CN110117722A - Vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation utilization system and method - Google Patents
Vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation utilization system and method Download PDFInfo
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- CN110117722A CN110117722A CN201910491175.XA CN201910491175A CN110117722A CN 110117722 A CN110117722 A CN 110117722A CN 201910491175 A CN201910491175 A CN 201910491175A CN 110117722 A CN110117722 A CN 110117722A
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- sulfuric acid
- ammonium
- filtrate
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- 239000003054 catalyst Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- WKXHZKXPFJNBIY-UHFFFAOYSA-N titanium tungsten vanadium Chemical compound [Ti][W][V] WKXHZKXPFJNBIY-UHFFFAOYSA-N 0.000 title claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000000706 filtrate Substances 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 40
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 37
- 239000003513 alkali Substances 0.000 claims abstract description 36
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 31
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 25
- 238000002386 leaching Methods 0.000 claims abstract description 22
- 238000009388 chemical precipitation Methods 0.000 claims abstract description 19
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 19
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 19
- 238000012870 ammonium sulfate precipitation Methods 0.000 claims abstract description 15
- 239000010937 tungsten Substances 0.000 claims abstract description 13
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 125
- 239000013049 sediment Substances 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 239000006228 supernatant Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 7
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000000701 coagulant Substances 0.000 claims description 6
- 239000004071 soot Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- -1 metavanadic acid radical ion Chemical class 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 230000036647 reaction Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims 1
- 150000005837 radical ions Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 52
- 239000012267 brine Substances 0.000 abstract description 10
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 8
- 150000003839 salts Chemical group 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 229910003206 NH4VO3 Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012492 regenerant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
-
- 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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1213—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by wet processes, e.g. using leaching methods or flotation techniques
-
- 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
-
- 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
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/14—Alkali metal compounds
- C25B1/16—Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/22—Inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- 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
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Catalysts (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention provides a kind of vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation use methods, after catalyst fines are successively carried out lye except titanium reaction, acid solution removal of impurities, ammonium sulfate precipitation and the heavy tungsten reaction of sulfuric acid, after being electrolysed to gained filtrate, it recycles and utilizes sulfuric acid and lye, and it discloses to be applicable in and adjusts unit, ammonium sulfate precipitation unit, sulfuric acid with the system of this method, pretreatment unit, alkali leaching unit, pH including being sequentially communicated and sink tungsten unit, chemical precipitation except ammonium unit and sodium sulphate electrolysis cells；The acid solution outlet connection pH of sodium sulphate electrolysis cells adjusts unit and the heavy tungsten unit of sulfuric acid, and the lye export connection alkali leaching unit of sodium sulphate electrolysis cells and chemical precipitation remove ammonium unit；It in conjunction with denitrating catalyst recycling recovery process and brine waste treatment for reuse technology, is recycled so that the brine waste generated in production process is available, reduces the generation of waste water, so that catalyst resource utilization process is more environmentally-friendly.
Description
Technical field
The invention belongs to denitrating catalysts to handle disposal technology field, and in particular to vanadium titanium tungsten system denitrating catalyst recycling
Recycling and water circulation utilization system and method.
Background technique
With the integral implementation of " fossil-fuel power plant atmospheric pollutant emission standard " (GB13223-2011), also with selective catalysis
Denitration technology based on former method (SCR) is widely applied in coal-burning power plant.Due to the limit of wherein catalyst service life
System, activity can be gradually reduced.For the catalyst of inactivation, the processing mode considered first is regeneration, if regeneration is still
It cannot restore its activity, then catalyst can only be replaced.
For discarded denitrating catalyst, " coal steam-electric plant smoke denitration engineering legislation-selective catalytic reduction "
(HJ562-2010) recommend to be handled by the way of crushing landfill.However, on the one hand landfill disposal can occupy a large amount of soil
Ground resource；Some toxic elements in another aspect catalyst can enter natural environment due to various effects, bring certain
Environmental risk；The WO that another further aspect catalyst itself contains3、V2O5And TiO2It is all valuable resource, directly landfill will cause
Imitate the waste of resource.Therefore, the substance in denitrating catalyst is separated and recovered to have obtained extensive concern.
