CN117551879A - Method for recycling vanadium and tungsten by using waste SCR catalyst - Google Patents
Method for recycling vanadium and tungsten by using waste SCR catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 145
- 239000002699 waste material Substances 0.000 title claims abstract description 131
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 110
- 239000010937 tungsten Substances 0.000 title claims abstract description 110
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 110
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 54
- 238000004064 recycling Methods 0.000 title abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 196
- 239000012074 organic phase Substances 0.000 claims abstract description 92
- 239000002002 slurry Substances 0.000 claims abstract description 91
- 239000003513 alkali Substances 0.000 claims abstract description 80
- 238000002386 leaching Methods 0.000 claims abstract description 35
- 239000007787 solid Substances 0.000 claims abstract description 14
- 230000001360 synchronised effect Effects 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 121
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 75
- 239000003350 kerosene Substances 0.000 claims description 40
- 229910052785 arsenic Inorganic materials 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 37
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 37
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 22
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 15
- 238000011084 recovery Methods 0.000 description 215
- 239000012071 phase Substances 0.000 description 82
- 238000000926 separation method Methods 0.000 description 39
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 33
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 33
- 229910052698 phosphorus Inorganic materials 0.000 description 33
- 239000011574 phosphorus Substances 0.000 description 33
- 229910052710 silicon Inorganic materials 0.000 description 33
- 239000010703 silicon Substances 0.000 description 33
- 239000007788 liquid Substances 0.000 description 29
- 230000008569 process Effects 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 15
- NWJUARNXABNMDW-UHFFFAOYSA-N tungsten vanadium Chemical compound [W]=[V] NWJUARNXABNMDW-UHFFFAOYSA-N 0.000 description 9
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 230000002457 bidirectional effect Effects 0.000 description 3
- 238000000658 coextraction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002918 waste heat Substances 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VXWYQEYFYNAZOD-UHFFFAOYSA-N 2-[3-[(4,4-difluoropiperidin-1-yl)methyl]-4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound FC1(F)CCN(CC2=NN(CC(=O)N3CCC4=C(C3)N=NN4)C=C2C2=CN=C(NC3CC4=C(C3)C=CC=C4)N=C2)CC1 VXWYQEYFYNAZOD-UHFFFAOYSA-N 0.000 description 1
- IKOKHHBZFDFMJW-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-(2-morpholin-4-ylethoxy)pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)OCCN1CCOCC1 IKOKHHBZFDFMJW-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- NEAPKZHDYMQZCB-UHFFFAOYSA-N N-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]ethyl]-2-oxo-3H-1,3-benzoxazole-6-carboxamide Chemical compound C1CN(CCN1CCNC(=O)C2=CC3=C(C=C2)NC(=O)O3)C4=CN=C(N=C4)NC5CC6=CC=CC=C6C5 NEAPKZHDYMQZCB-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- 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
- C22B7/009—General processes for recovering metals or metallic compounds 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
- C22B34/20—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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The application discloses a method for recycling vanadium and tungsten by utilizing a waste SCR catalyst, which comprises the following steps: and S100, crushing the waste SCR catalyst, namely adding the crushed waste SCR catalyst into alkali liquor with the mass concentration of 3.5-5.5% according to the liquid-solid ratio (5-7) to form slurry, conveying the slurry to be extracted to the top of a pulp extraction tower through a slurry pump, enabling an organic phase to enter the tower from the bottom, enabling the organic phase to be in countercurrent contact with the slurry to be extracted in the tower, obtaining an organic phase loaded with vanadium elements and tungsten elements, recording the organic phase as the loaded organic phase, preheating the organic phase in the step S200 after the loaded organic phase flows out from the top of the tower, discharging the slurry after the vanadium elements and tungsten elements are extracted from the bottom of the tower, and conveying the slurry to a heat exchanger to preheat the alkali liquor in the step S100. The method can control the leaching and extraction of vanadium and tungsten in the waste SCR catalyst to be synchronous, and has good extraction effect.
Description
Technical Field
The application relates to the technical field of nonferrous metal metallurgy, in particular to a method for recycling vanadium and tungsten by using a waste SCR catalyst.
Background
Coal-fired power plants are mainly produced from emission sources, and in order to control the emission of nitrogen oxides of a generator set, a Selective Catalytic Reduction (SCR) flue gas denitration technology is generally adopted. SCR catalyst is prepared by TiO 2 Is a carrier, V 2 O 5 、WO 3 Because of the poisoning and deactivation of the catalyst, a large amount of waste SCR denitration catalyst is produced every year. Development of a green recovery technology of a waste SCR catalyst is particularly important for reducing emission of nitrogen oxides and reducing production cost of a power plant. At present, the recovery of the waste SCR catalyst generally adopts repeated processes of leaching crystallization, extraction and the like to realize valuable element distribution extraction, but has long separation process flow, and a large number of operation units of repeated heating, cooling, slurry melting, filtering and the like exist in the process, so that the process energy consumption is huge. At present, a technology for recovering vanadium and tungsten from a waste SCR catalyst with short flow and low energy consumption is not available.
