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Preparation method of high-density ammonium polyvanadate

An ammonium polyvanadate, high-density technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of long time, low vanadium precipitation rate and high reaction temperature, and achieve the effect of saving energy consumption and cost

Active Publication Date: 2015-09-02
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the problems of low vanadium deposition rate, high reaction temperature and long time in the prior art, and provide a new method for preparing high-density ammonium polyvanadate

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preparation example Construction

[0021] According to the preparation method of the present invention, after the reaction ends, a layered system comprising the supernatant liquid and ammonium polyvanadate precipitate can be obtained, and the difference between the total vanadium concentration in the all-vanadium leaching solution and the vanadium concentration in the supernatant liquid is usually calculated. The percentage of the total vanadium concentration obtains the vanadium deposition rate. According to the preparation method of the present invention, the vanadium deposition rate after the reaction is above 99%.

[0022] In addition, in order to obtain dry ammonium polyvanadate, preferably, the method further includes: after the reaction is completed, the obtained precipitate is filtered and dried. The drying process may include: drying the precipitate in an oven at a temperature of 40-90° C. for 5-10 hours.

Embodiment 1

[0028] This embodiment is used to illustrate the preparation method of the high-density ammonium polyvanadate of the present invention.

[0029] Add 1000mL of the vanadium-containing solution in Table 1 to a 2000mL clean beaker, according to the NH 4 + The molar ratio of vanadium in the vanadium-containing solution is 0.5:1. Add ammonium sulfate and 0.3386g triethanolamine. After the ammonium sulfate is dissolved in the vanadium-containing solution, adjust the pH value to 5.0 with sulfuric acid, stir, and react at 10°C for 10 minutes Afterwards, filter to obtain wet ammonium polyvanadate precipitation, place the wet ammonium polyvanadate in a 50°C oven for drying, and the drying time is 12 hours, thereby making ammonium polyvanadate, and its density is 0.85g / cm 3, the detected vanadium content in the vanadium precipitation supernatant liquid is 0.34g / L, and the vanadium precipitation rate is 99.4%.

Embodiment 2

[0031] This embodiment is used to illustrate the preparation method of the high-density ammonium polyvanadate of the present invention.

[0032] Add 1000mL of the vanadium-containing solution in Table 1 to a 2000mL clean beaker, according to the NH 4 + The molar ratio of vanadium in the vanadium-containing solution is 2:1. Add ammonium sulfate and 1.7g triethanolamine. After the ammonium sulfate is dissolved in the vanadium-containing solution, adjust the pH value to 2.0 with sulfuric acid, stir, and react at 20°C for 10 minutes Afterwards, carry out filtration to obtain wet ammonium polyvanadate precipitation, place wet ammonium polyvanadate in 50 ℃ oven and dry, drying time is 12 hours, thereby makes ammonium polyvanadate, detects that its density is 1.2g / cm 3 , the detected vanadium content in the vanadium precipitation supernatant was 0.34g / L, and the vanadium precipitation rate was 99.2%.

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Abstract

The invention discloses a preparation method of high-density ammonium polyvanadate. The method comprises the following steps of mixing hydramine, soluble ammonia salt and vanadium-contained solution shown in formula (1), adjusting a pH value of the obtained mixture to be acidity, reacting under the pH value, and then carrying out solid-liquid separation on the reaction mixture obtained through reacting. According to the preparation method of the high-density ammonium polyvanadate provided by the invention, the preparation time is shortened to be 5 minutes from 60 minutes, the density reaches to 0.8g / cm<3>, and the molybdenum precipitation ratio can reach to more than 99 percent. The preparation method is simple and easy to use, low in equipment requirement, convenient to operate, wide in applicable range, and low in cost, and has good social benefit and economic benefit. According to the formula (1), R1, R2 and R3 are C1-C4 alkylene.

Description

technical field [0001] The invention relates to a preparation method of high-density ammonium polyvanadate. Background technique [0002] Ammonium polyvanadate is a light yellow crystalline powder, slightly soluble in cold water, hot ethanol and ether, soluble in hot water and dilute ammonium hydroxide; it turns into vanadium pentoxide when burned in air, which is poisonous. One of the main uses of ammonium polyvanadate is to prepare vanadium oxide products suitable for smelting ferrovanadium, and usually only have a density of 0.6g / cm 3 The above ammonium polyvanadate can meet the requirements. At present, the more common method for preparing ammonium polyvanadate is the acidic ammonium sulfate precipitation method. The specific process is to use ammonium salt as a precipitant under acidic conditions to precipitate ammonium polyvanadate from a vanadium-containing solution under conditions close to boiling. . The acidic ammonium sulfate precipitation method is because of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
Inventor 殷兆迁李千文高官金付自碧郭继科王俊
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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