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Comprehensive resource utilization method of tungsten-containing crystallization mother liquor and ammonia-containing steam

A technology of crystallization mother liquor and ammonia vapor, applied in tungsten compounds, chemical instruments and methods, preparation/separation of ammonia, etc., can solve the problems of low concentration of ammonia water recovered by ammonia-containing vapor, high equipment material requirements, and high acid-base consumption cost. , to achieve the effect of reducing material consumption, low operating cost and low cost

Active Publication Date: 2013-08-21
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] The technical solution of the present invention: In order to solve the problems of high acid and alkali consumption cost, excessive ammonia nitrogen, high requirements on equipment materials and low concentration of ammonia water recovered from ammonia-containing steam in the existing crystallization mother liquor treatment process, a tungsten-containing crystallization mother liquor and ammonia-containing steam are provided. The comprehensive resource utilization method, the WO in the crystallization mother liquor 3 It is converted into extremely insoluble calcium tungstate for recovery, and the ammonia-containing steam is proposed to directly enter the rectification tower for concentration treatment without being separated by a condenser, and recover ammonia water or ammonium chloride products. The tungsten and ammonia-containing steam in the crystallization mother liquor Comprehensive utilization of resources, zero pollution discharge during the process, simple operation, cheap raw materials, and easy industrialization

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  • Comprehensive resource utilization method of tungsten-containing crystallization mother liquor and ammonia-containing steam

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Embodiment 1

[0035] WO 3 APT crystallization mother liquor with a content of 20.5g / L; add calcium hydroxide with a theoretical multiple of 1.2 times to the crystallization mother liquor; mix in a mixing reactor, stir the mixture evenly, and pump it into a centrifugal filter for Filtration; the solid phase after filtration is calcium tungstate product for further processing and recovery of WO 3 ; The filtered liquid phase is heated by steam, and the heated solid phase is calcium chloride for further processing and recovery; the heated liquid phase is ammonia-containing steam.

[0036]Ammonium tungstate evaporation and crystallization to prepare ammonium paratungstate (APT) product process; ammonia-containing steam is mixed with the above-mentioned ammonia-containing steam through the pipeline and then enters the packed tower. The operating pressure in the tower is 0.8MPa, and the ammonia-containing steam concentrates ammonia in the packed tower; The steam at the top of the tower is the mix...

Embodiment 2

[0038] WO 3 APT crystallization mother liquor with a content of 32.5g / L; add calcium oxide with a theoretical multiple of 1.5 times to the crystallization mother liquor; after ultrasonic mixing, pump the mixed solution into a plate and frame filter press for pressure filtration; The final solid phase is calcium tungstate product for further processing and recovery of WO 3 ; The liquid phase after pressure filtration is heated by steam, and the heated solid phase is calcium chloride for further treatment and recovery; the heated liquid phase is ammonia-containing steam.

[0039] Ammonium tungstate evaporating and crystallizing ammonium paratungstate (APT) product process to prepare ammonium paratungstate (APT) steam; mixed with the above-mentioned ammonia-containing steam through the pipeline and then entering the plate tower, the operating pressure in the tower is 0.1MPa, and the ammonia-containing steam concentrates ammonia in the plate tower; The steam at the top of the tow...

Embodiment 3

[0041] WO 3 For the APT crystallization mother liquor with a content of 10.0g / L, adjust the pH value to 8 with NaOH; add calcium chloride with a theoretical multiple of 2.0 times to the crystallization mother liquor; after shaking and mixing evenly, pump the mixed solution into a vacuum filter Filtration; the solid phase after filtration is calcium tungstate product for further processing and recovery of WO 3 ; The filtered liquid phase is heated with heat transfer oil, and the heated solid phase is calcium chloride for further processing and recovery; the heated liquid phase is ammonia-containing steam.

[0042] Ammonium tungstate evaporating and crystallizing ammonium paratungstate (APT) product process; ammonia-containing steam mixed with the above-mentioned ammonia-containing steam through the pipeline and then enters the composite structure tower. The operating pressure in the tower is -0.03MPa. Concentration; the steam at the top of the tower is the mixed steam of ammon...

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Abstract

The invention relates to a comprehensive resource utilization method of tungsten-containing crystallization mother liquor and ammonia-containing steam in a process of preparing products including para-ammonium tungstate and the like by evaporating and crystallizing. After the method is implemented, zero-pollution discharge can be realized. Ammonium tungstate crystallization mother liquor and ammonia-containing steam are generated in a process of preparing a para-ammonium tungstate (APT) product by evaporating and crystallizing an ammonium tungstate solution. The comprehensive resource utilization method comprises the following steps of: adding auxiliary materials to react with tungsten in the crystallization mother liquor, wherein the solid phase after solid-liquid separation is a calcium tungstate product, and the liquid phase is a mixed solution of calcium chloride and ammonia; recycling the calcium chloride product by evaporating and recycling the mixed solution of the calcium chloride and the ammonia, wherein the gas phase is ammonia-containing steam; and enabling the ammonia-containing steam generated by calcium chloride evaporation and ammonia-containing steam generated by evaporating and crystallizing to enter a deamination tower after being mixed for recycling to be ammonia water or for further preparing to be an ammonia product. The comprehensive resource utilization method disclosed by the invention is simple to operate, cheap in materials and capable of realizing zero-pollution discharge in the process, so that the tungsten in the crystallization mother liquor and the ammonia in the steam can be recycled, and are easily industrialized.

Description

technical field [0001] The present invention relates to a comprehensive resource utilization method of tungsten-containing crystallization mother liquor and ammonia-containing steam, in particular to a resource comprehensive utilization method of tungsten and ammonia in the process of preparing ammonium paratungstate (APT) products by evaporation and crystallization of ammonium tungstate. Background technique [0002] Ammonium paratungstate (APT) is an important tungsten product, mainly used to manufacture tungsten trioxide or blue tungsten oxide. 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 produce ammonium tungstat...

Claims

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Application Information

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IPC IPC(8): C01G41/00C01C1/02C01C1/16
Inventor 林晓刘晨明曹宏斌
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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