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Tungsten processing water-cycling and collecting agent recycling method

A collector and water circulation technology, applied in flotation, solid separation, etc., can solve problems such as difficulty in separation of calcium-containing minerals, difficulty in tail water reuse, and large amount of water glass, so as to reduce the cost of chemicals, facilitate operation, and improve flow short effect

Active Publication Date: 2016-06-08
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems such as difficulty in separating calcium-containing minerals, large amount of water glass, low recovery rate, and difficulty in tail water reuse in the traditional fatty acid tungsten ore separation process, the purpose of the present invention is to provide a method for removing calcium-containing mineral inhibitors from water. In the presence of glass, tungsten-containing minerals (scheelite, wolframite, tungsten, etc.) are efficiently enriched by flotation, and at the same time, the tungsten ore beneficiation method is used to recycle the tungsten tailings wastewater; this method not only realizes It ensures the full utilization of collectors, greatly reduces the cost of chemicals, and realizes zero discharge of tungsten mine wastewater, which is conducive to environmental protection

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0057] Mix 1mol / L benzoic acid with 3mol / L anhydrous methanol, slowly add 30mL of concentrated acid, add a few grains of zeolite, heat to 75°C and reflux for 2h. Distill off excess methanol with a distillation device, and the residue is washed 4 times to obtain the corresponding ester; add 2.2 mol of hydroxylamine hydrochloride into a single-necked flask, and add 50 mL of ethanol, stir and cool in a water bath, add 88 g of sodium hydroxide to it, Stir in a water bath for 2 hours, filter out the unacceptable free hydroxylamine to obtain free hydroxylamine hydrochloride; add free hydroxylamine hydrochloride and 25mL methanol to a three-necked flask equipped with an electric stirrer and a dropping funnel, and stir dropwise at 50°C Add 1.7 mol of the obtained ester, react for 45 minutes after the dropwise addition, add 0.5 mol of aluminum sulfate to the solution obtained in the third step under agitation, and react at 40° C. for 1 hour to obtain the metal ion complex collector. fi...

Embodiment 2

[0060] Mix 1mol / L 1-naphthoic acid with 3mol / L anhydrous methanol, slowly add 30mL of concentrated acid, add a few grains of zeolite, heat to 75°C and reflux for 2h. Distill off excess methanol with a distillation device, and the residual liquid is washed 5 times to obtain the corresponding ester; add 2.2 mol of hydroxylamine hydrochloride into a single-necked flask, and add 50 mL of ethanol, stir and cool in a water bath, add 88 g of sodium hydroxide to it, Stir in a water bath for 2 hours, filter out the unacceptable free hydroxylamine to obtain free hydroxylamine hydrochloride; add free hydroxylamine hydrochloride and 25mL methanol to a three-necked flask equipped with an electric stirrer and a dropping funnel, and stir dropwise at 45°C Add 1.7 mol of the obtained ester, react for 45 minutes after the dropwise addition, add 0.125 mol of ferric sulfate to the solution obtained in the third step under stirring conditions, and keep the reaction at 40° C. for 2 hours to obtain t...

Embodiment 3

[0063] Mix 1mol / L salicylic acid with 3mol / L anhydrous methanol, slowly add 30mL of concentrated acid, add a few grains of zeolite, heat to 78°C and reflux for 1h. Distill off excess methanol with a distillation device, and the residual liquid is washed 5 times to obtain the corresponding ester; add 2.2 mol of hydroxylamine hydrochloride into a single-necked flask, and add 50 mL of ethanol, stir and cool in a water bath, add 88 g of sodium hydroxide to it, Stir in a water bath for 1.5h, filter out the unacceptable free hydroxylamine to obtain free hydroxylamine hydrochloride; add free hydroxylamine hydrochloride and 25mL methanol to a three-neck flask equipped with an electric stirrer and a dropping funnel, and stir at 45°C Add 1.7 mol of the obtained ester dropwise, react for 45 minutes after the dropwise addition is completed, add 0.25 mol of zinc sulfate to the solution obtained in the third step under stirring conditions, and react at 40°C for 2 hours to obtain the metal io...

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Abstract

The invention discloses a tungsten processing water-cycling and collecting agent recycling method. The method comprises the steps as follows: crushing and wet grinding of tungsten ores are carried out, so that ore pulp is obtained; deferrization and desulfuration of the ore pulp are carried out sequentially, and then roughing operation is started; during roughing, a metal ion complex serves as a collecting agent; on an inhibitor-free condition, tungsten rough concentrate is roughed and enriched; rougher tailings enter a thickener for concentration operation; an overflow liquid returns to roughing operation; and the tungsten rough concentrate enters concentration operation. According to the method, on the condition that calcium-containing mineral inhibitors such as water glass and the like are not used, efficient floatation concentration of tungsten-containing minerals (scheelite, wolframite, wolfram ocher and the like) and calcium-containing minerals is achieved; and the tailings have excellent natural sedimentation property, so that tailing wastewater of tungsten concentration can be recycled, the collecting agent in return water can be fully recovered and used, not only zero discharge of tungsten mine wastewater is achieved, but also the reagent cost is greatly reduced, and the recovery rate is increased.

Description

technical field [0001] The invention relates to a method for water circulation of tungsten beneficiation and recycling of collectors, belonging to the technical field of tungsten ore beneficiation. Background technique [0002] Tungsten is a precious rare metal, which has the highest melting point, the lowest thermal expansion coefficient, and the lowest vapor pressure among metal elements, and is one of the highest density metal elements. Tungsten has excellent high-temperature mechanical properties, very high compression modulus and With a series of unique properties such as elastic modulus, excellent high temperature creep resistance, high electrical and thermal conductivity, and very high electron emission coefficient, it is widely used in various fields such as civil, industrial, and military industries. For a long time, the mineral resources developed by my country's tungsten industry are mainly wolframite. According to the reserves of black tungsten announced in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B03D1/018B03D1/12B03D101/02B03D103/02
CPCB03D1/018B03D1/12B03D2201/02B03D2203/025
Inventor 孙伟胡岳华韩海生李晓东伏彩萍刘润清黄伟生谢加文陈玉林唐鸿鹄刘杰孟祥松郭衍哲
Owner CENT SOUTH UNIV