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Method for removing and recovering fluorine and chlorine from zinc sulfate solution

A technology of zinc sulfate solution, fluorine and chlorine, which is applied in the field of metallurgy and chemical industry, can solve the problems of high input cost, easy burning of plates, complicated process, etc., and achieve the effect of reducing desorption cost, increasing disposal cost, and simple process flow

Active Publication Date: 2021-02-12
KUNMING METALLURGY INST +1
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Problems solved by technology

CN102021336A discloses a method of pretreating zinc sulfate solution with zinc powder and calcium oxide, and then using di-(2-ethylhexyl) phosphoric acid to extract zinc, fluorine and chlorine enter the raffinate, and the separation efficiency of zinc and fluorine and chlorine is high more than 95%, but the zinc sulfate solution obtained by stripping will be brought into the organic phase, and the zinc electrolysis process is prone to burning
CN103451449B discloses a method for activated extraction and separation of fluoride and chloride ions in a zinc sulfate solution. The pH and temperature of the fluorine-containing chlorozinc sulfate solution are first adjusted, and then an activator is added to destroy the fluorine-containing metal complex, and the fluorine is converted to HF, and then N235 is used to Fluorine and chlorine ions are extracted by the organic phase composed of 1-octanol as the extractant, TBP as the co-extraction agent, n-octanol as the modifier, and 260# solvent oil as the diluent. , this method has the disadvantages of complicated process and high input cost
Disclosed in CN101492772A is a kind of technology of removing fluorine and chlorine by wet zinc industrialization ion exchange method, it is characterized in that zinc sulfate purification liquid pH2.5~5.5, resolving agent is the sulfuric acid solution of concentration 5~10%, this method has production cost relatively The advantages of low and large processing capacity, however; the disadvantage is that the loss rate of zinc is large, the concentration of fluorine and chlorine in the desorption liquid is not high, and the liquid after desorption directly enters the wastewater treatment, the amount of wastewater treatment is large, and the cost of desorption liquid treatment is high

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  • Method for removing and recovering fluorine and chlorine from zinc sulfate solution

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Effect test

Embodiment 1

[0052] The main components of the fluorine-containing zinc chlorosulfate solution in this embodiment are Zn150g / L, Cl600mg / L, F200mg / L, and the pH of the solution is 2.5-3.0. 20 ion exchange columns (diameter 18mm, height 300mm), each resin column is filled with a mass ratio of 80%: 18%: 2% 201×7, D201, D301 resin mixture type anion resin, to control the flow of liquid It is 1L / h. A total of 20L of solution was processed. The main components of the solution after adsorption were Zn148.2g / L, Cl86.24mg / L, F52.5mg / L, the loss rate of zinc was 1.20%, the removal rate of chlorine was 85.63%, and the removal rate of fluorine was 68.75%.

[0053] The chlorine-fluorine-loaded resin is desorbed with 396g / L sulfuric acid solution, the flow rate of the feed liquid is controlled at 1L / h, and the amount of desorption liquid is 1.2L. After desorption, the liquid contains Cl4170mg / L, F1523mg / L, and the desorption rates of fluorine and chlorine are respectively 96.46% and 97.40%. After the ...

Embodiment 2

[0056] The main components of the fluorine-containing zinc chlorosulfate solution in this embodiment are Zn113g / L, Cl440mg / L, F150mg / L, and the pH of the solution is 2.5-3.0. 5 ion exchange columns (diameter 2300mm, height 5400m), each resin column is filled with a mass ratio of 80%: 15%: 5% 201×7, D201, D301 resin mixture type anion resin. Control the liquid flow rate of 10m 3 / h, the solution temperature is 60~70°C, and the total treatment solution is 240m 3 The main components of the mixed liquid after adsorption are Zn110g / L, Cl21mg / L, F13mg / L, the loss rate of zinc is 2.65%, the removal rate of chlorine is 95.45%, and the removal rate of fluorine is 93.75%.

