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Method for high-efficiency preparation of high-purity sodium metavanadate

A technology of sodium metavanadate and sodium ammonium vanadate, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problem that the industrial powdery vanadium pentoxide is expensive and the powdery vanadium pentoxide has high quality requirements. , Incomplete removal of impurities by crystallization, etc., to achieve the effect of avoiding impurity wrapping, stable product quality, crystallization efficiency and yield improvement

Inactive Publication Date: 2017-12-01
PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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Problems solved by technology

This method is simple to operate and does not produce polluting waste gas (ammonia), and is currently the most widely used method. However, this method has higher requirements on the quality of powdered vanadium pentoxide, and at the same time, the price of industrial powdered vanadium pentoxide is relatively expensive. , high production cost
Another method is to evaporate and crystallize the vanadium-extracting leaching solution after removing impurities, so as to obtain sodium metavanadate solid. This method is simple in process and convenient to operate, but the components of the vanadium-extracting leaching solution are complex, and impurities are not completely removed by crystallization, resulting in product purity <97. %, not widely used

Method used

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  • Method for high-efficiency preparation of high-purity sodium metavanadate

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preparation example Construction

[0022] A preparation method of sodium metavanadate, the method may further comprise the steps:

[0023] A, add sulfuric acid and ammonium sulfate in vanadium extraction leaching solution;

[0024] b, adjust the pH of the solution to 4 to 6, and filter to obtain a solid sodium ammonium vanadate;

[0025] c. adding the sodium ammonium vanadate solid into the sodium hydroxide solution, deamination, and adjusting the pH value of the solution to 8-8.5 to obtain a sodium metavanadate solution;

[0026] d. Spray flash evaporation the sodium metavanadate solution to obtain sodium metavanadate solid.

[0027] The present invention adopts vanadium-extracting leaching liquid to be vanadium-titanium magnetite leaching vanadium solution, and its vanadium concentration is 20~50g / L, and silicon concentration is 1.0~6.0g / L, and chromium concentration is 2.0~8.0g / L; The clarity of sodium vanadate solution is not conducive to the dispersion of sodium metavanadate solution; hexavalent Cr is a ...

Embodiment 1

[0044] Take 3L of vanadium extraction solution, [V]35.2g / L, [Si]1.8g / L, [Cr]2.5g / L, add dilute sulfuric acid with a volume ratio of 1+4, adjust the pH value to 6.43, add 100g of ammonium sulfate, replenish Add 1+4 dilute sulfuric acid to pH 5.41, and filter to obtain orange ammonium ammonium vanadate sodium. Prepare 1L sodium hydroxide solution, the concentration of sodium hydroxide is 65g / L, add 250g sodium ammonium vanadate, heat to boiling, stir, degas, add acid stabilizer to adjust the pH value to 8.41, and obtain 1.1L sodium metavanadate solution. The solution was sprayed and flash evaporated using a NAI-GZJ small spray dryer, the drying temperature was 105°C, and the feed rate was 50mL / min to obtain 252.1g of light yellow sodium metavanadate powder with a purity greater than 99.6%, a yield of 99.4%, and a Cr content of 0.007 %, Si content 0.011%, Fe content 0.004%, As, P content < 0.001%; ​​sodium metavanadate crystal particle size is uniform, particle size in -60 ~ +12...

Embodiment 2

[0046]Take 3L of vanadium extraction leaching solution, [V] 23.2g / L, [Si] 1.1g / L, [Cr] 2.1g / L, add dilute sulfuric acid with a volume ratio of 1+4, adjust the pH value to 6.73, add 100g of ammonium sulfate, replenish Add 1+4 dilute sulfuric acid to pH 5.01, filter to obtain orange ammonium ammonium vanadate sodium. Prepare 1L sodium hydroxide solution, the concentration of sodium hydroxide is 75g / L, add 250g sodium ammonium vanadate, heat to boiling, stir, degas, add acid stabilizer to adjust the pH value to 8.32, and obtain 1.2L sodium metavanadate solution. The solution was sprayed and flashed by NAI-GZJ small spray dryer, the drying temperature was 105°C, the feed rate was 50mL / min, and 165.8g of light yellow sodium metavanadate powder with a purity greater than 99.5% was obtained, the yield was 99.1%, and its Cr content was 0.006% , Si content 0.014%, Fe content 0.005%, As, P content <0.001%; ​​sodium metavanadate crystal particle size is uniform, particle size in -60 ~ +...

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Abstract

The invention belongs to the field of metallurgy and particularly relates to a preparation method of sodium metavanadate. The invention aims at providing a method for high-efficiency preparation of high-purity sodium metavanadate. The method comprises the following steps: (a) adding sulfuric acid and ammonium sulfate into a vanadium-extracting leaching solution; (b) adjusting pH value of the solution to 4-6, and filtering to obtain sodium ammonium vanadate solid; (c) adding the sodium ammonium vanadate solid into a sodium hydroxide solution, deaminizing, and adjusting pH value of the solution to 8-8.5 to obtain sodium metavanadate solution; and (d) carrying out spraying and flash evaporation on the sodium metavanadate solution to obtain sodium metavanadate solid. The preparation method provided by the invention has the advantages that the high-purity sodium metavanadate can be prepared, the crystallization efficiency and the yield of sodium metavanadate are obviously improved, the purity of sodium metavanadate is more than 99.5%, the direct yield of crystallization is more than 99%, the crystallization efficiency is improved by 35% compared with evaporation concentration crystallization, and the product quality is stable.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for efficiently preparing high-purity sodium metavanadate. Background technique [0002] The fine chemical products of vanadium mainly include sodium / potassium / ammonium metavanadate, sulfuric acid / vanadyl oxalate, which are mainly used in the manufacture of catalysts (such as sulfuric acid industry, power plant flue gas denitrification, etc.). Vanadium has special catalytic activity, and other elements are difficult to replace. About 4% to 5% of vanadium products in the world are used in this. [0003] The traditional preparation method of sodium metavanadate is to dissolve powdery vanadium pentoxide with sodium hydroxide solution under heating conditions, obtain sodium vanadate solution after full reaction, and then prepare sodium metavanadate by evaporation and crystallization. This method is simple to operate and does not produce polluting waste gas (ammo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/00C01P2006/80
Inventor 吴刘柱彭一村李千文侯海军周芳王英
Owner PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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