Disclosure of Invention
In view of this, the application provides a method for recovering vanadium and tungsten by using a waste SCR catalyst, and the method couples a leaching process and an extraction separation process to an ore pulp extraction process, so that the leaching and extraction of vanadium and tungsten in the waste SCR catalyst can be controlled to be synchronously carried out, and the efficient separation of valuable elements of vanadium and tungsten is realized.
In a first aspect, the present application provides a method for recovering vanadium tungsten using a spent SCR catalyst, comprising the steps of: s100, crushing the waste SCR catalyst, wherein the crushed waste SCR catalyst is added into alkaline liquor with the mass concentration of 3.5-5.5% according to the liquid-solid ratio (5-7) to form slurry, namely, the slurry to be extracted is needed to be obtained, and the leaching process and the extraction process of the element to be extracted in the waste SCR catalyst are synchronously carried out to prepare the front stage. And S200, conveying the slurry to be extracted to the top of the ore pulp extraction tower through a slurry pump, enabling an organic phase to enter the tower from the bottom of the tower, and enabling the organic phase to be in countercurrent contact with the slurry to be extracted in the tower so as to enable the vanadium element and the tungsten element in the slurry to be extracted to complete synchronous leaching and extraction, and obtaining an organic phase loaded with the vanadium element and the tungsten element, wherein the organic phase is recorded as a loaded organic phase. S300, preheating the organic phase in the step S200 after the loaded organic phase flows out from the top of the tower, discharging slurry after vanadium element and tungsten element are extracted from the bottom of the tower, and conveying the slurry to a heat exchanger for preheating the alkali liquor in the step S100. At the moment, the waste heat of the slurry after extracting the vanadium and the tungsten and the waste heat of the organic phase loaded with the vanadium and the tungsten can be fully utilized, so that the leaching and the extraction reaction at proper temperature can be realized in a short time, the preheating section is reduced, the time of the process flow is shortened, and the height of the ore pulp extraction tower is indirectly shortened. The method has high comprehensive recovery rate of vanadium element and tungsten element, greatly reduces the repeated temperature rising, temperature reducing, filtering, washing and other working sections in the traditional process, and greatly shortens the process flow.
In some of these embodiments, in step S100, the spent SCR catalyst is mechanically crushed to a particle size of-0.074 mm mass fraction of 90% to 95%. At the moment, the leaching effect of vanadium element and tungsten element in the waste SCR catalyst is improved, and forward progress of leaching reaction is promoted.
In some of these embodiments, in step S200, the flow rate of the organic phase is noted as W 1 m/min, and recording the flow rate of the slurry to be extracted as W 2 m/min, satisfy: w is more than or equal to 0.04 2 Less than or equal to 0.09, and W 2 ≤W 1 . Preferably, 0.04.ltoreq.W 2 ≤0.07,0.04≤W 1 ≤0.09,W 2 =W 1 . When the flow rates of the continuous phase (namely the organic phase) and the disperse phase (namely the slurry to be extracted) meet the range, the forward progress of the vanadium element and the tungsten element in the leaching process is facilitated, the leaching kinetics of the vanadium element and the tungsten element is improved, meanwhile, the self parameters (such as the liquid-solid ratio and the alkali solution concentration) of the slurry to be extracted are the flow rate and the components of the organic phase which are adapted to be in countercurrent contact with the slurry to be extracted, the flow rate relation of the organic phase and the slurry to be extracted is further adjusted, the emulsification of liquid drops generated in the countercurrent contact process is avoided, the forward progress of the leaching process is promoted, the good extraction effect is realized while the leaching effect of the vanadium element and the tungsten element is improved, the bidirectional synchronous lifting of leaching and the process flow shortening is facilitated.
In some embodiments, in step S200, the organic phase includes an extractant N263, a secondary octanol, and kerosene, the addition amount of the extractant N263 is 20 to 30% by volume, the addition amount of the secondary octanol is 5 to 10% by volume, and the addition amount of the kerosene is 60 to 75% by volume, based on the volume of the organic phase. The proper organic phase components are beneficial to further improving the extraction effect while taking the leaching process into consideration.
In some embodiments, in step S200, the pulp extraction tower has a tower diameter of 15cm, a tower height of 10m, a tower plate spacing of 2cm to 5cm, and a pulse amplitude of 0.2m to 0.3m and a pulse frequency of 0.25Hz to 0.3Hz. When the tower plate spacing is proper and the pulse amplitude and the pulse frequency are in the ranges, the extraction effect is further improved while the leaching process is considered, the bidirectional synchronous lifting of leaching and extraction is achieved, and the process flow is further shortened. The pulp extraction tower is a baffle plate extraction tower.
In some of these embodiments, in step S200, the temperature within the pulp extraction column is from 70 ℃ to 95 ℃. The preheated organic phase and the preheated alkali liquor enter the extraction tower with the temperature, so that the proper temperature of the leaching process and the extraction process can be achieved in a short time, the forward progress of the vanadium-tungsten leaching reaction is promoted, and meanwhile, the good extraction effect is achieved, namely, the bidirectional lifting of leaching and extraction is facilitated.
In some of these embodiments, in step S100, the solute of the lye comprises sodium hydroxide and sodium carbonate in a mass ratio of 6:4 to 8:2. The solute of the alkali liquor is proper, so that the leaching effect is improved, and the parameter of the extraction process can be better adapted.
