand for 5h, then the organic phase was taken, and the organic phase was washed 3 times with distilled water. Add 69.45 g of hydroxylamine hydrochloride and 40 g of sodium hydroxide to the filtered organic phase (xanthic acid thioformic anhydride), maintain the reaction temperature at 70° C., and react for 18 hours at a magnetic stirrer stirring speed of 250 r / min. The reacte...

Embodiment 2

[0054] Put 15.61g of sodium butyl xanthate into a 500ml beaker, add 150ml of absolute ethanol, heat and dissolve in a water bath for 40min at a magnetic stirring speed of 250r / min and a temperature of 60°C to obtain sodium butyl xanthate solution. Then add dropwise the vitriol oil of 2.56ml (concentration is 98%) and the oxalic acid of 9.0g in the solution with the speed of 2 drops / second, maintain reaction temperature to be 60 ℃, the magnetic stirrer stirring speed is the reaction under the condition of 250r / min 18h. The product after the reaction was transferred to a separatory funnel and left to stand for 5h, then the organic phase was taken, and the organic phase was washed 3 times with distilled water. Add 7 g of hydroxylamine hydrochloride and 4 g of sodium hydroxide to the filtered organic phase (xanthic acid thioformic anhydride), maintain the reaction temperature at 70° C., and react for 18 h at a magnetic stirrer stirring speed of 250 r / min. The reacted product was...

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Abstract

The invention relates to a preparation method of xanthic acid alkyl hydroxamic acid ester. The method comprises the following steps: heating and dissolving xanthate in distilled water or absolute ethyl alcohol, adding carbonic acid (or oxalic acid) and concentrated sulfuric acid to react, standing, taking an organic phase, cleaning with distilled water, and adding hydroxylamine hydrochloride and sodium hydroxide. According to the invention, the prepared collecting agent can well recover copper sulfide and copper oxide in mixed ore while reduce collecting of pyrite and other gangue minerals as much as possible, improves the grade and the recycling rate of flotation copper concentrate of the mixed copper ore, and avoids the problems of difficulty in dispensing, large field investment and inconvenience in inventory management caused by mixed medication.

Description

technical field [0001] The invention belongs to the technical field of organic medicament synthesis, and in particular relates to a preparation method of xanthate alkyl hydroxamate. Background technique [0002] Mixed copper ore is mainly a mixed ore body of copper sulfide and copper oxide. At present, the flotation technology for copper sulfide is relatively mature at home and abroad, but for copper oxide ore, the conventional flotation methods are mainly: direct flotation, sulfide flotation method and chemical beneficiation method. The most widely used in practice is the sulfidation flotation method, which requires the sulfidation of copper oxide first. Therefore, incomplete sulfidation often occurs, resulting in a large amount of copper oxide ore not being effectively recovered, which is lost in the tailings, resulting in a sharp drop in the recovery rate of copper. [0003] The flotation of copper sulfide ore mainly uses xanthate and black medicine sulfide ore collecto...

Claims

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Application Information

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IPC IPC(8): C07C329/06B03D1/012B03D101/02B03D103/02
CPCC07C329/06B03D1/012B03D2201/02B03D2203/02Y02P10/20
Inventor 周仕庆郭芸杉田小松蒋太国朱艳芬
Owner YUNNAN COPPER CO LTD
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