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Method for extracting sodium metavanadate from vanadium extraction leaching solution

A sodium metavanadate, sodium vanadium leaching technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve problems such as difficult washing, high production cost, and complex leachate components

Active Publication Date: 2010-06-23
PANGANG GRP PANZHIHUA STEEL & VANADIUM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Evaporation concentration and crystallization method is to evaporate and concentrate the vanadium extraction leachate obtained by leaching to obtain solid sodium metavanadate after removing impurities. This method is simple in process and easy to operate, but the composition of the leachate is complex and the removal of impurities is not complete, resulting in low product purity. High, difficult to be widely used
The ammonium polyvanadate solid alkali dissolution method is to add ammonium salt precipitation to the vanadium-containing leaching solution to obtain ammonium polyvanadate. The precipitation temperature is required to be around 90-95°C, and then add sodium hydroxide solid to dissolve to obtain sodium metavanadate solid. The shortcoming of a kind of method is that the pH value is adjusted to 2-2.5 in the precipitation ammonium polyvanadate process, consumes a large amount of acid, needs to add the sodium hydroxide of equal molar quantity with vanadium then in the process of adding sodium hydroxide back to dissolve, and alkali consumption Large, so the production cost is higher, the reaction principle is (NH 4 ) 2 V 6 o 16 +6NaOH=6NaVO 3 +2NH 3 ↑+4H 2 O: Ammonium polyvanadate usually presents a flocculent or polycrystalline polymer, and contains impurities such as sodium sulfate that are not easy to wash, resulting in low product purity
The third method is to dissolve V with sodium hydroxide solution 2 o 5 Method, heating and fully reacting to obtain sodium metavanadate, this method is easy to operate, the product has high purity, and solves the generation of polluted waste gas ammonia. This method is the most widely used method at present, but this method has great impact on V 2 o 5 Higher purity requirements, V 2 o 5 The price is more expensive, so the production cost is high, and the reaction principle is V 2 o 5 +2NaOH=2NaVO 3 +H 2 o

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preparation example Construction

[0014] In the method for preparing sodium metavanadate according to the present invention, the inorganic acid can be at least one of sulfuric acid, hydrochloric acid, nitric acid; the soluble ammonium salt can be at least one of ammonium sulfate, ammonium chloride, ammonium nitrate A sort of.

[0015] According to the method for preparing sodium metavanadate of the present invention, in step (1), the temperature of the precipitated ammonium-containing polyvanadate sodium is 75°C-85°C, and when the precipitation temperature is greater than 85°C, part of the ammonium-containing polyvanadium in the precipitate Sodium acid is converted to ammonium polyvanadate, resulting in Na in the precipitated product + The content decreases and the sulfur content of wrapped impurities in the product increases. When the precipitation temperature is lower than 75°C, the precipitation time is prolonged.

[0016] According to the method for preparing sodium metavanadate of the present invention, ...

Embodiment 1

[0023] Take 500mL of sodium roasting leaching solution (concentration of vanadium is 29.23g / L), adjust the pH value of the solution to 4.2 with concentrated sulfuric acid, heat the solution to 75°C, and 4 + : Add (NH 4 ) 2 SO 4 Solid, fully stirred, reacted for 50 minutes, filtered the obtained solid, and washed quickly to obtain ammonium-containing sodium polyvanadate crystals. The obtained ammonium-containing sodium polyvanadate is placed in a sealed reactor, and 100 mL of sodium hydroxide solution is put into it according to the molar ratio of Na:V=0.8, and stirred at 90 ° C until white solids start to precipitate in the solution, and then the solution is Cool to room temperature under stirring condition, filter and dry to obtain 33.3 g of sodium metavanadate solid, the product purity is 99.6%, and the recovery rate is 95%.

Embodiment 2

[0025] Take 500mL of sodium roasting leaching solution (concentration of vanadium is 21.5g / L), adjust the pH value of the solution to 4.5 with concentrated hydrochloric acid, heat the solution to 80°C, and 4 + : Add NH to the solution at a mass ratio of V=1.8 4 Cl solid, fully stirred, reacted for 30 minutes, filtered the resulting solid, and washed it quickly to obtain ammonium-containing sodium polyvanadate crystals. The obtained ammonium-containing sodium polyvanadate was placed in a sealed reactor, and 50 mL of sodium hydroxide solution was dropped in according to the molar ratio of Na:V=0.8, and stirred at 92 ° C until white solids began to precipitate in the solution, and then the solution was Cool to room temperature under stirring condition, filter and dry to obtain 23.3 g of sodium metavanadate solid, the product purity is 99.5%, and the yield is 90%.

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Abstract

The invention discloses a method for extracting sodium metavanadate from a vanadium extraction leaching solution, comprising the following steps of: adjusting the pH value of the sodium-ionized vanadium extraction leaching solution to 4-4.5 by using inorganic acid, then heating the solution to the temperature of 75-85 DEG C, then adding a soluble ammonium salt into the solution according to the mass ratio of NH4+:V=1.5-2, fully and uniformly stirring, and obtaining sodium polyvanadate containing ammonium after the reaction is finished; putting the obtained sodium polyvanadate containing ammonium into a sealed reactor, adding sodium hydroxide according to the mol ratio of Na:V=0.8-0.9, stirring at the temperature ranging from 90 DEG C to the boiling temperature till the solution starts to precipitate a white or light yellow solid, cooling the solution to the room temperature under the condition of stirring, filtering and drying to obtain a sodium metavanadate solid.

Description

technical field [0001] The invention relates to a method for preparing sodium metavanadate from vanadium extraction leaching solution. Background technique [0002] Sodium metavanadate is widely used in the chemical industry. It can be used as chemical reagent, catalyst, drier, mordant, manufacture ammonium vanadate and potassium metavanadate, and can also be used in medical photography, plant inoculation and corrosion inhibitor, etc. . [0003] At present, the preparation of sodium metavanadate at home and abroad is mainly extracted from the vanadium-containing sodium roasting leaching solution. There are three main methods: one method is to use the vanadium extraction leaching solution to evaporate, concentrate and crystallize; the second is to use the vanadium extraction leaching solution to precipitate more Ammonium vanadate, and then dissolve with sodium hydroxide solution; the third is to dissolve V with sodium hydroxide solution 2 o 5 Law. [0004] Evaporation con...

Claims

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Application Information

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IPC IPC(8): C01G31/00
Inventor 陈亮熊仁利李千文李大标
Owner PANGANG GRP PANZHIHUA STEEL & VANADIUM
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