CN111270076A - Method for leaching vanadium and tungsten elements in waste SCR denitration catalyst - Google Patents

Method for leaching vanadium and tungsten elements in waste SCR denitration catalyst Download PDF

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CN111270076A
CN111270076A CN202010193863.0A CN202010193863A CN111270076A CN 111270076 A CN111270076 A CN 111270076A CN 202010193863 A CN202010193863 A CN 202010193863A CN 111270076 A CN111270076 A CN 111270076A
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denitration catalyst
scr denitration
waste scr
vanadium
waste
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张亚平
滕玉婷
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Southeast University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C22B34/225—Obtaining vanadium from spent catalysts
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/36—Obtaining tungsten
    • C22B34/365—Obtaining tungsten from spent catalysts
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention discloses a leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst, which comprises the following steps: (1) immersing the pretreated waste SCR denitration catalyst into NH at a liquid-solid ratio of 20: 1-23·H2O、H2O2Magnetically stirring the mixed solution and reacting in a high-pressure reaction kettle for 4-8 hours; (2) and (3) centrifugally separating the mixture treated in the step (1), and transferring the leaching solution into a volumetric flask. The leaching method of vanadium and tungsten elements in the waste SCR denitration catalyst can leach the vanadium and tungsten elements to a large extent, lays foundation for subsequent resource recovery of the vanadium and tungsten elements, realizes green chemistry, and is low in cost and very simple and convenient to operate.

