Process for recycling ammonium tungstate from ammonium paratungstate crystallization mother liquor

A crystallization mother liquor, ammonium paratungstate technology, applied in the direction of improvement of process efficiency, tungsten compounds, inorganic chemistry, etc., can solve the problems of high energy consumption, high consumption of auxiliary materials, high production cost, etc., to save energy costs, short process flow, and production The effect of cost reduction

Active Publication Date: 2013-11-06
成都西顿硬质合金有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main purpose of the present invention is to provide a process for recovering ammonium tungstate from the ammonium paratungstate crystallization mother liquor in view of the problems in the above-mentioned prior art that the ammonium paratungstate crystallization mother liquor consumes more ammonium tungstate auxiliary materials, the production cost is high, and the energy consumption is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 This example is a process for recovering ammonium tungstate from ammonium paratungstate crystallization mother liquor

[0046] Including the following steps:

[0047] Step (1): Formation of ammonium tungstophosphate precipitation

[0048] Crystallization mother liquor 500l (WO 3 : 30g / l), add 1.7kg of phosphoric acid (85% phosphoric acid) with a theoretical amount of 300%, stir evenly and let it stand for 30 minutes, add 60l hydrochloric acid under stirring conditions to make the pH value = 0.5, and obtain ammonium tungstophosphate precipitation. Leave for 12 hours;

[0049] Step (2): Ammonium Tungstophosphate Precipitation Ammonia Dissolution

[0050] Add 37l of ammonia water with a mass concentration of 10% into the dissolution tank, heat the temperature to 45°C, add the ammonium dodecatungtophosphate precipitate obtained in step (1) under stirring conditions (make a slurry with 13 l of water to facilitate addition), and control the reaction The temperat...

Embodiment 2

[0053] Example 2 This example is a process for recovering ammonium tungstate from ammonium paratungstate crystallization mother liquor

[0054] Including the following steps:

[0055] Step (1): Formation of ammonium tungstophosphate precipitation

[0056] Crystallization mother liquor 500l (WO 3 :30g / l), add 1.7kg of phosphoric acid (85 phosphoric acid) with a theoretical amount of 300%, stir evenly and let it stand for 30 minutes, add 80l of hydrochloric acid under stirring conditions to make the pH value = 0.3, and obtain ammonium tungstophosphate precipitation. Leave it for 16 hours;

[0057] Step (2): Ammonium Tungstophosphate Precipitation Ammonia Dissolution

[0058] Add 37L of ammonia water with a mass concentration of 10% into the dissolution tank, heat the temperature to 55°C, add the dodeca-tungsten ammonium phosphate precipitation obtained in step (1) under stirring conditions (add 7 l of water to make a slurry, which is convenient to add), and control the reacti...

Embodiment 3

[0061] Example 3 This example is a process for recovering ammonium tungstate from ammonium paratungstate crystallization mother liquor

[0062] Including the following steps:

[0063] Step (1): Formation of ammonium tungstophosphate precipitation

[0064] Crystallization mother liquor 500l (WO 3 :30g / l), add 1.7kg of phosphoric acid (85 phosphoric acid) with a theoretical amount of 300%, stir evenly and let it stand for 30 minutes, add 60l of hydrochloric acid under stirring conditions to make the pH value = 0.5, and obtain ammonium tungstophosphate precipitation. Leave it for 16 hours;

[0065] Step (2): Ammonium Tungstophosphate Precipitation Ammonia Dissolution

[0066] Add 37 l of ammonia water with a mass concentration of 10% into the dissolution tank, heat the temperature to 50°C, and add the ammonium dodecatungtophosphate precipitate obtained in step (1) under stirring conditions (add 10 l of water to make a slurry), and control the reaction temperature at 65 ℃, the...

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Abstract

The invention relates to the technical field of wet smelting of tungsten for production of ammonium paratungstate and particularly discloses a process for recycling ammonium tungstate from ammonium paratungstate crystallization mother liquor. The process comprises the steps of: (1) generating an ammonium dodecatungstophosphate precipitate; (2) dissolving the ammonium dodecatungstophosphate precipitate obtained in the step (2) in ammonia; and (3) removing impurities from a solution obtained in the step (2), then removing molybdenum from the solution in a molybdenum removal groove, and then recycling to obtain an ammonium tungstate solution. Furthermore, the impurity removal in the step (3) includes a phosphorous removal sub-step and a magnesium removal sub-step. According to the process for recycling the ammonium tungstate from the ammonium paratungstate crystallization mother liquor, disclosed by the invention, ammonium tungstate with high purity is obtained, and the production cost is lowered efficiently.

Description

technical field [0001] The invention belongs to the technical field of producing ammonium paratungstate (APT) by tungsten hydrometallurgy, and particularly relates to a new process for recovering ammonium tungstate from ammonium paratungstate crystallization mother liquor. Background technique [0002] my country is the country with the most abundant tungsten reserves in the world. According to the data released by the U.S. Geological Survey in 2006, my country has 1.8 million tons of tungsten reserves, accounting for 61% of the world, of which scheelite is about 70% and wolframite is about 30%. The main technologies of tungsten hydrometallurgy in my country are: acid decomposition of scheelite, alkali pressure cooking-extraction, alkali pressure cooking-ion exchange. Among them, ammonium paratungstate is an important intermediate product in the tungsten smelting process. The classic ammonium paratungstate production process mainly includes ore decomposition, transformatio...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C22B3/44C01G41/00C22B34/36
CPCY02P10/20
Inventor袁茂强肖新志
Owner成都西顿硬质合金有限公司