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A method for recycling waste vanadium catalysts with phosphoric acid solution

A waste vanadium catalyst and phosphoric acid technology, applied in chemical recovery, silicate, alkali metal silicate, etc., can solve the problems of increased energy consumption, high cost, inconvenient control, etc., and achieve the effect of reducing energy consumption and avoiding extraction

Active Publication Date: 2022-01-14
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, SO 2 Gas, inconvenient to control, increases the cost of absorption device and recovery, and requires high-temperature calcination in the process of obtaining vanadium pentoxide, which also increases energy consumption

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 pulverizing 500 g of spent catalyst and sieving through 200 mesh, add 3000 g of 10 wt% phosphoric acid solution, stir for 3 min, and filter 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, filter, and was...

Embodiment 3

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

[0043] (1) After pulverizing 500 g of spent catalyst and sieving through 20 mesh, add 3000 g of 20 wt% phosphoric acid solution, stir for 5 min, and filter 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 min to ful...

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PUM

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Abstract

The invention discloses a method for recycling spent vanadium catalysts with phosphoric acid solution, comprising: reacting spent vanadium catalysts with phosphoric acid solution, filtering and separating to obtain filtrate I and filter residue I; filtrate I is statically filtered to obtain filtrate III and primary precipitate I, the filtrate III is separated by static filtration to obtain the secondary precipitate II and the filtrate IV; the filter residue I is added to potassium oxalate solution, fully reacted, left to filter and washed with water for 2 to 3 times to obtain the filtrate II and the filter residue II; the filtrate II is returned to replace Potassium oxalate solution, when the vanadium content in the solution exceeds 40 g / L, stop leaching to obtain a mixed solution; separate the mixed solution to obtain potassium sulfate and filtrate V; the filtrate V is treated to obtain vanadium pentoxide; the initial precipitate After I is processed, potassium vanadyl phosphate is obtained. Filter residue II is processed to obtain potassium silicate. The invention has high recovery rate at normal temperature, simple process and low energy consumption.

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 (pentavalen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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