In some of these embodiments, the spent SCR catalyst contains the following components in mass content: v (V) 2 O 5 0.5~0.6%、WO 3 3~3.5%、SiO 2 2.5~3%、As 2 O 3 0.3~0.35%、P 2 O 5 0.2 to 0.3%. Preferably, it comprises: v (V) 2 O 5 0.534%、WO 3 3.227%、SiO 2 2.699%、As 2 O 3 0.318%、P 2 O 5 0.267%. The waste SCR catalyst containing the components and the content is more suitable for the method disclosed in the application, and the leaching and extraction synchronous effect is better.
The technical scheme provided by some embodiments of the present application has the beneficial effects that at least includes: the application discloses a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst (namely, the waste SCR catalyst), in particular to a pulp extraction system, which can directly extract vanadium and tungsten elements while leaching the waste SCR catalyst, is a novel recovery process system different from the traditional waste SCR denitration catalyst in alkaline leaching recovery.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of a method for recovering vanadium and tungsten using a spent SCR catalyst as described herein;
FIG. 2 is a schematic flow chart of a method for recovering vanadium and tungsten using a spent SCR catalyst as described herein.
In the figure: 1. an ore pulp extraction tower; 2. a spent SCR catalyst; 3. alkali liquor; 4. a heat exchanger; 5. a slurry melting tank; 6. a pulse device; 7. a condenser; 8. a loaded organic phase storage tank; 9. and an organic phase storage tank.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
The extraction tower is an important separation device in the extraction field, has the advantages of strong continuity, high safety and small investment, and the basic principle is that the disperse phase is in the form of small liquid drops, and the mass transfer is achieved by countercurrent contact in the tower by means of density difference with the continuous phase. The application provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst on the basis of a baffle plate extraction tower, wherein the leaching process and the extraction process are synchronously carried out, the waste heat utilization is good, and vanadium concentrate and tungsten concentrate with high purity are obtained by carrying out sectional back extraction on a loaded organic phase, and then the next refining is carried out. The method reduces the energy consumption of the recovery process of the waste SCR denitration catalyst to a large extent, omits the working sections of repeated heating, cooling, filtering, washing and the like, shortens the process flow, has small equipment investment and has low operation cost of a process system.
Method for recycling vanadium and tungsten by using waste SCR catalyst
Referring specifically to FIG. 1, the present inventionThe application describes a process flow chart of a method for recovering vanadium and tungsten by using a waste SCR catalyst, which specifically comprises the steps of pulp trend and equipment: fully stirring the crushed waste SCR denitration catalyst 2 and preheated alkali liquor 3 in a slurry dissolving tank 5 to obtain slurry to be extracted, conveying the slurry to be extracted into the top of a slurry extraction tower 1 through a slurry pump, fully extracting and transferring mass as a disperse phase and a continuous phase (organic phase), discharging the slurry after vanadium and tungsten extraction from the bottom of the tower through a slurry pump, conveying the slurry to a heat exchanger 4 to preheat the alkali liquor 3, and filtering the slurry after vanadium and tungsten extraction again (conventional filtering) to obtain qualified TiO 2 A carrier.
The method also comprises the following steps of organic phase trend and equipment: the organic phase is preheated and then flows out from the bottom of the tower to enter the tower through an organic phase storage tank 9, the loaded organic phase obtained after full extraction and mass transfer with the dispersed phase (slurry to be extracted) flows out from the top of the tower, and flows into the loaded organic phase storage tank 8 after preheating the empty organic phase (namely the organic phase before mass transfer with the slurry to be extracted) through a heat exchanger 4, the effect of the tower top condenser 7 is to prevent evaporation of the organic phase, the pulse device 6 can drive the continuous phase to perform up-down pulse motion, and the dispersed phase is dispersed into dispersed phase liquid drops with proper size due to gravity and drag force brought by the continuous phase, so that the dispersed phase and the organic phase perform normal countercurrent mass transfer process in the tower, and the mass transfer performance is remarkably improved.
Referring back to fig. 2, the method specifically includes the following steps:
s100, crushing the waste SCR catalyst, and adding the crushed waste SCR catalyst into alkaline liquor with the mass concentration of 3.5-5.5% according to a liquid-solid ratio (5-7) of 1 to form slurry, so as to obtain slurry to be extracted.
And S200, conveying the slurry to be extracted to the top of the ore pulp extraction tower through a slurry pump, enabling an organic phase to enter the tower from the bottom of the tower, enabling the organic phase to be in countercurrent contact with the slurry to be extracted in the tower, and enabling the vanadium element and the tungsten element in the slurry to be extracted to finish synchronous leaching and extraction, so as to obtain an organic phase loaded with the vanadium element and the tungsten element, and marking the organic phase as a loaded organic phase.
S300, preheating the organic phase in the step S200 after the loaded organic phase flows out from the top of the tower, discharging slurry after vanadium element and tungsten element are extracted from the bottom of the tower, and conveying the slurry to a heat exchanger for preheating the alkali liquor in the step S100.
In some embodiments, in step S100, the spent SCR catalyst is mechanically crushed to a particle size of-0.074 mm mass fraction of 90% to 95%.
Illustratively, the spent SCR catalyst is mechanically crushed to a particle size of-0.074 mm, by mass fraction 90%, 91%, 92%, 93%, 94%, 95% or a range of any two of the above values.