Currently, for WO in waste denitration catalyst3、V2O5And TiO2It leaches and extracts and recycle, mainly there is reduction to impregnate
Method, acidic leaching method, alkaline leaching method etc..But during most of technique does not pay close attention to denitrating catalyst resource utilization
The circulating and recovering problem of water eventually generates the salt bearing liquid wastes of high concentration, be easy to cause secondary pollution.Therefore, how to gather de-
The problem of denox catalyst resource utilization and water circulation use technology push green production, are industry urgent need to resolve.
Summary of the invention
In order to solve problems of the prior art, the invention discloses a kind of vanadium titanium tungsten system denitrating catalyst resources
Change recycling and water circulation utilization system and method, realizes following for soda acid during vanadium titanium tungsten system denitrating catalyst resource utilization
Ring utilizes.
To achieve the goals above, the technical solution adopted by the present invention is that, vanadium titanium tungsten system denitrating catalyst resource utilization
With water circulation use method, comprising the following steps:
Step 1, catalyst fines of the partial size less than 100 mesh are obtained after denitrating catalyst being pre-processed；
Step 2, step 1 gained catalyst fines are mixed with sodium hydroxide solution, heats and stir, sufficiently reacts laggard
Row filtering obtains the sediment A containing titanium dioxide and containing alkaline filtrate B, collects sediment A；
Step 3, sulphur acid for adjusting pH value is added into step 2 gained alkaline filtrate B to clean, products therefrom is stood and is analysed
Crystal C out, then be filtered removal crystal C and obtain filtrate, the pH value of the filtrate is adjusted, is obtained containing vanadic acid radical ion and tungsten
The filtrate D of acid ion；
Step 4, step 3 gained filtrate D is mixed with ammonium sulfate, is stirred to react after stablizing, is obtained by filtration containing metavanadic acid
The sediment E of ammonium and contain tungstate ion and ammonium ion (NH4 +) filtrate F, collect sediment E；
Step 5, sulfuric acid is added into step 4 gained filtrate F, is stirred to react, generate sediment, be obtained by filtration containing wolframic acid
Solid G and filtrate H containing ammonium ion, collect sediment G；
Step 6, sodium hydroxide solution is added into step 5 gained filtrate H and adjusts pH, add MgSO4And Na2HPO4It is raw
At Mg (NH4)PO4Then precipitating is added the suspended matter in coagulant removal water body, staticly settles after reaction, realize and be separated by solid-liquid separation,
Obtain supernatant I and sediment J；
Step 7, step 6 gained supernatant I progress cell reaction is obtained into sulfuric acid solution and sodium hydroxide solution, recycles sulphur
Acid solution and sodium hydroxide solution；
Step 8, the sulfuric acid solution recycled in step 7 is back to step 3 and step 5, sodium hydroxide solution is back to
Step 2 and step 6.
Sodium hydroxide solution used in step 2 is that concentration is 30wt%-50wt%, and catalyst fines are molten with sodium hydroxide
The ratio between liquid is 1g:(4mL-10mL).
The concentration of sulfuric acid solution is 30wt%-50wt%, pH adjustable range 8-12 in step 3.
The additional amount of ammonium salt is according to V and NH in step 44 +Molar ratio be 1:(2-6).
The additional amount of sulfuric acid is according to tungsten and sulfate ion (SO in step 54 2-) molar ratio be 1:(2-6).
PH is adjusted to 6-9 using sodium hydroxide solution in step 6, MgSO is added4And Na2HPO4So that Mg:N:P's rubs
You are than being 1:1:1.
Coagulant is the polyaluminum sulfate aluminum solutions that mass concentration is 5%-15% in step 6.
It is electrolysed in step 7 using constant current.
