Process of resource comprehensive utilization of tungsten crystal-containing mother solution and washing water

A technology for crystallization mother liquor and resource utilization, which is applied in the field of tungsten smelting, can solve the problems such as metatungstate and heteropolysalt cannot be effectively destroyed, limit stable operation and wide application, and affect ion exchange operations, etc., and reduce ammonia nitrogen pollution. The transfer of materials, the speed of process transformation, and the effect of reducing material consumption

Active Publication Date: 2013-11-20
BEIJING CYCLE COLUMBUS ENVIRONMENTAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can recover tungsten and ammonia-containing compounds, the problem is that the metatungstate and heteropolyacid salts in the crystallization mother liquor cannot be effectively destroyed, and the ion exchange operation will eventually be affected after multiple cycles.
[0007] The impact of multiple cycles of CN101838750A on ion exchange limits the stable operation and wide application of this process; CN101607739A and CN1266022A bring secondary pollution while realizing closed loop

Method used

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  • Process of resource comprehensive utilization of tungsten crystal-containing mother solution and washing water

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Experimental program
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Effect test

Embodiment 1

[0041] The ammonium tungstate solution is evaporated and crystallized to produce the crystallization mother liquor of ammonium paratungstate and other products and the washing water produced by washing the ammonium paratungstate with pure water; add sodium hydroxide solution and mix in the mixing reaction kettle to control the alkalinity of the mixed solution at 8.0g / L; The mixed liquid is transported to the packed tower with a pump, steam is directly fed into the bottom of the tower, and the operating pressure in the tower is 0.02MPa. After the ammonia in the tungsten-containing crystallization mother liquor is deammonized by the packed tower, the ammonia-containing steam is recovered as ammonia water through condensation; APT It is converted into sodium tungstate in the packed tower, and the conversion time is about 90 minutes. Part of the converted sodium tungstate solution is refluxed through the circulating water pump, and the reflux flow rate is 1.5 times that of the feed ...

Embodiment 2

[0043] The ammonium tungstate solution is evaporated and crystallized to produce the crystallization mother liquor of ammonium paratungstate and other products and the washing water produced by washing the ammonium paratungstate with pure water; in the mixing reaction kettle, add sodium carbonate solution to adjust the pH of the mixed solution to 10, and then add sodium hydroxide solution, Control the alkalinity of the mixed solution at 9.0g / L; use a pump to transport the mixed solution to the plate tower, and a reboiler is installed at the bottom of the tower to heat the liquid to generate steam. After the deamination treatment of the plate tower, the ammonia-containing vapor is absorbed by hydrochloric acid to prepare ammonium chloride product; APT is converted into sodium tungstate in the plate tower, and the conversion time is about 40 minutes. The converted sodium tungstate solution is partially refluxed through the circulating water pump. The return flow is 2.0 times of t...

Embodiment 3

[0045] The ammonium tungstate solution is evaporated and crystallized to produce the crystallization mother liquor of ammonium paratungstate and other products and the washing water produced by washing ammonium paratungstate with pure water; in the mixing reaction kettle, add sodium bicarbonate solution to adjust the pH of the mixed solution to 10, and then add sodium hydroxide solution , control the alkalinity of the mixed solution at 10.0g / L; use a pump to transport the mixed solution to the composite structure tower, a reboiler is installed at the bottom of the tower to heat the liquid to generate steam, the operating pressure in the tower is 1.2MPa, and the tungsten-containing crystallization mother liquor After the ammonia is deaminated by the composite structure tower, the ammonia-containing steam is recovered as ammonia water through condensation; APT is converted into sodium tungstate in the composite structure tower, and the conversion time is about 30 minutes. The conv...

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Abstract

The invention relates to a process for preparing sodium tungstate and ammonia water and / or an ammonium salt product through resource comprehensive utilization of a tungsten-containing solution, and is applied to a tungsten crystal-containing mother solution and washing water which are produced in a course of preparation of ammonium paratungstate (APT), ammonium metatungstate (AMT) and other products by carrying out evaporation crystallization of an ammonium tungstate solution. The process comprises the following steps: mixing and adding an alkali; preheating; deaminizing and converting; after condensing at a tower top, recycling ammonia water and / or the ammonium salt product; and yielding water from a tower kettle to recycle a sodium tungstate solution as a raw material to be reused in a tungsten smelting system, or to be directly used in production of sodium tungstate or other products. The process can optimize a conventional process course, and has the advantages of simple method, energy saving, emission reduction, low recovery cost, good quality of the recovery product, and high utilization rate of resources.

Description

technical field [0001] The present invention relates to the field of tungsten smelting, in particular, the present invention relates to a process for preparing sodium tungstate, ammonia water and / or ammonium salt through comprehensive utilization of tungsten-containing crystallization mother liquor and washing water. Background technique [0002] Ammonium paratungstate (APT) is an important intermediate product in the tungsten smelting process. At present, the production process of APT products is mainly based on the alkaline method. The wolframite or scheelite concentrate is used to extract and prepare tungsten-containing solution through high-pressure alkali cooking, soda pressure cooking, caustic soda fluoride salt pressure cooking, etc., and then through solvent extraction or ion extraction. The exchange method is purified and concentrated to prepare an ammonium tungstate solution, and finally the APT product is prepared by evaporation and crystallization of the ammonium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00C02F9/04
Inventor 林晓李金涛刘晨明
Owner BEIJING CYCLE COLUMBUS ENVIRONMENTAL SCI & TECH
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