In some embodiments, in step S200, the flow rate of the organic phase is noted as W 1 m/min, and recording the flow rate of the slurry to be extracted as W 2 m/min, satisfy: w is more than or equal to 0.04 2 Less than or equal to 0.09, and W 2 ≤W 1 。
Illustratively, the flow rate W of the slurry to be extracted 2 Is 0.04m/min, 0.05m/min, 0.06m/min, 0.07m/min, 0.08m/min, 0.09m/min or a range of any two values.
In some embodiments, in step S200, 0.04+.W 1 ≤0.09。
Illustratively, the flow rate W of the organic phase 1 Is 0.04m/min, 0.05m/min, 0.06m/min, 0.07m/min, 0.08m/min, 0.09m/min or a range of any two values.
In some embodiments, W 2 =W 1 。
In some embodiments, in step S200, the organic phase includes an extractant N263, a secondary octanol, and kerosene, the extractant N263 is added in an amount of 20 to 30% by volume, the secondary octanol is added in an amount of 5 to 10% by volume, and the kerosene is added in an amount of 60 to 75% by volume, based on the volume of the organic phase.
In some embodiments, in step S200, the pulp extraction tower has a tower diameter of 15cm, a tower height of 10m, a tower plate spacing of 2cm to 5cm, and a pulse amplitude of 0.2m to 0.3m and a pulse frequency of 0.25Hz to 0.3Hz.
Illustratively, the tray spacing is 2cm, 3cm, 4cm, 5cm, or a range of any two of the values recited above.
Illustratively, the pulp extraction tower has a pulse amplitude of 0.2m, 0.23m, 0.25m, 0.28m, 0.3m, or a range of any two values recited above.
Illustratively, the pulp extraction tower has a pulse frequency of 0.25Hz, 0.26Hz, 0.27Hz, 0.28Hz, 0.29Hz, 0.3Hz, or a range of any two values.
In some embodiments, in step S200, the temperature within the pulp extraction column is from 70 ℃ to 95 ℃.
Illustratively, the temperature within the slurry extraction column is 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, or a range of any two values recited above.
In some embodiments, in step S100, the solute of the lye comprises sodium hydroxide and sodium carbonate in a mass ratio of 6:4 to 8:2.
In some embodiments, the spent SCR catalyst contains the following components in mass content: v (V) 2 O 5 0.5~0.6%、WO 3 3~3.5%、SiO 2 2.5~3%、As 2 O 3 0.3~0.35%、P 2 O 5 0.2~0.3%。
The method of the present application will be described in detail below with reference to examples of specific parameters.
In order to more intuitively understand the effect of vanadium-tungsten co-extraction of the pulp extraction system, the application is further described by examples below. The influence of the organic phase proportion and the alkali liquor proportion on the vanadium-tungsten co-extraction effect is examined; and then observing the influence of the structural parameters and the operation parameters of the extraction tower on the vanadium-tungsten co-extraction effect.
TABLE 1 elemental species and content of soluble leachate during alkaline leaching of spent SCR catalyst
The present invention is further illustrated by, but not limited to, the following examples.
Example 1
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to the ratio of 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 and mm accounting for 95% are mixed in a slurry melting tank according to the liquid-solid ratio of 5:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2 cm at the flow rate of 0.04m/min, a preheated organic phase prepared from 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 95.11%, the recovery rate of tungsten was 94.89%, the recovery rate of silicon was 0.34%, the recovery rate of arsenic was 0.24%, and the recovery rate of phosphorus was 0.33%.
Example 2
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to the ratio of 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 and mm accounting for 95% are mixed in a slurry dissolving tank according to the liquid-solid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2 cm at the flow rate of 0.04m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 95.69%, the recovery rate of tungsten was 95.24%, the recovery rate of silicon was 0.26%, the recovery rate of arsenic was 0.34%, and the recovery rate of phosphorus was 0.21%.
Example 3
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to the ratio of 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are subjected to pulp mixing in a pulp dissolving tank according to the solid-liquid ratio of 7:1, then a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm is pumped at the flow rate of 0.04m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 95.73%, the recovery rate of tungsten was 95.21%, the recovery rate of silicon was 0.33%, the recovery rate of arsenic was 0.34%, and the recovery rate of phosphorus was 0.28%.
Example 4
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the liquid-solid ratio of 5:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase configured by 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.03%, the recovery rate of tungsten was 95.78%, the recovery rate of silicon was 0.22%, the recovery rate of arsenic was 0.14%, and the recovery rate of phosphorus was 0.29%.
Example 5
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 and mm accounting for 95% are mixed in a slurry dissolving tank according to the liquid-solid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.20%, the recovery rate of tungsten was 96.24%, the recovery rate of silicon was 0.34%, the recovery rate of arsenic was 0.26%, and the recovery rate of phosphorus was 0.27%.
Example 6
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 7:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase configured by 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.23%, the recovery rate of tungsten was 96.34%, the recovery rate of silicon was 0.27%, the recovery rate of arsenic was 0.22%, and the recovery rate of phosphorus was 0.34%.
Example 7
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 5:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase configured by 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.78%, the recovery rate of tungsten was 96.39%, the recovery rate of silicon was 0.29%, the recovery rate of arsenic was 0.34%, and the recovery rate of phosphorus was 0.27%.