The system of a kind of vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation use method, including what is be sequentially communicated
Pretreatment unit, alkali leaching unit, pH adjust unit, ammonium sulfate precipitation unit, sulfuric acid sink tungsten unit, chemical precipitation except ammonium unit with
And sodium sulphate electrolysis cells；Alkali soaks unit, pH adjusts unit, ammonium sulfate precipitation unit, sulfuric acid sink tungsten unit, chemical precipitation except ammonium
Unit sodium sulphate electrolysis cells are provided with independent reaction chamber；And it is connected between adjacent reaction chamber by process pipe, sulphur
The acid solution outlet connection pH of sour sodium electrolysis cells adjusts unit and the heavy tungsten unit of sulfuric acid, the lye export of sodium sulphate electrolysis cells
It connects alkali leaching unit and chemical precipitation removes ammonium unit；Pretreatment unit includes soot cleaning system and grinding system, wherein soot cleaning system
For removing dust in catalyst, the discharge port connection alkali of grinding system soaks unit, has heating inside the reaction chamber of alkali leaching unit
Device.
Medium flow direction is provided with valve, flowmeter and liquid delivery pump on process pipe between the reaction chamber；
Alkali leaching unit, pH adjust unit, ammonium sulfate precipitation unit and sulfuric acid sink tungsten unit reaction chamber inside be provided with stirring dress
It sets.
Compared with prior art, vanadium titanium tungsten disclosed by the invention system denitrating catalyst resource utilization and water circulation use dress
It sets and method, improves vanadium titanium tungsten system denitrating catalyst resource utilization efficiency, and combine brine waste treatment for reuse technology, make
The brine waste that generates in production process is available recycles, reduce the generation of waste water, so that catalyst recycling
Removal process is more environmentally-friendly.
Further, catalyst is ground into the contact area that solid-liquid reaction is improved less than 100 mesh powders, favorably
The abundant leaching of the substances such as Yu Fan, tungsten.
Further, before precipitation technique, using sulphur acid for adjusting pH and removing impurity by means of precipitation is carried out, silicon in solution, aluminium can be removed
Influence of the equal impurity to subsequent precipitation, heavy tungsten technique, improves the purity of regenerant.
Further, precipitation and the reaction of heavy tungsten are carried out respectively using ammonium sulfate and sulfuric acid, drug is cheap and easy to get, technological operation
Simply.
Further, strong brine is handled using electrolysis process, recycling obtains acid solution and lye, can be back to de-
Denox catalyst recycling and water treatment technology, realize recycling for waste water.
Detailed description of the invention
Fig. 1 is the process flow chart of vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation use；
Fig. 2 is vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation utilization system schematic diagram.
In attached drawing: 1- pretreatment unit, 2- alkali leaching unit, 3-pH adjust unit, 4- ammonium sulfate precipitation unit, 5- sulfuric acid and sink
Tungsten unit, 6- chemical precipitation remove ammonium unit, 7- sodium sulphate electrolysis cells.
Specific embodiment
Present invention will be further explained by specific examples below, but these embodiments are only in more detail specifically
Ground purposes of discussion but should not be understood as present invention is limited in any form.
As shown in Figure 1, vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation use method, comprising the following steps:
Step 1, catalyst fines of the partial size less than 100 mesh are obtained after denitrating catalyst being pre-processed；
Step 2, step 1 gained catalyst fines are mixed with sodium hydroxide solution, heats and stir, sufficiently reacts laggard
Row filtering obtains the sediment A containing titanium dioxide and containing alkaline filtrate B, collects sediment A；
Step 3, sulphur acid for adjusting pH value is added into step 2 gained alkaline filtrate B to clean, products therefrom is stood and is analysed
Crystal C out, then be filtered removal crystal C and obtain filtrate, the pH value of the filtrate is adjusted, is obtained containing vanadic acid radical ion and tungsten
The filtrate D of acid ion；
Step 4, step 3 gained filtrate D is mixed with ammonium sulfate, is stirred to react after stablizing, is obtained by filtration containing metavanadic acid
The sediment E of ammonium and filtrate F containing tungstate ion and ammonium root collects sediment E；
Step 5, sulfuric acid is added into step 4 gained filtrate F, is stirred to react, generate sediment, be obtained by filtration containing wolframic acid
Solid G and filtrate H containing ammonium ion, collect sediment G；
Step 6, sodium hydroxide solution is added into step 5 gained filtrate H and adjusts pH, add MgSO4And Na2HPO4It is raw
At Mg (NH4)PO4Then precipitating is added the suspended matter in coagulant removal water body, staticly settles after reaction, realize and be separated by solid-liquid separation,
Obtain supernatant I and sediment J；
Step 7, step 6 gained supernatant I progress cell reaction is obtained into sulfuric acid solution and sodium hydroxide solution, recycles sulphur
Acid solution and sodium hydroxide solution；
Step 8, the sulfuric acid solution recycled in step 7 is back to step 3 and step 5, sodium hydroxide solution is back to
Step 2 and step 6.
