United decomposition technology of tungstite, wolframite alkali decomposition

A technology of wolframite and scheelite, which is applied in the field of alkali decomposition to extract tungsten from tungsten mineral raw materials and tungsten metallurgical extraction, can solve the problem of tungsten-alkali separation that has not been fundamentally solved, and has not completely solved the problem of tungsten-alkali separation, which affects the technology industry process and other issues, to achieve the effect of saving tungsten-alkali separation operation, significant economic and social benefits, and reducing the cost of three wastes treatment

Inactive Publication Date: 2004-09-15
ZHUZHOU HARD ALLOY GRP CO LTD
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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
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Effect test

Embodiment 1

[0018] Embodiment 1: 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 is added to the autoclave for decomposition, and the amount of NaOH added is based on the amount of WO in the mineral 3 2.7 times the theoretical amount calculated by weight (abbreviated as theoretical amount in the following examples), solid-liquid ratio 1: 1.26, control NaOH initial concentration 500g / L, pressure cooking temperature 190~200°C, pressure 0.90~0.95MPa, time 1.5 hours . After the decomposition is completed, dilute and filter, control the concentration of NaOH to 180g / L, the temperature is 70-80°C, add phosphoric acid, and the amount of addition is PO 4 3- and Ca in scheelite 2+ 1.9% of the theoretically calculated weight of the reaction (abbreviated as theoretical amount in the following examples), after filtering and washing the slag: containing WO in the tungsten slag 3 (total) 0.95%, WO 3 (Soluble) Trac...

example 2

[0019] Example 2: A scheelite concentrate (WO 368.22%, Ca 11.8%, Mo 0.51%) a total of 27Kg, grind to a particle size of 96%-0.045mm, add 3.16 times the theoretical amount of alkali together to decompose in a 50-liter autoclave, the solid-liquid ratio is 1: 1.34, and control the initial NaOH The concentration is 550g / L, the cooking pressure is 0.9MPa, the temperature is 200°C, and the cooking time is 1.5 hours. In addition, 27Kg of scheelite concentrate from the same ore source was ground to a particle size of 98%-0.045mm, and added to another 50-liter autoclave for decomposition together with 3.2 times the theoretical amount of alkali, the solid-liquid ratio was 1:1.5, and the initial concentration of NaOH was controlled to be 510g / L, autoclaving pressure 0.9MPa, temperature 200°C, time 1.5 hours. After the decomposition is completed, dilute and filter respectively, add 1.8% theoretical amount of phosphoric acid each, control NaOH concentration 180g / L, temperature 70-80°C, af...

Embodiment 3

[0020] Embodiment 3: certain scheelite concentrate (WO 3 67.5%, Ca 11.8%, Mo 0.04%) 700Kg, grind to particle size 97%-0.045mm, add 2.0m 3 Decompose in an autoclave, control the initial concentration of NaOH to be 514g / L, cook at a temperature of 195°C, a pressure of 0.9MPa, and a time of 1.5 hours. After the decomposition is completed, dilute and filter, add a theoretical amount of 9.7% phosphoric acid, control the NaOH concentration at 190g / L, and the temperature at 80°C. After filtering and washing the slag: the tungsten slag 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 was transferred to the decomposition of wolframite. Wolframite (WO 3 67.8%, Ca1.0%) 2500Kg, ground to a particle size of 93%-0.045mm, and the above filtered 5.5m 3 The solution and the theoretical amount of 0.92 times phosphoric acid were added together for 10m 3 Decompose in an autoclave, t...

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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, in particular to the field of extracting tungsten from tungsten mineral raw materials by alkali decomposition method. Background technique: [0002] It is well known that (Fe, Mn)WO in tungsten-containing mineral raw materials 4 Wolframite (Ca ≤ 1.5%), which is dominated by morphology, has been widely used in industrial production by alkaline pressure cooking decomposition method, while CaWO 4 Scheelite (Ca content > 1.5%) with the main form is still hydrochloric acid decomposition or soda pressure cooking method used in industry. The alkali decomposition method of scheelite has not been well applied in industrial production, the main problem is: the decomposition rate is difficult to increase 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 i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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