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
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[0025] The invention provides a preparation method of xanthate alkyl hydroxamate, which comprises the following steps:
[0026] Step (1): place the xanthate in a beaker, add distilled water or dehydrated ethanol, and heat in a water bath under agitation to dissolve the xanthate quickly and thoroughly;
[0027] Step (2): add a certain amount of carbonic acid and vitriol oil in the dissolved xanthate solution, make xanthate and carbonic acid generation dehydration reaction, generate medicament, and its reaction formula is as follows:
[0028] where R is selected from C 1 -C 5 alkyl, 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. , dehydration reaction of xanthate and oxalic acid occurs to generate medicament, and its reaction formula is as follows:
[0030] where R is selected from C 1 -C 5 alkyl, such as methyl, ethyl, ...
Example Embodiment
[0051] Example 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 under the conditions of a magnetic stirring speed of 250r / min and a temperature of 60°C to prepare a sodium butylxanthate solution. Then, 25.62ml (98% concentration) of concentrated sulfuric acid and 90g of oxalic acid were added dropwise to the solution at a rate of 2 drops / second, and the reaction was maintained for 18h under the conditions that the reaction temperature was 105°C and the stirring speed of the magnetic stirrer was 250r / min. . Transfer the reacted product to a separatory funnel and let it stand for 5 hours, then take the organic phase and wash the organic phase three times with distilled water. Then, 69.45g of hydroxylamine hydrochloride and 40g of sodium hydroxide were added to the filtered organic phase (xanthogen acid sulfuric anhydride), and the reaction temperature was maintained at 70°C and the stir...
Example Embodiment
[0053] Example 2
[0054] Put 15.61g of sodium butylxanthate into a 500ml beaker, add 150ml of absolute ethanol, heat and dissolve it in a water bath for 40min under the conditions of a magnetic stirring speed of 250r / min and a temperature of 60°C to prepare sodium butylxanthate solution. Then, 2.56 ml (98% concentration) of concentrated sulfuric acid and 9.0 g of oxalic acid were added dropwise to the solution at a rate of 2 drops / second, and the reaction was maintained under the conditions that the reaction temperature was 60 °C and the stirring speed of the magnetic stirrer was 250 r / min. 18h. Transfer the reacted product to a separatory funnel and let it stand for 5 hours, then take the organic phase and wash the organic phase three times with distilled water. Then, 7g of hydroxylamine hydrochloride and 4g of sodium hydroxide were added to the filtered organic phase (xanthogen sulfuric anhydride), and the reaction was maintained for 18h under the condition that the react...
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