Example 8
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.88%, the recovery rate of tungsten was 96.42%, the recovery rate of silicon was 0.26%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.33%.
Example 9
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 3.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 7:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 2cm at the flow rate of 0.04m/min, a preheated organic phase configured by 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.04m/min, the pulse amplitude is adjusted to 0.2m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.89%, the recovery rate of tungsten was 96.73%, the recovery rate of silicon was 0.28%, the recovery rate of arsenic was 0.34%, and the recovery rate of phosphorus was 0.37%.
Example 10
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the liquid-solid ratio of 5:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.22%, the recovery rate of tungsten was 95.88%, the recovery rate of silicon was 0.29%, the recovery rate of arsenic was 0.20%, and the recovery rate of phosphorus was 0.31%.
Example 11
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.21%, the recovery rate of tungsten was 96.00%, the recovery rate of silicon was 0.27%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.30%.
Example 12
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 7:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 96.55%, the recovery rate of tungsten was 95.57%, the recovery rate of silicon was 0.29%, the recovery rate of arsenic was 0.22%, and the recovery rate of phosphorus was 0.34%.
Example 13
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 5:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 20% of N263, 5% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 97.24%, the recovery rate of tungsten was 96.99%, the recovery rate of silicon was 0.28%, the recovery rate of arsenic was 0.36%, and the recovery rate of phosphorus was 0.31%.
Example 14
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 25% of N263, 10% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 97.32%, the recovery rate of tungsten was 97.11%, the recovery rate of silicon was 0.26%, the recovery rate of arsenic was 0.27%, and the recovery rate of phosphorus was 0.31%.
Example 15
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 7:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 97.56%, the recovery rate of tungsten was 97.99%, the recovery rate of silicon was 0.34%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.25%.
Example 16
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the liquid-solid ratio of 5:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 98.11%, the recovery rate of tungsten was 99.02%, the recovery rate of silicon was 0.41%, the recovery rate of arsenic was 0.37%, and the recovery rate of phosphorus was 0.30%.
Example 17
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 98.51%, the recovery rate of tungsten was 99.24%, the recovery rate of silicon was 0.34%, the recovery rate of arsenic was 0.33%, and the recovery rate of phosphorus was 0.29%.
Example 18
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 7:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 98.23%, the recovery rate of tungsten was 99.09%, the recovery rate of silicon was 0.33%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.34%.
Example 19
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 7:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.04m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 98.23%, the recovery rate of tungsten was 99.09%, the recovery rate of silicon was 0.33%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.34%.
Example 20
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are subjected to pulp mixing in a pulp dissolving tank according to the liquid-solid ratio of 5:1, then a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm is pumped at the flow rate of 0.09m/min, a preheated organic phase configured by 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 88.09%, the recovery rate of tungsten was 88.34%, the recovery rate of silicon was 0.28%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.33%.
Example 21
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are subjected to pulp mixing in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm is pumped at the flow rate of 0.09m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 88.93%, the recovery rate of tungsten was 88.42%, the recovery rate of silicon was 0.29%, the recovery rate of arsenic was 0.34%, and the recovery rate of phosphorus was 0.31%.
Example 22
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 6:4, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 7:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 89.07%, the recovery rate of tungsten was 88.43%, the recovery rate of silicon was 0.24%, the recovery rate of arsenic was 0.21%, and the recovery rate of phosphorus was 0.29%.
Example 23
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 5:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase prepared from 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 91.73%, the recovery rate of tungsten was 92.01%, the recovery rate of silicon was 0.24%, the recovery rate of arsenic was 0.28%, and the recovery rate of phosphorus was 0.25%.
Example 24
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 92.21%, the recovery rate of tungsten was 92.97%, the recovery rate of silicon was 0.34%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.28%.
Example 25
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 7:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 92.74%, the recovery rate of tungsten was 93.86%, the recovery rate of silicon was 0.31%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.30%.
Example 26
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 5:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase prepared from 20% of N263, 5% of sec-octanol and 75% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 70 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 92.11%, the recovery rate of tungsten was 92.24%, the recovery rate of silicon was 0.24%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.33%.
Example 27
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 92.88%, the recovery rate of tungsten was 93.87%, the recovery rate of silicon was 0.25%, the recovery rate of arsenic was 0.33%, and the recovery rate of phosphorus was 0.27%.
Example 28
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 5.5% according to 8:2, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 7:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 5cm at the flow rate of 0.09m/min, a preheated organic phase prepared from 30% of N263, 10% of sec-octanol and 60% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.09m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 93.21%, the recovery rate of tungsten was 94.89%, the recovery rate of silicon was 0.24%, the recovery rate of arsenic was 0.29%, and the recovery rate of phosphorus was 0.21%.
Example 29
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.07m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.25m, the pulse frequency is adjusted to 0.25Hz, the temperature in the extraction tower is kept at 65 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 78.1%, the recovery rate of tungsten was 77.6%, the recovery rate of silicon was 0.21%, the recovery rate of arsenic was 0.19%, and the recovery rate of phosphorus was 0.21%.
Example 30
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 1cm at the flow rate of 0.07m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.1m, the pulse frequency is adjusted to 0.2Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. At this time, the slurry cannot normally flow in the tower.