[0057] The fluorine- and chlorine-loaded resin is desorbed with 196g / L (2mol / L) sulfuric acid solution, and the influent flow rate is controlled at 5 m 3 / h, the amount of desorption liquid is 30L, the desorption liquid contains Cl3840mg / L, F1195mg / L, and the desorption rates of fluorine and chlorine are 96.98% and...

Embodiment 3

[0060] The main components of the fluorine-containing zinc chlorosulfate solution in this embodiment are Zn180g / L, Cl1000mg / L, F800mg / L, and the solution pH2.5~3.0. 20 ion exchange columns (diameter 18mm, height 300mm), each resin column is filled with a mass ratio of 87%: 10%: 3% 201×7, D201, D301 resin mixture type anion resin, to control the inflow flow It is 1L / h. A total of 20L of solution was processed. The main components of the solution after adsorption were Zn148.2g / L, Cl86.24mg / L, F52.5mg / L, the loss rate of zinc was 1.20%, the removal rate of chlorine was 85.63%, and the removal rate of fluorine was 68.75%.

[0061] Fluorine- and chlorine-loaded resin is desorbed with 396g / L sulfuric acid solution, the feed flow rate is controlled to be 1L / h, and the desorption liquid consumption is 1.2L. After desorption, the liquid contains Cl4480mg / L, F2015mg / L, and the desorption rates of fluorine and chlorine are respectively 97.68% and 98.12%. After desorption and regenerati...

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Abstract

The invention discloses a method for removing and recovering fluorine and chlorine from a zinc sulfate solution, which comprises the steps of adsorption, resin regeneration, desorption solution regeneration and fluorine and chlorine recycling, and specifically comprises the following steps: sequentially passing a zinc sulfate solution containing fluorine and chlorine through an ion exchange columnfrom bottom to top to obtain fluorine and chlorine-loaded resin a, carrying out countercurrent desorption by using a sulfuric acid solution to obtain a desorbed solution c, distilling to obtain a regenerated desorption solution d and a mixed gas of HF and HCl, condensing to obtain a hydrofluoric acid product, and absorbing the residual HCl gas with water to obtain a hydrochloric acid product, thereby respectively recycling fluorine and chlorine. The method has the advantages of simple process, recycling of the desorption solution, solving of the problems of large ion exchange desorption solution use amount and large wastewater amount, realization of preparation of hydrofluoric acid and hydrochloric acid products from fluorine and chlorine impurities, high fluorine and chlorine removal efficiency, low production cost, greenness, environmental protection, no generation of three wastes in the process, easiness in connection with a zinc smelting system, and industrial production promotionand application values.

Description

technical field [0001] The invention belongs to the technical field of metallurgy and chemical industry, and in particular relates to a method for removing and recovering fluorine and chlorine from a zinc sulfate solution. Background technique [0002] In the process of wet zinc smelting, the acid leaching slag and zinc-lead slag produced by calcine leaching are processed by high temperature and high acid leaching, Ausmelt, rotary kiln, fuming furnace and other technologies. About 80% of the leaching slag in my country's zinc production is volatilized by rotary kiln or fuming furnace to obtain zinc oxide fumes, and then valuable components such as lead, zinc, germanium, and indium are recovered from zinc oxide fumes. During the volatilization process, most of the fluorine and chlorine are volatilized and enriched in the zinc oxide dust, resulting in a high content of fluorine and chlorine in the zinc oxide dust, which causes great difficulties for the subsequent treatment of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/06C22B19/20C22B3/42C01B7/03C01B7/07C01B7/19
CPCC01G9/06C01G9/003C22B19/26C22B3/42C01B7/035C01B7/0706C01B7/191C01B7/195Y02P10/20
Inventor 邹维杨大锦刘俊场曲洪涛付维琴付光李衍林顾利坤张特牟兴兵翟忠标谢天鉴刁微之闫森
Owner KUNMING METALLURGY INST
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