Description

Method for leaching vanadium and tungsten elements in waste SCR denitration catalyst
Technical Field
The invention belongs to the field of catalyst recovery, and particularly relates to a leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst.
Background
China is a country with large energy consumption mainly based on thermal power generation, and a large amount of NOx is discharged while coal is fired. With the progress of times, the electricity demand of China is increasing, and pollutants such as nitrogen oxides emitted by China are gradually increased. Nitrogen oxides can cause great harm to the environment, and reducing the content of the nitrogen oxides in the atmosphere is an important component for reducing environmental pollution. The SCR denitration technology has good selectivity, high denitration efficiency and strong stability, so the SCR denitration technology is widely applied to coal-fired power plants in particular. High-temperature catalysts are frequently used, among which TiO is used2Is a carrier, mainly comprisesIs divided into V2O5-WO3And the cost of the catalyst is always the most expensive part of the whole denitration process. Ideally, the denitration catalyst can Be used for a long time, but the fly ash can block the micropores of the catalyst, and compounds from toxic smoke, such As alkali metals (Na, K, and the like), alkaline earth metals (Be, Ca, and the like) and heavy metals (As, Pb), can cause the catalyst to Be gradually deactivated during operation, so that the service life of the catalyst is shortened.
The denitration catalyst absorbs fly ash generated by combustion of a coal-fired power plant in the using process, wherein the fly ash contains a certain amount of heavy metals (such as lead, mercury, cadmium, arsenic, chromium and the like), and the active component V of the denitration catalyst2O5And WO3Also toxic metal oxides, where V2O5The heavy metal is a highly toxic substance, so the main potential hazardous characteristic of the waste denitration catalyst is leaching toxicity, wherein the leaching concentration of the adsorbed heavy metal is generally higher than that of the new denitration catalyst, and the leaching concentration of the heavy metal in part of the waste denitration catalyst exceeds the leaching concentration limit value of GB5085.3-2007 'hazardous waste identification Standard leaching toxicity identification'. If the deactivated SCR denitration catalyst is disposed according to a landfill mode, not only can a great amount of landfill requirements be generated, but also the environmental pollution risk of toxic substances can not be effectively solved, and WO contained in the SCR denitration catalyst3、V2O5And TiO2The waste catalyst is precious resource, and the discarding of the waste catalyst can cause various valuable metal resources contained in the waste catalyst not to be recycled, thereby causing huge waste of effective resources.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide the method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst, which has high leaching rate and is suitable for industrial popularization.
The technical scheme is as follows: the invention relates to a leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst, which comprises the following steps:
(1) after the waste SCR denitration catalyst is washed for 20-30 min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1-2 h with ultrasonic wave with the power of 40-60 kHz in an auxiliary mode, drying the waste SCR denitration catalyst, performing ball milling for 30-40 min, and sieving the waste SCR denitration catalyst with a sieve of 150-200 meshes to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing the pretreated waste SCR denitration catalyst into NH with the concentration of 5-10 mol/L according to the liquid-solid ratio of 20: 1-23·H2O and H with the concentration of 1-5 mol/L2O2Magnetically stirring the mixed solution at the rotating speed of 1000-1200 rad/min, and reacting for 4-8 h at the temperature of 200-240 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1000-1200 rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Wherein, NH in the step (2)3·H2The concentration of O is preferably 7-8 mol/L, H2O2The concentration of (b) is preferably 1 to 2 mol/L. The waste SCR denitration catalyst is waste V generated in the denitration process of the selective catalytic reduction method2O5-WO3/TiO2A catalyst.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics: the leaching method of vanadium and tungsten elements in the waste SCR denitration catalyst can leach the vanadium and tungsten elements to a greater extent, lays foundation for subsequent resource recovery of the vanadium and tungsten elements, realizes green chemistry, and has the advantages of high leaching rate of the vanadium and tungsten elements, low cost, low energy consumption, low pollution and very simple and convenient operation.
Detailed Description
In the following examples, waste V2Os-WO3/TiO2The SCR denitration catalyst is obtained from an inactivated commercial V which runs for about 5 years by national institute of electrical environmental protection2O5-WO3/TiO2Catalyst, the content of main oxides in the spent catalyst as determined by XRF, table 1, NH3·H2O and H2O2All purchased from Nanjing Shengjiangquan glass instruments Ltd.
TABLE 1 spent SCR denitration catalyst main oxide composition
Figure BDA0002415582980000021
Example 1
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) after the waste SCR denitration catalyst is washed for 20min under high pressure, the waste SCR denitration catalyst is immersed in deionized water and is washed for 1h with the aid of ultrasonic waves with the power of 40kHz, the waste SCR denitration catalyst is dried and is subjected to ball milling for 30min, and the waste SCR denitration catalyst is sieved by a 150-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 5mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 1mol/L2O2The mixed solution is 1000mL, is magnetically stirred at the rotating speed of 1000rad/min and reacts for 4 hours at the temperature of 200 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1000rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Example 2
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) washing the waste SCR denitration catalyst for 30min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 2h with ultrasonic wave with the power of 60kHz, drying, performing ball milling for 40min, and sieving the waste SCR denitration catalyst with a 200-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 10mol/L according to the liquid-solid ratio of 10: 13·H2O, H with the concentration of 5mol/L2O21000mL of the mixed solution is magnetically stirred at the rotating speed of 1200rad/min and reacts for 8 hours at the temperature of 240 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1200rad/min, transferring the leaching solution into a volumetric flask, using deionized water for constant volume, and selecting ICP-OES for measuring the concentration of vanadium and tungsten elements.
Example 3
