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United decomposition technology of tungstite, wolframite alkali decomposition

A technology of wolframite and scheelite, applied in the direction of improving process efficiency, etc., can solve the problem of tungsten-alkali separation that has not been fundamentally solved, affects the process of technology industrialization, and has not completely solved the problems of tungsten-alkali separation, so as to save tungsten Alkali separation operation, significant economic and social benefits, and the effect of reducing the cost of three wastes treatment

Inactive Publication Date: 2003-04-16
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkali decomposition method of scheelite has not been well applied in industrial production, the main problem is: the decomposition rate is difficult to improve and stabilize at more than 98%
In order to improve the decomposition rate, it is often necessary to add a large amount of additives, resulting in an increase in production costs; or it is necessary to increase the amount of alkali to 3 to 8 times the theoretical amount, and a large amount of residual alkali must be recovered. The energy consumption of the tungsten-alkali separation process is high. and alkali losses are also greater
Chinese patent 00113250.4 discloses "sodium hydroxide decomposition method of scheelite and black and white tungsten mixed ore". Calcium 3.0~7.0% PO 4 3- , or 20±5% NaF, or 20±5% Na 2 CO 3 , the problems existing in alkali decomposition of scheelite, especially the separation of tungsten and alkali have not been fundamentally resolved
The applicant's patent 00126770.1 proposed a "high-calcium tungsten mineral alkali pressure boiling decomposition method", the amount of sodium hydroxide still reached 1.8 to 4 times the theoretical amount, although the amount has been reduced, but still not completely solved the tungsten alkali The problem of separation has affected the process of industrialization of the technology

Method used

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  • United decomposition technology of tungstite, wolframite alkali decomposition
  • United decomposition technology of tungstite, wolframite alkali decomposition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: A certain scheelite concentrate (WO 3 67.%, Ca11.6%) 0.5Kg, ground to a particle size of 97%-0.045mm, and 630ml of liquid caustic soda added to the autoclave for decomposition, the amount of caustic added is 2.7 times the theoretical amount, solid-liquid ratio 1:1.26, The initial alkalinity is controlled to 500g / l, the autoclave temperature is 190~200℃, the pressure is 0.90~0.95MPa, and the time is 1.5 hours. After the decomposition is complete, dilute and filter, control the alkalinity 180g / l, the temperature is 70~80℃, add the theoretical amount of 1.9% phosphoric acid, after filtering and washing the residue: the tungsten residue contains WO 3 (Total) 0.95%, WO 3 (Soluble) trace amount, the decomposition rate of tungsten is 99.4%. Get 1.3 liters of solution, the solution contains WO 3 234.93g / l, NaOH 136g / l. Transfer this solution to the decomposition of wolframite. Wolframite (including WO 3 67.8%, Ca1.0%) 0.5Kg, after grinding to a particle size of 95%-0.045...

example 2

[0019] Example 2: A certain scheelite concentrate (WO 3 68.22%, Ca11.8%, Mo 0.51%) total 27Kg, ground to a particle size of 96%-0.045mm, add 3.16 times the theoretical amount of alkali into a 50-liter autoclave for decomposition, solid-liquid ratio 1:1.34, control the initial The alkalinity is 550g / l, the autoclaving pressure is 0.9MPa, the temperature is 200°C, and the time is 1.5 hours. In addition, 27Kg of scheelite concentrate from the same ore source is ground to a particle size of 98%-0.045mm, and 3.2 times the theoretical amount of alkali is added to another 50 liters autoclave for decomposition. The solid-liquid ratio is 1:1.5, and the initial alkalinity is controlled as 510g / l, autoclave pressure 0.9MPa, temperature 200℃, time 1.5 hours. After the decomposition is completed, dilute and filter separately, add 1.8% of the theoretical amount of phosphoric acid, control alkalinity 180g / l, temperature 70~80℃, filter and wash the residue: the scheelite residue contains WO 3 (To...

Embodiment 3

[0020] Example 3: A certain scheelite concentrate (WO 3 67.5%, Ca11.8%, Mo0.04%) 700Kg, ground to a particle size of 97%-0.045mm, add 2.0m together with 3.7 times the theoretical amount of alkali 3 The decomposition is carried out in the autoclave, the initial alkalinity is controlled to 514g / l, the autoclave temperature is 195°C, the pressure is 0.9MPa, and the time is 1.5 hours. After the decomposition is completed, dilute and filter, add 9.7% of the theoretical amount of phosphoric acid, control alkalinity 190g / l, temperature 80℃, filter and wash the residue: the tungsten residue contains WO 3 (Total) 1.39%, WO 3 (Soluble) 0.1%, WO in solution 3 182.1g / l, NaOH 190g / l, tungsten decomposition rate 99.26%.

[0021] The filtered solution is transferred to the decomposition of wolframite. Wolframite (WO 3 67.8%, Ca1.0%) 2500Kg, grinded to a particle size of 93%-0.045mm, which is equivalent to 5.5m after filtration 3 Add 10m of the solution and the theoretical amount of 0.92 times ph...

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Abstract

A process for alkaline decomposition of both scheelite and wolframite includes such steps as grinding and pressure-digestion of the two ores in NaOH solution respectively at 140-200 deg.C and under 0.3-1.1 MPa for 1-6 hr, diluting and filtering the decomposed scheelite to obtain a solution of sodium tungstate, and directly using it to decompose the wolframite while adding additive containing PO4 ions. Its advantages are high decomposition percentage (99%), and reduced pollution and low alkali consumption.

Description

Technical field: [0001] The invention belongs to the field of tungsten metallurgical extraction, and particularly relates to the field of extracting tungsten from tungsten mineral raw materials by an alkali decomposition method. Background technique: [0002] As we all know, the raw materials of tungsten-containing minerals use (Fe, Mn)WO 4 Wolframite (Ca≤1.5%), which is mainly morphological, has been widely used in industrial production by alkaline pressure boiling decomposition method, and CaWO 4 The main form of scheelite (Ca content>1.5%) still uses hydrochloric acid decomposition or soda pressure cooking. The alkaline decomposition method of scheelite has not been well applied in industrial production. The main problem is that the decomposition rate is difficult to increase and stabilizes above 98%. In order to increase the decomposition rate, a large number of additives need to be added to the residence, resulting in an increase in production costs; or the amount of alka...

Claims

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Application Information

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IPC IPC(8): C22B3/12
CPCY02P10/20
Inventor 普崇恩谢盛德姚珍刚蒋荣仁李玲孙照华
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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