Example 31
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a slurry dissolving tank according to the solid-liquid ratio of 6:1, then the slurry is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 6cm at the flow rate of 0.07m/min, a preheated organic phase configured by 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.4m, the pulse frequency is adjusted to 0.35Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 72.4%, the recovery rate of tungsten was 68.8%, the recovery rate of silicon was 0.19%, the recovery rate of arsenic was 0.22%, and the recovery rate of phosphorus was 0.30%.
Example 32
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.11m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.07m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 85 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 83.4%, the recovery rate of tungsten was 86.3%, the recovery rate of silicon was 0.32%, the recovery rate of arsenic was 0.22%, and the recovery rate of phosphorus was 0.29%.
Example 33
The embodiment provides a pulp extraction system and a separation process suitable for extracting vanadium and tungsten from a waste SCR denitration catalyst, wherein the mass ratio of sodium hydroxide to sodium carbonate is configured into alkali liquor with the mass concentration of 4.5% according to 7:3, the preheated alkali liquor and the waste SCR denitration catalyst with the particle size of-0.074 mm accounting for 95% are mixed in a pulp dissolving tank according to the solid-liquid ratio of 6:1, then the pulp is pumped into a dispersed phase feed inlet at the top of a baffle pulp extraction tower with the plate spacing of 3.5cm at the flow rate of 0.04m/min, a preheated organic phase prepared from 25% of N263, 10% of Zhong Xin and 65% of kerosene is pumped into a continuous phase feed inlet at the bottom of the extraction tower at the flow rate of 0.11m/min, the pulse amplitude is adjusted to 0.3m, the pulse frequency is adjusted to 0.3Hz, the temperature in the extraction tower is kept at 95 ℃, and the recovery rate is directly calculated based on the content of soluble elements in the waste SCR denitration catalyst. The recovery rate of vanadium was 79.3%, the recovery rate of tungsten was 81.2%, the recovery rate of silicon was 0.3%, the recovery rate of arsenic was 0.24%, and the recovery rate of phosphorus was 0.28%.
Comparative examples 1 to 4
Comparative examples 1 to 4 differ from example 14 in that comparative examples 1 to 4 changed part of the parameters in step S100, resulting in the resulting slurry to be extracted unsuitable, specific parameters are shown in table 2, and recovery results are shown in table 3.
Table 2 discussion of parameter values under different conditions
Examples | Alkali mass ratio (hydrogen oxidation) Sodium carbonate sodium | Alkali liquor quality Concentration/% | Liquid-solid Ratio of | Volume ratio of organic phase (extractant N263 sec-octanol kerosene) | Between trays Distance/cm | Dispersed phase flow Speed m/min | Continuous phase flow Speed m/min | Pulse vibration Web/m | Pulse frequency Rate/Hz | In the extraction tower Temperature/. Degree.C |
Example 1 | 6:4 | 3.5 | 5:1 | 20:5:75 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 70 |
Example 2 | 6:4 | 3.5 | 6:1 | 25:10:65 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 85 |
Example 3 | 6:4 | 3.5 | 7:1 | 30:10:60 | 2 | 0.04 | 0.04 | 0.2 | 0.3 | 95 |
Example 4 | 7:3 | 3.5 | 5:1 | 20:5:75 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 70 |
Example 5 | 7:3 | 3.5 | 6:1 | 25:10:65 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 85 |
Example 6 | 7:3 | 3.5 | 7:1 | 30:10:60 | 2 | 0.04 | 0.04 | 0.2 | 0.3 | 95 |
Example 7 | 8:2 | 3.5 | 5:1 | 20:5:75 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 70 |
Example 8 | 8:2 | 3.5 | 6:1 | 25:10:65 | 2 | 0.04 | 0.04 | 0.2 | 0.25 | 85 |
Example 9 | 8:2 | 3.5 | 7:1 | 30:10:60 | 2 | 0.04 | 0.04 | 0.2 | 0.3 | 95 |
Example 10 | 6:4 | 4.5 | 5:1 | 20:5:75 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 70 |
Example 11 | 6:4 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Example 12 | 6:4 | 4.5 | 7:1 | 30:10:60 | 3.5 | 0.07 | 0.07 | 0.25 | 0.3 | 95 |
Example 13 | 7:3 | 4.5 | 5:1 | 20:5:75 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 70 |
Example 14 | 7:3 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Example 15 | 7:3 | 4.5 | 7:1 | 30:10:60 | 3.5 | 0.07 | 0.07 | 0.25 | 0.3 | 95 |