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) washing the waste SCR denitration catalyst for 25min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1.5h with ultrasonic wave with the power of 50kHz in an auxiliary manner, drying, performing ball milling for 35min, and sieving the waste SCR denitration catalyst with a 175-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) 4g of pretreated waste SCR denitration catalyst is immersed into NH with the concentration of 7.5mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 3mol/L2O21000mL of the mixed solution is magnetically stirred at the rotating speed of 1100rad/min and reacts for 6 hours in a high-pressure reaction kettle at the temperature of 230 ℃;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1100rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Example 4
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) washing the waste SCR denitration catalyst for 22min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1h with the aid of ultrasonic waves with the power of 42kHz, drying, performing ball milling for 31min, and sieving the waste SCR denitration catalyst with a 160-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 7mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 2mol/L2O21000mL of the mixed solution is magnetically stirred at the rotating speed of 1050rad/min and reacts in a high-pressure reaction kettle at the temperature of 200-240 ℃ for 5 hours;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1040rad/min, transferring the leaching solution into a volumetric flask, using deionized water for constant volume, and selecting ICP-OES for measuring the concentration of vanadium and tungsten elements.
Example 5
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) after washing the waste SCR denitration catalyst for 27min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 2h with ultrasonic wave with the power of 55kHz, drying, performing ball milling for 38min, and sieving the waste SCR denitration catalyst by a 190-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 8mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 4mol/L2O21000mL of the mixed solution is magnetically stirred at the rotating speed of 1150rad/min and reacts for 7 hours at the temperature of 230 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1150rad/min, transferring the leaching solution into a volumetric flask, using deionized water for constant volume, and selecting ICP-OES for measuring the concentration of vanadium and tungsten elements.
Example 6
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) after washing the waste SCR denitration catalyst for 30min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1h with the aid of ultrasonic waves with the power of 40kHz, drying, performing ball milling for 30min, and sieving the waste SCR denitration catalyst with a 150-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 7mol/L according to the liquid-solid ratio of 20: 13·H21000mL of O solution, magnetically stirring at 1000rad/min and reacting for 4h at 200 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1000rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Comparative example 1
Example 6 in step (2), NH was reacted in a 100mL autoclave3·H2The concentration of O is 0, 1, 2, 3, 4, 5, 6 and 7mol/L in sequence, the other conditions are the same as the example 6, and the leaching rates of vanadium and tungsten are shown in the following table 2:
TABLE 2 different NH3·H2The concentration of O is opposite to that of vanadium,Influence of tungsten Leaching Rate
Figure BDA0002415582980000051
As can be seen from Table 2, with NH3·H2The increase in the concentration of O solution, due to the relatively high temperature and pressure in the sealed autoclave, corresponds to NH3·H2The actual molar concentration of the O solution is gradually saturated, the diffusion of solid-liquid interface mass transfer is enhanced, the speed of the following reactions (a) and (b) is accelerated, and the leaching rate of vanadium and tungsten is improved.
WO3+2NH3·H2O＝＝(NH4)2WO4+H2O (a)
V2O5+2NH3·H2O＝＝2NH4VO3+H2O (b)
Example 7
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) after washing the waste SCR denitration catalyst for 30min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1h with the aid of ultrasonic waves with the power of 40kHz, drying, performing ball milling for 30min, and sieving the waste SCR denitration catalyst with a 150-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 7mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 2mol/L2O2The mixed solution is 1000mL, is magnetically stirred at the rotating speed of 1000rad/min and reacts for 4 hours at the temperature of 200 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1000rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Comparative example 2
Example 7 in step (2), 100mL of high pressure reactor was charged with H2O2The concentrations of (A) and (B) are 0, 0.5, 1, 1.5 and 2mol/L in this order, and the other conditions are the same as in example 7, vanadium,The tungsten leaching rate is shown in table 3 below:
TABLE 3 different H2O2Influence of concentration on leaching rate of vanadium and tungsten
Figure BDA0002415582980000061
As can be seen from Table 3, with H2O2The concentration of the solution is increased, the leaching rate of vanadium is increased from 25.1 percent to 39.7 percent, mainly because V in the waste SCR denitration catalyst4+Oxidation to V5+Can be more easily reacted with NH3·H2And (4) reacting.
Example 8
A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst comprises the following steps:
(1) after washing the waste SCR denitration catalyst for 30min under high pressure, immersing the waste SCR denitration catalyst in deionized water, washing the waste SCR denitration catalyst for 1h with the aid of ultrasonic waves with the power of 40kHz, drying, performing ball milling for 30min, and sieving the waste SCR denitration catalyst with a 150-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst;
(2) immersing 4g of pretreated waste SCR denitration catalyst into NH with the concentration of 7mol/L according to the liquid-solid ratio of 20: 13·H2O, H with the concentration of 2mol/L2O2The mixed solution is 1000mL, is magnetically stirred at the rotating speed of 1000rad/min and reacts for 4 hours at the temperature of 240 ℃ in a high-pressure reaction kettle;
(3) and (3) centrifugally separating the mixture treated in the step (2), wherein the centrifugal speed is 1000rad/min, transferring the leaching solution into a volumetric flask, performing constant volume with deionized water, and determining the concentration of vanadium and tungsten elements by using ICP-OES.
Comparative example 3
Example 8 in step (2), the waste SCR denitration catalyst was immersed in a solution/solid ratio of 20: 1 containing 7mol/L NH3·H2O and 2mol/L H2O2In a 1000mL magnetically stirred autoclave with the solution, the reaction temperature is 100, 130, 170, 210, 240 ℃, the other conditions are the same as in example 8, and the leaching rates of vanadium and tungsten are shown in the following Table 4:
TABLE 4 influence of reaction temperature on vanadium and tungsten leaching rates
Figure BDA0002415582980000071
As can be seen from Table 4, NH was promoted with increasing temperature3·H2O solution with WO3The leaching reaction between the two. However, the reaction temperature has little effect on the leaching rate of V. When the temperature is in the range of 100 ℃ to 240 ℃, the leaching rate of V does not change significantly, probably because the low-valence V in the solution is VOSO4Exist in the form of (1). H2O2Has an oxidizing effect, and can improve the leaching rate of vanadium element as an oxidizing agent.

