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Method for separating and purifying vanadium and molybdenum of waste vanadium-molybdenum SCR (selective catalytic reduction) catalyst

An SCR catalyst and molybdenum-based technology, which is applied in the field of molybdenum separation and purification, waste vanadium-molybdenum-based SCR catalyst vanadium, can solve the problems that are not suitable for industrial applications, will change the properties of the organic phase, and cannot obtain high purity, and achieve high reliability. Effect

Active Publication Date: 2015-08-12
BOTREE CYCLING SCI & TECH CO LTD
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Problems solved by technology

Among them, the chemical precipitation method is simple to operate, but it is expensive and cannot achieve advanced treatment, and cannot produce high-purity (>99%) vanadium and molybdenum products; the ion exchange method can deeply separate vanadium and molybdenum and produce high-purity vanadium and molybdenum products. But the scale is small, the investment is expensive, and it is not suitable for industrial application; separated from molybdenum
Similar to the chemical precipitation method, this method cannot realize the deep separation of vanadium and molybdenum, and cannot obtain high-purity (>99%) vanadium products; the simultaneous extraction-selective stripping method refers to the use of substances with stripping selectivity as stripping Extraction agent, selective stripping of vanadium or molybdenum from the organic phase rich in vanadium and molybdenum
This method will not only change the properties of the organic phase, but also change the extraction mechanism of the organic phase, thus affecting the cyclic extraction capacity of the blank organic phase.
On the other hand, this method cannot obtain high-purity (>99%) vanadium and molybdenum products; the solvent extraction separation method uses the different forms of vanadium and molybdenum in the solution to selectively extract vanadium or molybdenum to achieve the separation of the two , is the most mature separation and purification technology for vanadium and molybdenum in industry
[0015]According to the above findings, so far there is no industrial case for the separation, recovery and purification of vanadium and molybdenum from waste vanadium-molybdenum-based SCR catalysts in my country. A set of mature, complete and highly feasible vanadium and molybdenum separation recovery and purification process

Method used

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  • Method for separating and purifying vanadium and molybdenum of waste vanadium-molybdenum SCR (selective catalytic reduction) catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The spent vanadium-molybdenum-based SCR catalyst provided by a laboratory, V 2 o 5 The content is 1.5%, MoO 3 4.5%, TiO 2 94%.

[0047] (1) Take the above spent catalyst, press m add :m metal Add additive NaOH at a ratio of = 1, then mix evenly and place in a muffle furnace to roast for conversion and removal of impurities, the roasting temperature is 600°C, and the roasting time is 3 hours; pure water is used as the leaching agent to extract vanadium and molybdenum from the roasted solid phase product, The liquid-solid ratio is 0.02L / g, the leaching temperature is 20°C, and the leaching time is 0.5h. The single-stage leaching rate of vanadium is 82%, and that of molybdenum is 72%. After filtration, the residue is recovered;

[0048] (2) Use the extraction system composed of 5% primary amine extractant JMT and kerosene as the organic phase to conduct a one-stage extraction and separation of vanadium and molybdenum in the vanadium and molybdenum leach solution, O / A=...

Embodiment 2

[0055] The spent vanadium-molybdenum-based SCR catalyst provided by a laboratory, V 2 o 5 The content is 2.1%, MO 3 3.5%, TiO 2 94.4%

[0056] (1) Take the above spent catalyst, press m add :m metal =1.2, add the additive NaCl, then mix it evenly and put it in the muffle furnace to roast for conversion and removal of impurities, the roasting temperature is 500°C, and the roasting time is 4.5h; use 1mol / L NaOH as the leaching agent, and leaching from the solid phase product after roasting For vanadium and molybdenum, the liquid-solid ratio is 0.025L / g, the leaching temperature is 25°C, the leaching time is 4h, the single-stage leaching rate of vanadium is 83%, and that of molybdenum is 74%. After filtering, the residue is recovered;

[0057] (2) Use an extraction system composed of 10% neutral phosphine extractant TBP and kerosene as the organic phase to conduct a one-stage extraction and separation of vanadium and molybdenum in the vanadium-molybdenum leach solution, O / A=...

Embodiment 3

[0064] The spent vanadium-molybdenum-based SCR catalyst provided by a laboratory, V 2 o 5 Content 0.9%, MO 3 2.7%, TiO 2 It was 96.4%.

[0065] (1) Take the above spent catalyst, press m add :m metal =6 Add the additive KOH, then mix it evenly and put it in the muffle furnace for roasting to convert and remove impurities. The roasting temperature is 800°C and the roasting time is 4.5h; pure water is used as the leaching agent to extract vanadium and molybdenum from the solid phase product after roasting , the liquid-solid ratio is 0.05L / g, the leaching temperature is 25°C, the leaching time is 2.5h, the single-stage leaching rate of vanadium is 81%, and that of molybdenum is 70%. After filtering, the residue is recovered;

[0066] (2) Use an extraction system composed of 25% organic phosphine D2EHPA and kerosene as the organic phase to conduct a one-stage extraction and separation of vanadium and molybdenum in the vanadium-molybdenum leach solution, O / A=1:1, initial pH of...

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Abstract

The invention discloses a method for separating and purifying vanadium and molybdenum of a waste vanadium-molybdenum SCR (selective catalytic reduction) catalyst. The method comprises the following steps: firstly, carrying out pretreatment on a catalyst to obtain a titanium slag and a vanadium-molybdenum solution; extracting and separating the vanadium-molybdenum solution, acidifying the obtained molybdenum-rich raffinate, and reprocessing to prepare a molybdenic acid product; carrying out reverse extraction on the obtained molybdenum-rich organic phase, then carrying out a two-stage extraction and vanadium purification process, and carrying out reverse extraction again to obtain a vanadium-rich solution; and reprocessing the vanadium-rich solution to prepare vanadium pentoxide. According to the method disclosed by the invention, the problem of difficult vanadium and molybdenum separation, recovery and purification of the waste vanadium-molybdenum SCR catalyst in industry is thoroughly solved; in addition, the recovery rates of vanadium and molybdenum exceed 95%; a high-purity (greater than 99%) molybdenic acid product and a vanadium pentoxide product of which the purity exceeds 99.5% can be respectively obtained; recycling of resources is really realized; and the method has good environmental and economic benefits, and is suitable for industrial popularization and application.

Description

technical field [0001] The invention belongs to the field of solid waste treatment, in particular to a method for separating and purifying vanadium and molybdenum of a waste vanadium-molybdenum-based SCR catalyst. Background technique [0002] As we all know, selective catalytic reduction technology (SCR) is a denitrification technology with high reliability and simple process. SCR catalyst is the core part of this technology, and its investment ratio directly determines the operating cost of the denitrification process. SCR catalysts are divided into vanadium-molybdenum series and vanadium-tungsten series, both of which are based on V 2 o 5 As the active component, TiO 2 As a carrier, the difference is that the additive of vanadium-molybdenum-based SCR catalyst is MoO 3 , while the vanadium-tungsten catalyst is WO 3 . When the SCR catalyst cannot be regenerated, it becomes a spent SCR catalyst. The "Technical Specifications for Flue Gas Denitrification Engineering of...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B34/34C22B34/22
CPCY02P10/20
Inventor 林晓刘晨明潘尹银李志强
Owner BOTREE CYCLING SCI & TECH CO LTD
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