Method for recycling spent vanadium catalyst through phosphoric acid solution

A waste vanadium catalyst and phosphoric acid technology, which is applied in the direction of chemical recovery, silicate, alkali metal silicate, etc., can solve the problems of increased energy consumption, high cost, increased absorption device and recovery cost, etc., to achieve reduced energy consumption, Avoid the effects of extraction

Active Publication Date: 2020-06-19
贵州威顿催化技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this scheme is that it realizes the efficient recovery of potassium and vanadium and the purity is high. The disadvantage is that the process is long, with many steps and high cost. At the same time, S

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A method for recycling spent vanadium catalysts with phosphoric acid solution, comprising the following steps:

[0021] (1) After 500 g of spent catalyst was pulverized and sieved with 50 mesh, 1500 g of 30 wt% phosphoric acid solution was added, stirred for 5 min, and filtered to obtain dark green filtrate I and filter residue I.

[0022] (2) After the filtrate I was allowed to stand for 3 hours, the dark green primary precipitate I solid (with a vanadium pentoxide content of 49.42%) and the filtrate III were obtained by filtration and separation. The filtrate III was allowed to stand for 12 h, and the secondary precipitate II was obtained by filtration ( Yellow solid, potassium vanadyl phosphate) and filtrate IV, the filtrate IV is mixed with 10 wt% phosphoric acid in a ratio of 10:1 and returned to step (1) and can continue to be used for spent catalyst soaking.

[0023] (3) Pour the filter residue I into 1000 g of 10 wt% potassium oxalate solution, stir for 20 min t...

Embodiment 2

[0031] A method for recycling spent vanadium catalysts with phosphoric acid solution, comprising the following steps:

[0032] (1) After 500 g of spent catalyst was pulverized and sieved with 200 mesh, 3000 g of 10 wt% phosphoric acid solution was added, stirred for 3 min, and filtered to obtain dark green filtrate I and filter residue I.

[0033](2) After the filtrate I was allowed to stand for 3 hours, the green primary precipitate solid (the content of vanadium pentoxide was 48.7 wt%) and the filtrate III were separated by filtration. The filtrate III was allowed to stand for 24 h, and the secondary precipitate II (yellow solid, potassium vanadyl phosphate) and filtrate IV, the filtrate IV is mixed with 10 wt% phosphoric acid in a ratio of 10:1 and returned to step (1) and can continue to be used for spent catalyst soaking.

[0034] (3) Pour the filter residue I into 2000 g of 10 wt% potassium oxalate solution, stir for 30 min to fully react, let it stand for 2 hours, filte...

Embodiment 3

[0042] A method for recycling spent vanadium catalysts with phosphoric acid solution, comprising the following steps:

[0043] (1) After 500 g of spent catalyst was pulverized and sieved with 20 mesh, 3000 g of 20 wt% phosphoric acid solution was added, stirred for 5 min, and filtered to obtain dark green filtrate I and filter residue I.

[0044] (2) After the filtrate I was allowed to stand for 3 hours, the green primary precipitate I was separated by filtration (the content of vanadium pentoxide was 49.35 wt%) and the filtrate III was obtained by filtration. The filtrate III was allowed to stand for 48 h, and the secondary precipitate II was obtained by filtration ( Yellow solid, potassium vanadyl phosphate) and filtrate IV, the filtrate IV is mixed with 10 wt% phosphoric acid in a ratio of 10:1 and returned to step (1) and can continue to be used for spent catalyst soaking.

[0045] (3) Pour the filter residue I into 2000 g of 10 wt% potassium oxalate solution, stir for 20 ...

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Abstract

The invention discloses a method for recycling a spent vanadium catalyst through a phosphoric acid solution. The method comprises the steps: after the spent vanadium catalyst reacts with the phosphoric acid solution, filtering and separation are conducted to obtain filtrate I and filter residue I; the filtrate I is subjected to still standing and filtered to obtain filtrate III and primary precipitate I, and the filtrate III is subjected to still standing, filtered and separated to obtain secondary precipitate II and filtrate IV; a potassium oxalate solution is added into the filter residue Ifor sufficient reacting, still standing and filtering are conducted, a solid is washed with water for 2-3 times, and filtrate II and filter residue II are obtained; the filtrate II is returned to replace the potassium oxalate solution, and when the content of vanadium in a solution exceeds 40 g/L, leaching is stopped to obtain a mixed solution; after the mixed solution is treated, potassium sulfate and filtrate V are obtained; after the filtrate V is treated, vanadium pentoxide is obtained; after the primary precipitate I is treated, potassium vanadium phosphate is obtained; and the filter residue II is treated to obtain potassium silicate. According to the method, at the normal temperature, the recovery rate is high, the process is simple, and energy consumption is low.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for recycling spent vanadium catalysts with phosphoric acid solution. Background technique [0002] With the rapid development of the sulfuric acid industry, the production capacity of sulfuric acid in my country is about 100 million tons. Catalysts are used in the production of sulfuric acid. This catalyst is a vanadium catalytic system composed of diatomaceous earth as the carrier, vanadium pentoxide as the active component, and alkali metal (Na, K, Cs) sulfate as the co-catalyst. The composition is as follows: the diatomite content is 50-70%, the alkali metal sulfate content is 15-28%, and the active component vanadium pentoxide content is 5-10%. The vanadium catalyst promotes the conversion of sulfur dioxide to sulfur trioxide, which provides a strong guarantee for the mass production of sulfuric acid. However, the active component (pentaval...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B34/22C22B26/10C01B33/32
CPCC22B7/007C22B34/225C22B26/10C01B33/32Y02P10/20Y02P20/584
Inventor 田坤杨胜飞
Owner 贵州威顿催化技术有限公司
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