Claims (8)

1. A leaching method of vanadium and tungsten elements in a waste SCR denitration catalyst is characterized by comprising the following steps:
(1) immersing the pretreated waste SCR denitration catalyst into NH at a liquid-solid ratio of 20: 1-23·H2O、H2O2Magnetically stirring the mixed solution and reacting in a high-pressure reaction kettle for 4-8 hours;
(2) and (3) centrifugally separating the mixture treated in the step (1), and transferring the leaching solution into a volumetric flask.
2. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 1, is characterized in that: before the step (1), the waste SCR denitration catalyst is subjected to high-pressure water washing for 20-30 min, then is immersed in deionized water and is cleaned for 1-2 h with the aid of ultrasonic waves, the waste SCR denitration catalyst is dried and is subjected to ball milling for 30-40 min, and the waste SCR denitration catalyst is sieved by a 150-200-mesh sieve to obtain a reclaimed material of the waste SCR denitration catalyst.
3. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 2, is characterized in that: the ultrasonic power is 40-60 kHz.
4. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 1, is characterized in that: said step (1)) Middle NH3·H2The concentration of O is 5-10 mol/L, H2O2The concentration of (b) is 1 to 5 mol/L.
5. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 4, wherein the method comprises the following steps: NH in the step (1)3·H2The concentration of O is 7-8 mol/L, H2O2The concentration of (b) is 1 to 2 mol/L.
6. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 1, is characterized in that: in the step (1), the reaction temperature is 200-240 ℃, and the rotating speed is 1000-1200 rad/min.
7. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 1, is characterized in that: the waste SCR denitration catalyst is waste V generated in a selective catalytic reduction denitration process2O5-WO3/TiO2A catalyst.
8. The method for leaching vanadium and tungsten elements in the waste SCR denitration catalyst according to claim 1, is characterized in that: the centrifugal speed in the step (2) is 1000-1200 rad/min.
CN202010193863.0A 2020-03-18 2020-03-18 Method for leaching vanadium and tungsten elements in waste SCR denitration catalyst Pending CN111270076A (en)

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CN117025983A (en) * 2023-10-10 2023-11-10 中国科学院过程工程研究所 Method for realizing vanadium-chromium oxidation leaching by adopting combination of ultrasonic external field and micro-bubbles

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CN103160690A (en) * 2011-12-14 2013-06-19 虹京环保有限公司 Method for recovering metal oxide from SCR denitration waste catalyst

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CN103160690A (en) * 2011-12-14 2013-06-19 虹京环保有限公司 Method for recovering metal oxide from SCR denitration waste catalyst

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Publication number Priority date Publication date Assignee Title
CN117025983A (en) * 2023-10-10 2023-11-10 中国科学院过程工程研究所 Method for realizing vanadium-chromium oxidation leaching by adopting combination of ultrasonic external field and micro-bubbles
CN117025983B (en) * 2023-10-10 2023-12-19 中国科学院过程工程研究所 Method for realizing vanadium-chromium oxidation leaching by adopting combination of ultrasonic external field and micro-bubbles

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