Example 16 | 8:2 | 4.5 | 5:1 | 20:5:75 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 70 |
Example 17 | 8:2 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Example 18 | 8:2 | 4.5 | 7:1 | 30:10:60 | 3.5 | 0.07 | 0.07 | 0.25 | 0.3 | 95 |
Example 19 | 8:2 | 4.5 | 7:1 | 30:10:60 | 3.5 | 0.04 | 0.07 | 0.25 | 0.3 | 95 |
Example 20 | 6:4 | 5.5 | 5:1 | 20:5:75 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 70 |
Example 21 | 6:4 | 5.5 | 6:1 | 25:10:65 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 85 |
Example 22 | 6:4 | 5.5 | 7:1 | 30:10:60 | 5 | 0.09 | 0.09 | 0.3 | 0.3 | 95 |
Example 23 | 7:3 | 5.5 | 5:1 | 20:5:75 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 70 |
Example 24 | 7:3 | 5.5 | 6:1 | 25:10:65 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 85 |
Example 25 | 7:3 | 5.5 | 7:1 | 30:10:60 | 5 | 0.09 | 0.09 | 0.3 | 0.3 | 95 |
Example 26 | 8:2 | 5.5 | 5:1 | 20:5:75 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 70 |
Example 27 | 8:2 | 5.5 | 6:1 | 25:10:65 | 5 | 0.09 | 0.09 | 0.3 | 0.25 | 85 |
Example 28 | 8:2 | 5.5 | 7:1 | 30:10:60 | 5 | 0.09 | 0.09 | 0.3 | 0.3 | 95 |
Example 29 | 7:3 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 65 |
Example 30 | 7:3 | 4.5 | 6:1 | 25:10:65 | 1 | 0.07 | 0.07 | 0.1 | 0.2 | 95 |
Example 31 | 7:3 | 4.5 | 6:1 | 25:10:65 | 6 | 0.07 | 0.07 | 0.4 | 0.35 | 95 |
Example 32 | 7:3 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.11 | 0.07 | 0.3 | 0.3 | 85 |
Example 33 | 7:3 | 4.5 | 6:1 | 25:10:65 | 3.5 | 0.04 | 0.11 | 0.3 | 0.3 | 95 |
Comparative example 1 | 7:3 | 4.5 | 4:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Comparative example 2 | 7:3 | 4.5 | 8:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Comparative example 3 | 7:3 | 3 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
Comparative example 4 | 7:3 | 6 | 6:1 | 25:10:65 | 3.5 | 0.07 | 0.07 | 0.25 | 0.25 | 85 |
TABLE 3 recovery of elements under different conditions
Examples | Vanadium recovery/% | Tungsten recovery/% | Silicon recovery/% | Phosphorus recovery/% | Arsenic recovery/% |
Example 1 | 95.11 | 94.89 | 0.34 | 0.24 | 0.33 |
Example 2 | 95.69 | 95.24 | 0.26 | 0.34 | 0.21 |
Example 3 | 95.73 | 95.21 | 0.33 | 0.34 | 0.28 |
Example 4 | 96.03 | 95.78 | 0.22 | 0.14 | 0.29 |
Example 5 | 96.20 | 96.24 | 0.34 | 0.26 | 0.27 |
Example 6 | 96.23 | 96.34 | 0.27 | 0.22 | 0.34 |
Example 7 | 96.78 | 96.39 | 0.29 | 0.34 | 0.27 |
Example 8 | 96.88 | 96.42 | 0.26 | 0.29 | 0.33 |
Example 9 | 96.89 | 96.73 | 0.28 | 0.34 | 0.37 |
Example 10 | 96.22 | 95.88 | 0.29 | 0.20 | 0.31 |
Example 11 | 96.21 | 96.00 | 0.27 | 0.29 | 0.30 |
Example 12 | 96.55 | 95.57 | 0.29 | 0.22 | 0.34 |
Example 13 | 97.24 | 96.99 | 0.28 | 0.36 | 0.31 |
Example 14 | 97.32 | 97.11 | 0.26 | 0.27 | 0.31 |
Example 15 | 97.56 | 97.99 | 0.34 | 0.29 | 0.25 |
Example 16 | 98.11 | 99.02 | 0.41 | 0.37 | 0.30 |
Example 17 | 98.51 | 99.24 | 0.34 | 0.33 | 0.29 |
Example 18 | 98.23 | 99.09 | 0.33 | 0.29 | 0.34 |
Example 19 | 98.1 | 99.04 | 0.35 | 0.31 | 0.32 |
Example 20 | 88.09 | 88.34 | 0.28 | 0.29 | 0.33 |
Example 21 | 88.93 | 88.42 | 0.29 | 0.34 | 0.31 |
Example 22 | 89.07 | 88.43 | 0.24 | 0.21 | 0.29 |
Example 23 | 91.73 | 92.01 | 0.24 | 0.28 | 0.25 |
Example 24 | 92.21 | 92.97 | 0.34 | 0.29 | 0.28 |
Example 25 | 92.74 | 93.86 | 0.31 | 0.29 | 0.30 |
Example 26 | 92.11 | 92.24 | 0.24 | 0.29 | 0.33 |
Example 27 | 92.88 | 93.87 | 0.25 | 0.33 | 0.27 |
Example 28 | 93.21 | 94.89 | 0.24 | 0.29 | 0.21 |
Example 29 | 78.1 | 77.6 | 0.21 | 0.19 | 0.21 |
Example 30 | 0 | 0 | 0 | 0 | 0 |
Example 31 | 72.4 | 68.8 | 0.19 | 0.22 | 0.30 |
Example 32 | 83.4 | 86.3 | 0.32 | 0.22 | 0.29 |
Example 33 | 79.3 | 81.2 | 0.30 | 0.24 | 0.28 |
Comparative example 1 | 69.4 | 68.3 | 0.24 | 0.29 | 0.26 |
Comparative example 2 | 63.4 | 62.8 | 0.19 | 0.21 | 0.21 |
Comparative example 3 | 56.3 | 58.2 | 0.18 | 0.29 | 0.24 |
Comparative example 4 | 59.4 | 58.5 | 0.27 | 0.22 | 0.23 |
In combination with tables 2 and 3, in example 1, example 1 was matched with example 19 in a suitable range of parameters in the leaching process and the extraction process, and in comparison with example 2 to example 19, it can be seen that the recovery rates of vanadium element and tungsten element in example 1 to example 19 were higher and were not lower than 95%. Therefore, the parameters in the method are in a mutually adaptive relationship, the values of the parameters are suitable for the synchronous leaching and extraction of vanadium and tungsten, and a good extraction effect can be obtained.
