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Collecting agent with amide group and thioamide group as well as preparation method and application thereof

A technology of thioamide and amide groups, applied in the field of collectors with amide groups and thioamide groups and their preparation, can solve the problems of no collector reports, achieve good selectivity, and enhance chelation performance , Improve the effect of harvesting ability

Active Publication Date: 2019-04-26
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there is no relevant report on collectors with amido and thioamido groups

Method used

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  • Collecting agent with amide group and thioamide group as well as preparation method and application thereof
  • Collecting agent with amide group and thioamide group as well as preparation method and application thereof
  • Collecting agent with amide group and thioamide group as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation of 3-ethylamino-N-phenyl-3-oxygenide thiopropionamide: 1.04g purity is 95% ethyl isothiocyanate, 1.38g purity is 99% potassium carbonate, 1.77g Add acetoacetanilide with a purity of 98% to 30 mL of absolute ethanol with a purity of 99.7%, stir at room temperature for 30 min, heat the system to reflux, and stir at room temperature for 2.5 h. After the reaction, distill off the ethanol, add 30mL of 10% dilute hydrochloric acid after cooling, stir, filter the resulting precipitate, wash with water, and dry in vacuum to obtain 3-ethylamino-N-phenyl-3-oxylidenethiopropane Amide, the yield (based on acetoacetanilide) is 91.2%, and the proton nuclear magnetic resonance spectrum is as figure 1 As shown, the infrared spectrum as figure 2 As shown, the mass spectrum is as image 3 shown, from Figure 1-3The synthesis of 3-ethylamino-N-phenyl-3-oxylidenethiopropionamide can be further illustrated.

Embodiment 2

[0039] The preparation of 3-ethylamino-N-(tolyl)-3-oxygenide thiopropionamide: 1.91g purity is 99% 2-methyl acetoacetanilide, 1.38g purity is 99% potassium carbonate 1.62 g of phenyl isothiocyanate with a purity of 98% was added to 30 ml of absolute ethanol with a purity of 99.7%, stirred at room temperature for 30 min, the system was heated to reflux, and stirred at room temperature for 2 h. After the reaction, distill ethanol off, add 30mL of 10% dilute hydrochloric acid after cooling, stir, filter the resulting precipitate, wash with water, and dry in vacuo to obtain 3-ethylamino-3-(methylphenyl)-3-oxylidene Thiopropionamide, the yield (based on 2-methylacetoacetanilide) was 84.2%. H NMR spectrum such as Figure 4 shown. from Figure 4 The synthesis of 3-ethylamino-N-(tolyl)-3-oxylidenethiopropionamide could be further confirmed.

Embodiment 3

[0041] The preparation of 3-anilino-N, N-dimethyl-3-oxygenide thiopropionamide: 1.62g purity is 98% phenyl isothiocyanate, 1.38g purity is 99% potassium carbonate, 1.29 g of N,N-dimethylacetoacetamide with a purity of 98% was added to 30 mL of absolute ethanol with a purity of 99.7%, stirred at room temperature for 30 min, the system was heated to reflux, and stirred at room temperature for 1.8 h. After the reaction, distill off the ethanol, add 30mL of 10% dilute hydrochloric acid after cooling, stir, filter the resulting precipitate, wash with water, and dry in vacuum to obtain 3-anilino-N,N-dimethyl-3-oxyethylenesulfur On behalf of propionamide, the yield (based on N,N-dimethylacetoacetamide) is 88.6%, and the proton nuclear magnetic resonance spectrum is as follows: Figure 5 shown. from Figure 5 The synthesis of 3-anilino-N,N-dimethyl-3-oxylidenethiopropionamide can be further illustrated.

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Abstract

The invention relates to a collecting agent with an amide group and a thioamide group as well as a preparation method and application thereof. The collecting agent has both the amide group and the thioamide group and has stronger collecting capacity. The preparation method of the collecting agent comprises the following steps: carrying out a reflux reaction of ester containing an isothiocyano group or ester containing an isothiocyano group and an alkoxycarbonyl group, carbonate and amine containing an acetoacetyl group by taking ethanol as a solvent, removing the ethanol and adding hydrochloric acid, so as to obtain the collecting agent with the amide group and the thioamide group. The invention further provides the application of the collecting agent with the amide group and the thioamidegroup in flotation of metal sulfide minerals. The collecting agent in a structure with the amide group and the thioamide group has stronger collecting capacity for precious metal minerals such as chalcopyrites, galena, gold, silver and the like and also has good selectivity for minerals such as pyrites, sphalerites and the like, and the adaptive scope of the pH value of ore pulp is wide.

Description

technical field [0001] The invention relates to the technical field of mineral flotation, in particular to a collector with amide groups and thioamide groups, a preparation method and application thereof. Background technique [0002] Flotation is a process of selectively enriching the target minerals in the pulp with the help of the buoyancy of the air bubbles to achieve mineral separation based on the differences in the surface properties of the minerals. With the "poor, fine and miscellaneous" ore, there is an urgent need to develop new high-efficiency collectors. The development of new flotation collectors to improve the surface hydrophobicity of mineral particles plays an important role in improving the comprehensive recovery rate of metals. [0003] As a kind of important thiocarboxylic acid derivatives, thioamides have received extensive attention in pharmaceutical synthesis, chemical industry and related fields. Thioamides and their derivatives are widely used in a...

Claims

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Application Information

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IPC IPC(8): B03D1/012B03D1/02B03D101/02B03D103/02
CPCB03D1/012B03D1/02B03D2201/02B03D2203/02
Inventor 钟宏贾云王帅曹占芳
Owner CENT SOUTH UNIV
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