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Method for separating and recycling tungsten in alkaline sodium tungstate solution with high chlorine content

A separation and recovery, high-chlorine alkaline technology, applied in chemical instruments and methods, tungsten compounds, alkali metal chlorides, etc., can solve the problems of affecting the ion exchange process and cannot be applied to ion exchange recovery, etc., and achieves simple process and easy operation. , the effect of high recovery rate

Active Publication Date: 2016-03-30
湖北绿钨资源循环有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

According to the provisions of the Environmental Protection Industry Standard of the People's Republic of China "Chlorine Calibration Method for the Determination of Chemical Oxygen Demand in High Chlorine Wastewater", waste water with a chloride ion content greater than 1g / L is high chloride waste water, and for high chloride sodium tungstate solution, Its initial pH is 13.5~14. Because chloride ions are difficult to remove from the solution, it will seriously affect the ion exchange process. Therefore, in the prior art, the perchloric alkaline sodium tungstate solution cannot be recovered by ion exchange. tungsten

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  • Method for separating and recycling tungsten in alkaline sodium tungstate solution with high chlorine content

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Experimental program
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Effect test

Embodiment 1

[0028] Analysis and detection steps: Sampling the sodium perchlortungstate leaching solution, and analyzing and detecting the content of each element in it, the detection results are: Cu4.0mg / L, Ni1.4mg / L, Co2.0mg / L, Mn0.9mg / L, Zn3.6mg / L, Fe0.9mg / L, Ca0.9mg / L, Mg0.8mg / L, Al1.9mg / L, S 2- 15mg / L, W32.5g / L, Cl - 14.8g / L and OH - 5.4g / L.

[0029] Tungsten sinking step: take 5000mL sodium tungstate perchlorate solution, adjust the pH of sodium tungstate solution to 9 with hydrochloric acid, and carry out tungsten sinking with saturated calcium chloride solution, the amount of calcium chloride is CaCl 2 : W=1.15:1 (molar ratio), the temperature is 80°C, and the time is 3 hours to obtain calcium tungstate precipitation and tungsten precipitation mother liquor.

[0030] Concentration and crystallization step: adjust the pH of the tungsten sinking mother liquor obtained in the tungsten sinking step to 7 with hydrochloric acid, and concentrate the solution to obtain pure sodium chlo...

Embodiment 2

[0035] Analysis and detection steps: Sampling the sodium perchlortungstate leaching solution, and analyzing and detecting the content of each element in it, the detection results are: Cu12.0mg / L, Ni7.5.mg / L, Co0.5mg / L, Mn0 .3mg / L, Zn4.2mg / L, Fe0.7mg / L, Ca1.1mg / L, Mg1.0mg / L, Al1.7mg / L, S 2- 20mg / L, W40.9g / L, Cl - 12.0g / L and OH - 16.4g / L.

[0036] Tungsten sinking step: take 5000mL sodium perchlortungstate solution, adjust the pH of the sodium tungstate solution to 13 with hydrochloric acid, and carry out tungsten sinking with saturated calcium chloride solution, the amount of calcium chloride is CaCl 2 : W=1.25:1 (molar ratio), the temperature is 65°C, and the time is 4h, to obtain calcium tungstate precipitation and tungsten precipitation mother liquor.

[0037] Concentration and crystallization step: adjust the pH of the tungsten sinking mother liquor obtained in the tungsten sinking step to 7 with hydrochloric acid, and concentrate the solution to obtain pure sodium chlo...

Embodiment 3

[0042] Analysis and detection steps: Sampling the sodium perchlortungstate leaching solution, and analyzing and detecting the content of each element in it, the detection results are: Cu15.0mg / L, Ni6.4.mg / L, Co3.1mg / L, Mn0 .5mg / L, Zn2.6mg / L, Fe1.5mg / L, Ca3.4mg / L, Mg0.5mg / L, Al2.5mg / L, S 2- 25mg / L, W29.1g / L and Cl - 17.5g / L, OH - 10.1g / L.

[0043] Tungsten sinking step: take 5000mL sodium perchlortungstate solution, adjust the pH of the sodium tungstate solution to 13 with hydrochloric acid, and carry out tungsten sinking with saturated calcium chloride solution, the amount of calcium chloride is CaCl 2 : W=1.15:1 (molar ratio), the temperature is 80°C, and the time is 3 hours to obtain calcium tungstate precipitation and tungsten precipitation mother liquor.

[0044] Concentration and crystallization step: adjust the pH of the tungsten sinking mother liquor obtained in the tungsten sinking step to 7 with hydrochloric acid, and concentrate the solution to obtain pure sodium ...

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Abstract

The invention discloses a method for separating and recycling tungsten in an alkaline sodium tungstate solution with a high chlorine content. The method comprises the following steps: (1) precipitating tungsten: adjusting the pH value of an alkaline sodium tungstate solution with high chlorine content to 9-13 by hydrochloric acid, then adding enough saturated calcium chloride solution to fully carry out reactions so as to precipitate tungsten, washing the precipitate, and filtering to obtain precipitate (calcium tungstate) and a tungsten precipitation mother liquor; (2) alkali decomposition: using sodium phosphate as a leaching agent to fully decompose calcium tungstate in a sodium hydroxide solution to obtain a sodium tungstate solution; (3) ion exchange: subjecting the obtained sodium tungstate solution in the alkali decomposition step to ion exchange according to a convention ion exchange method, and after desorption, performing evaporation and crystallization to obtain high purity secondary ammonium tungstate. According to the method, in the tungsten precipitation step, the tungstate groups in the alkaline sodium tungstate solution with a high chlorine content are precipitated so as to separate the tungstate groups from the chlorine ions; and then obtained calcium tungstate is decomposed by a leaching agent (sodium phosphate) under an alkaline condition so as to obtain a sodium tungstate solution, which can be applied to ion exchange, so that the alkaline sodium tungstate solution with a high chlorine content can be processed by an ion exchanged method to recycle tungsten to obtain a high purity secondary ammonium tungstate product.

Description

technical field [0001] The invention relates to the recycling technology of industrial waste produced in the smelting process of nonferrous metal waste, in particular to a method for separating and recycling tungsten in a perchloric alkaline sodium tungstate solution. Background technique [0002] Industrial waste containing heavy metals such as copper, nickel, cobalt, manganese, and tungsten can be treated in an appropriate way, and the valuable components in it can be recovered, so that the harmless and resourceful utilization of industrial waste can be realized. At present, metal recovery methods for such industrial waste include wet recovery treatment methods: generally, alkali leaching is used, using sodium hydroxide or sodium carbonate as a leaching agent, and tungsten is first leached under normal pressure or pressurized conditions, and tungsten and Other metals are separated, and the obtained tungstate solution is purified and enriched by ion exchange before proceedi...

Claims

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Application Information

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IPC IPC(8): C01G41/00C01D3/04
CPCC01D3/04C01G41/00C01P2006/80
Inventor 张云河熊磊
Owner 湖北绿钨资源循环有限公司
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