Example 29 compared to example 1, it can be seen that an unsuitable ambient temperature for leaching and extraction results in a significant reduction in vanadium-tungsten recovery. As compared with example 1, examples 30 to 31 were found to be unsuitable in plate spacing and disadvantageous in terms of improvement in recovery rate of vanadium tungsten. Compared with example 1, it can be seen that the flow rate of the disperse phase and the continuous phase is not suitable, which is also unfavorable for improving the recovery rate of vanadium and tungsten, namely, in order to realize synchronous performance of the leaching and extraction of vanadium and tungsten and good extraction effect, cooperative cooperation among various parameters is required, the selection of parameters is not suitable or the range among the parameters is not suitable, and the promotion of the recovery rate of vanadium and tungsten is not favorable.
Comparative examples 1 to 4 compared with example 14, it can be seen that the process parameters of the slurries to be extracted of comparative examples 1 to 4 (in particular their liquid-solid ratio to lye and concentration of lye) are unsuitable, which is disadvantageous for the simultaneous progress of the leaching process and the extraction process, and that the parameters of the leaching process and the extraction process are not adapted, which results in an adverse forward progress of the leaching reaction on the one hand and in a failure to achieve a good extraction result simultaneously on the other hand, the recovery rate of vanadium tungsten for comparative examples 1 to 4 is not higher than 70%, whereas the recovery rate of vanadium element for example 14 is as high as 97.32%, the recovery rate of tungsten element is as high as 97.11%, which is significantly higher than the recovery rate of vanadium tungsten for comparative examples 1 to 4, at least about 27%.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (9)
1. A method for recovering vanadium and tungsten by using a waste SCR catalyst, comprising the steps of:
s100, crushing the waste SCR catalyst, and adding the crushed waste SCR catalyst into alkaline liquor with the mass concentration of 3.5-5.5% according to a liquid-solid ratio (5-7) of 1 to form slurry to obtain slurry to be extracted;
S200, conveying the slurry to be extracted to the top of a slurry extraction tower through a slurry pump, enabling an organic phase to enter the tower from the bottom of the tower, and enabling the organic phase to be in countercurrent contact with the slurry to be extracted in the tower so as to enable the vanadium element and the tungsten element in the slurry to be extracted to complete synchronous leaching and extraction, and obtaining an organic phase loaded with the vanadium element and the tungsten element, wherein the organic phase is recorded as a loaded organic phase;
s300, preheating the organic phase in the step S200 after the loaded organic phase flows out from the top of the tower, discharging slurry after vanadium element and tungsten element are extracted from the bottom of the tower, and conveying the slurry to a heat exchanger for preheating the alkali liquor in the step S100.
2. The method according to claim 1, characterized in that in step S100 the spent SCR catalyst is mechanically crushed to a particle size of-0.074 mm in mass fraction of 90% to 95%.
3. The method according to claim 1, characterized in that in step S200 the flow rate of the organic phase is noted as W 1 m/min, and recording the flow rate of the slurry to be extracted as W 2 m/min, satisfy:
0.04≤W 2 less than or equal to 0.09, and W 2 ≤W 1 。
4. A method according to claim 3, wherein at least one of the following conditions is met:
(1)0.04≤W 2 ≤0.07;
(2)0.04≤W 1 ≤0.09;
(3)W 2 =W 1 。
5. the method according to claim 1, characterized in that in step S200, the organic phase comprises extractant N263, sec-octanol and kerosene;
Based on the volume of the organic phase, the addition amount of the extractant N263 is 20-30 vol%, the addition amount of the sec-octanol is 5-10 vol%, and the addition amount of the kerosene is 60-75 vol%.
6. The method according to claim 1, wherein in step S200, the pulp extraction tower has a tower diameter of 15cm, a tower height of 10m, and a tray pitch of 2cm to 5cm;
the pulse amplitude of the ore pulp extraction tower is 0.2m to 0.3m, and the pulse frequency is 0.25Hz to 0.3Hz.
7. The method according to claim 1, wherein in step S200, the temperature in the pulp extraction tower is 70 ℃ to 95 ℃.
8. The method according to claim 1, characterized in that in step S100 the solutes of the lye comprise sodium hydroxide and sodium carbonate;
the mass ratio of the sodium hydroxide to the sodium carbonate is 6:4 to 8:2.
9. The method of claim 1, wherein the spent SCR catalyst comprises the following components in mass content: v (V) 2 O 5 0.5~0.6%、WO 3 3~3.5%、SiO 2 2.5~3%、As 2 O 3 0.3~0.35%、P 2 O 5 0.2~0.3%。
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