Method for preparing high-density ammonium polyvanadate by calcified roasting pickle liquor through heat preservation
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A calcification roasting, ammonium polyvanadate technology, applied in chemical instruments and methods, inorganic chemistry, vanadium compounds, etc., can solve the problems of large loss of vanadium, high production cost, low density of ammonium vanadate, etc. The effect of reducing vanadium loss
Active Publication Date: 2020-06-02
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD +1
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Problems solved by technology
[0007] The technical problems to be solved in the present invention are: low density of ammonium polyvanadate product of vanadium slag calcification roasting acid leaching solution, low density of ammonium polyvanadate, large loss of vanadium, high production cost, etc.
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Embodiment 1
[0038] Embodiment 1 adopts the inventive method to prepare high-density ammonium polyvanadate
[0039] Take 500mL of calcified roasting pickling solution, where TV=31.06g / L, NH 4 + =7.20g / L, pH=2.89, add 11.65g of ammonium sulfate, NH in the solution 4 + The / V concentration ratio is 0.44. After stirring and dissolving, add sulfuric acid to adjust the pH=1.8, put it into a water bath and heat up to 87°C, keep it warm for 90min, then heat up to boiling precipitation for 45min, filter, wash and dry to obtain ammonium polyvanadate; The vanadium precipitation rate is 99.72% according to the concentration calculation, and the bulk density measured by ammonium polyvanadate is 0.71g / com 3 .
Embodiment 2
[0040] Embodiment 2 adopts the inventive method to prepare high-density ammonium polyvanadate
[0041] Take 500mL of calcified roasting pickling solution, where TV=28.77g / L, NH 4 + =3.28g / L, pH=2.96, add 11.25g of ammonium sulfate, NH in the solution 4 + The / V concentration ratio is 0.33. After stirring and dissolving, add sulfuric acid to adjust the pH=1.9, put it into a water bath and heat up to 83°C, keep it warm for 60min, then heat up to boiling and precipitate for 60min, filter, wash and dry to obtain ammonium polyvanadate; The vanadium precipitation rate is 99.28% according to the concentration calculation, and the bulk density measured by ammonium polyvanadate is 0.51g / com 3 .
Embodiment 3
[0042] Embodiment 3 adopts the inventive method to prepare high-density ammonium polyvanadate
[0043] Add about 20m of calcified roasting acid leaching solution into the precipitation tank 3 , where TV=24.72g / L, NH 4 + =5.34g / L, pH=3.07, add 155kg of ammonium sulfate, NH in the solution 4 + The / V concentration ratio is 0.22, after stirring and dissolving, add sulfuric acid to adjust the pH=2.0, pass high-temperature steam to raise the temperature to 91°C, keep warm for 75 minutes, then continue to pass high-temperature steam to heat up to boiling precipitation for 60 minutes, filter, wash and dry to obtain ammonium polyvanadate; Calculated according to the concentration of vanadium in the upper layer, the vanadium deposition rate is 99.06%, and the bulk density measured by ammonium polyvanadate is 0.58g / com 3 .
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Abstract
The invention belongs to the technical field of hydrometallurgy of vanadium, and particularly relates to a method for preparing high-density ammonium polyvanadate by calcified roasting pickle liquor through heat preservation. The method aims at the problems of low density and the like of ammonium polyvanadate which is a vanadium precipitation product of the calcified roasting pickle liquor of vanadium slags. The method for preparing the high-density ammonium polyvanadate comprises the following steps that a. the calcified roasting pickle liquor of the vanadium slags is taken, the pH value is regulated to 2.2 - 3.8, and the temperature is regulated to be 20 DEG C - 75 DEG C, the concentration of NH4<+> is controlled to be 0.22 - 0.44 time of the concentration of vanadium in the pickle liquor; b, the pH value of the liquor is adjusted to 1.7 - 2.1, the temperature is regulated to be 83 DEG C-91 DEG C, and heat preservation is carried out for 60 min - 90 min under the stirring condition;c, after heat preservation is finished, the temperature is raised till the liquor is boiled, and reaction is carried out; and d, solid-liquid separation, washing and drying are carried out to obtain the high-density ammonium polyvanadate. According to the method for preparing the high-density ammonium polyvanadate by the calcified roasting pickle liquor through heat preservation, the ammonium polyvanadate with the density being 0.5 g/cm<3> or above is prepared from the calcified roasting pickle liquor of the vanadium slags, the density is increased by two times compared with an existing method, and meanwhile, vanadium in the pickle liquor is fully recycled, so that economic benefits are remarkable.
Description
technical field [0001] The invention belongs to the technical field of vanadium hydrometallurgy, and in particular relates to a method for preparing high-density ammonium polyvanadate with heat preservation of calcified roasting acid leaching solution. Background technique [0002] Precipitation of vanadium in acid leaching solution refers to the process of preparing ammonium polyvanadate by using vanadium slag as raw material, using acid immersion solution obtained by calcification roasting-acid leaching, and using acidic ammonium salt vanadium precipitation technology. At present, the quality of ammonium polyvanadate and subsequent vanadium oxide products prepared by this process can meet the requirements of the industry, but the obtained ammonium polyvanadate product has a fine particle size and low density, resulting in fine particles and flocs in the precipitated slurry. Settling is slow, the filter cloth penetrates severely during liquid-solid separation, and at the sa...
Claims
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Application Information
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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/22C22B3/44C01G31/00
CPCC01G31/00C01P2006/11C22B3/44C22B34/22Y02P10/20
Inventor 叶露何文艺彭毅陈燕
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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