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Method for recovering acid liquor and separating vanadium in process of reducing acid leaching vanadium-containing waste catalyst

A technology for waste catalysts and catalysts, applied in the direction of improving process efficiency, can solve the problems of low leaching rate, only reaching 85%, low product purity, etc., and achieve the effects of mild leaching conditions, low leaching temperature, and high vanadium leaching rate.

Active Publication Date: 2020-08-04
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid system involved in the reductive acid leaching process is generally an inorganic sulfuric acid system. Because sulfuric acid itself does not have reducing properties, it is necessary to add reducing agents such as sodium sulfite, sulfur dioxide, etc., as reported in CN103290223A, but the method has low leaching rate and additional reduction The shortcoming that other impurity ions such as sodium, sulfur etc. are not easy to remove is introduced by agent; Do not add reductant in direct acid leaching process, directly use acid solution leaching, as reported in CN103966447A, pre-leaching with dilute sulfuric acid, after leaching again with concentrated sulfuric acid However, the vanadium leaching rate only reaches 85% in the two leaching processes; the alkali leaching process adds sodium hydroxide leaching under normal pressure or high pressure to form sodium vanadate leaching solution, but the product purity obtained by the method is lower , as reported by CN103484678A, CN1305537A, CN1927726A, CN101631598A, CN102936039A, etc.
[0005] The vanadium-containing leaching solution in the patent CN106244828A is obtained by adding potassium sulfate to crystallize to obtain potassium alum to remove aluminum. After the crystallization, the solution is reduced by adding reduced iron powder or sodium sulfite and other substances to reduce the iron in the solution. Add oxalic acid to realize the removal of iron impurities in the form of oxalate. After removing impurities, the removal rate of aluminum reaches 70-85%, and the removal rate of iron is 80-95%, but the waste acid solution produced in the preparation process is serious to environmental pollution; The process of preparing vanadyl sulfate from an acidic vanadium-containing solution, but it produces more waste during the preparation process and causes serious environmental pollution
[0006] Therefore, this area needs to develop a kind of method of novel reclaiming vanadium, makes recovery process simple, low energy consumption, can industrialized production, and can solve the serious pollution that exists in the prior art, leaching rate is lower, product purity is lower and impurity ion Difficult to control, unusable waste acid, etc.

Method used

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  • Method for recovering acid liquor and separating vanadium in process of reducing acid leaching vanadium-containing waste catalyst
  • Method for recovering acid liquor and separating vanadium in process of reducing acid leaching vanadium-containing waste catalyst

Examples

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Embodiment 1

[0064] A method for recovering acid solution and separating vanadium in the process of reductive acid leaching waste catalyst containing vanadium comprises the following steps:

[0065] (1) Add the vanadium-tungsten-titanium-aluminum system catalyst to oxalic acid for leaching at 70°C for 6 hours to obtain an organic acid immersion solution with a vanadium element content of 4.5g / L, and evaporate water under reduced pressure at 80°C in the organic acid immersion solution , the evaporation volume is 80% of the volume of the organic acid immersion solution, then crystallize oxalic acid at 0°C for 8 hours, and filter the oxalic acid crystals to obtain the enrichment solution;

[0066] (2) According to the volume ratio of the enriched solution and hydrogen peroxide as 10:1, mix the enriched solution with hydrogen peroxide, oxidize at 70°C, add ammonia water to the oxidized enriched solution to adjust the first pH value to 3, Add 1g of ethylenediaminetetraacetic acid, carry out the...

Embodiment 2

[0068] The difference from Example 1 is that step (2) adjusts the first pH value to 2.

Embodiment 3

[0070] The difference from Example 1 is that step (2) adjusts the first pH value to 4.

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Abstract

The invention relates to a method for recovering acid liquor and separating vanadium in a process of reducing an acid leaching vanadium-containing waste catalyst. The method comprises the following steps: (1) carrying out acid leaching on the vanadium-containing waste catalyst by using an organic acid to obtain an organic acid leaching solution, and separating the organic acid to obtain an enrichment solution; and (2) oxidizing the enrichment solution, removing iron elements in the oxidized enrichment solution to obtain a purification solution, and then carrying out a vanadium element precipitation process on the purification solution to obtain a recovery product, wherein the recovery product is a vanadium compound. According to the method, the organic acid is recovered at first, the recovery rate reaches 80-90%, then the enrichment solution is oxidized, Fe2+ and V4+ in the enrichment solution are oxidized into Fe3+ and V5+ in the oxidation process, then the iron element is removed, the loss of the vanadium element in the iron element removal process is avoided, and the recovery rate of the vanadium compound is improved.

Description

technical field [0001] The invention belongs to the field of non-ferrous metallurgy and resource recycling, in particular to a method for recovering acid solution and separating vanadium in the process of reducing acid leaching waste catalyst containing vanadium, and in particular to a method for recovering acid solution in the process of reducing acid leaching waste catalyst containing vanadium And a method for separating vanadium and tungsten. Background technique [0002] Vanadium is an important beneficial metal element, known as "monosodium glutamate of modern industry", is an important strategic resource of the country, widely used in iron and steel, non-ferrous metals and chemical and chemical industries, such as vanadium-containing steel in the iron and steel industry, which has strength High toughness, good wear resistance and other advantages, so it is widely used in machinery, automobiles, shipbuilding and railway industries; it is widely used as a catalyst in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B34/22
CPCC22B7/007C22B7/009C22B34/225Y02P10/20
Inventor 李会泉武文粉王晨晔王兴瑞陈艳赵晨
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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