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Method for preparing high-purity ammonium metavanadate from spent catalyst

A waste catalyst and ammonium metavanadate technology, which is applied in the preparation of vanadium compounds, chemical instruments and methods, vanadium compounds, etc., can solve the problems of inability to prepare high-purity ammonium metavanadate, achieve low cost, solve molybdenum entrainment, The effect of short process

Active Publication Date: 2015-05-20
DALIAN DONGTAI RESOURCE RENEWABLE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can effectively remove vanadium in molybdate solution, but these resins also adsorb a small amount of molybdenum while adsorbing vanadium.
High-purity ammonium metavanadate cannot be prepared even by chemical precipitation of vanadium in analytical solution

Method used

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  • Method for preparing high-purity ammonium metavanadate from spent catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] After the spent catalyst is leached and filtered, 26m 3 The leaching solution contains 0.67g / L of phosphorus, 12.73g / L of molybdenum, and 17.81g / L of vanadium.

[0021] (1) Phosphorus removal

[0022] Adjust the pH value of the leaching solution to 6.5, enter the ion exchange system, pass through the ion exchange column, and use gel-type anion exchange resin to adsorb phosphorus in the leaching solution. Adjust the valve to control the feed flow rate to 0.2 times the column volume. After testing, after 270 minutes of contact between the feed liquid and the resin, the phosphorus content in the effluent is greater than 2ppm, the resin is saturated, and the adsorption is stopped immediately.

[0023] The resin is rinsed and analyzed with 4% ammonia solution, and the regeneration is completed at the same time. After the ammonium phosphate solution is concentrated and crystallized, it can be used for the production of phosphate fertilizer.

[0024] (2) Separation of molyb...

Embodiment 2

[0031] After the spent catalyst was leached and filtered, 24.6m 3 The leaching solution contains 1.34g / L of phosphorus, 12.72g / L of molybdenum, and 18.16g / L of vanadium.

[0032] (1) Phosphorus removal

[0033] Adjust the pH value of the leaching solution to 7, enter the ion exchange system, pass through the ion exchange column, and use gel-type anion exchange resin to adsorb phosphorus in the leaching solution. Adjust the valve to control the feed flow rate to be 0.5 times the column volume. After testing, after 200 minutes of contact between the feed liquid and the resin, the phosphorus content in the effluent is greater than 2ppm, the resin is saturated, and the adsorption is stopped immediately.

[0034] The resin is rinsed and analyzed with 4.2% ammonia solution, and the regeneration is completed at the same time. After the ammonium phosphate solution is concentrated and crystallized, it can be used for the production of phosphate fertilizer.

[0035] (2) Separation of...

Embodiment 3

[0042] After the spent catalyst was leached and filtered, 21.3m 3 The leach solution contains 1.55g / L phosphorus, 18.97g / L molybdenum and 23.2g / L vanadium.

[0043] (1) Phosphorus removal

[0044]Adjust the pH value of the leaching solution to 7.5, enter the ion exchange system, pass through the ion exchange column, and use gel-type anion exchange resin to adsorb phosphorus in the leaching solution. Adjust the valve to control the feed flow rate to be 1 times the column volume. After testing, after 150 minutes of contact between the feed liquid and the resin, the phosphorus content in the effluent is greater than 2ppm, the resin is saturated, and the adsorption is stopped immediately.

[0045] The resin is rinsed and analyzed with 4.4% ammonia solution, and the regeneration is completed at the same time. After the ammonium phosphate solution is concentrated and crystallized, it can be used for the production of phosphate fertilizer.

[0046] (2) Separation of molybdenum and...

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Abstract

The invention discloses a method for preparing high-purity ammonium metavanadate from a spent catalyst, which comprises the following steps: dephosphorization: collecting a spent catalyst leach solution in a leaching mode, filtering the leach solution, sending into an ion-exchange dephosphorization system, and carrying out phosphorus adsorption on the spent catalyst leach solution by using a resin; molybdenum-vanadium separation: sending the dephosphorized molybdenum / vanadium-containing solution into an ion-exchange system, and carrying out molybdenum adsorption by using a resin to separate the molybdenum and vanadium; and vanadium precipitation: pumping the vanadium-containing mother solution subjected to dephosphorization and separation molybdenum into a vanadium precipitation tank, and precipitating vanadium by using a weakly alkaline ammonium salt to obtain the high-purity ammonium metavanadate product. The method has the characteristics of short process, simple technique, energy saving, environmental protection, high efficiency, low cost and the like.

Description

technical field [0001] The present invention proposes a method for preparing high-purity ammonium metavanadate from molybdenum-vanadium-containing waste catalyst, which is a separation and purification technology for preparing high-purity ammonium metavanadate by combining molybdenum-vanadium ion exchange separation and chemical precipitation method, which belongs to chemical industry separation and purification field. Background technique [0002] Rare metals such as molybdenum and vanadium are contained in the spent oil refinery catalysts. During the treatment and disposal process, due to the very similar properties of vanadium and molybdenum, after wet leaching of molybdenum and vanadium ions to remove impurities, chemical precipitation of vanadium to prepare ammonium metavanadate is due to molybdenum entrainment. , can only make 98.5% refined vanadium, and cannot do one-time precipitation of vanadium to prepare high-purity ammonium metavanadate. If the traditional proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/003C01P2006/80
Inventor 李俊梁昌雄邵成志刘忠军迟洪建于校生管殿春
Owner DALIAN DONGTAI RESOURCE RENEWABLE
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