Sodium hydroxide solution used in step 2 is that concentration is 30wt%-50wt%, and catalyst fines are molten with sodium hydroxide
The ratio between liquid is 1g:(4mL-10mL).
The concentration of sulfuric acid solution is 30wt%-50wt%, pH adjustable range 8-12 in step 3.
The additional amount of ammonium salt is according to V and NH in step 44 +Molar ratio be 1:(2-6).
The additional amount of sulfuric acid is according to tungstate ion and SO in step 54 2-Molar ratio be 1:(2-6).
PH is adjusted to 6-9 using sodium hydroxide solution in step 6, MgSO is added4And Na2HPO4So that Mg:N:P's rubs
You are than being 1:1:1.
Coagulant is the polyaluminum sulfate aluminum solutions that mass concentration is 5%-15% in step 6.
It is electrolysed in step 7 using constant current.
Embodiment 1
Discarded vanadium titanium tungsten system's denitrating catalyst carries out deashing in pretreatment unit 1, is crushed and grinds and be sieved and is made
Partial size is sent into the reaction chamber of the alkali leaching unit 2 using sodium hydroxide less than 100 mesh powders；It is 40% that mass fraction, which is added,
NaOH solution, wherein the solid-to-liquid ratio of catalyst fines and NaOH solution is 1g:5mL, is then heated to 80 DEG C, constant temperature is stirred to react
4 hours；Reaction product is obtained after filtering containing TiO2Sediment and alkaline filtrate containing vanadium and tungsten；Filtrate is sent into
The reaction chamber of unit 3 is adjusted using the pH of sulfuric acid, and the H that mass fraction is 30% is added2SO4Solution adjusts pH value to 11, stands
It is filtered after 12h, removes crystalline solid, after filtrate is adjusted to pH=11, be delivered to the reaction chamber of ammonium sulfate precipitation unit 4,
(NH is added4)2SO4 solution, wherein V:NH4 +Molar ratio be 1:6, stood after being stirred to react 1.5h, filtrate be obtained by filtration and contains
There is NH4VO3Sediment；Filtrate is sent to sulfuric acid again and sinks the reaction chamber of tungsten unit 5, the concentrated sulfuric acid is added, wherein W:SO4 2+Mole
Than being stood after being stirred to react 1.5h, filtrate and the solid containing wolframic acid being obtained by filtration for 1:4；It is heavy except ammonium to chemistry that filtrate is sent
The reaction chamber of unit 6 is added 40% NaOH solution adjustment pH to 8, MgSO is added4And Na2HPO4, so that Mg:N:P=1:1:
1, it is stirred to react the polyaluminium sulfate of addition 10% after 3h, is stirred to react 10min, 30min is precipitated, obtains sediment and supernatant
Liquid, the sediment include Mg (NH4)PO4And polyaluminium sulfate；Supernatant is sent into the reaction chamber of sodium sulphate electrolysis cells 7,
Adjusting current density is 1600A/m2, electrolysis time 10 hours, sulfuric acid solution reuse in sour tank to pH adjusted unit 3 and sulfuric acid
Heavy tungsten unit 5, NaOH solution reuse to the alkali in alkali tank soaks unit 2 and chemical precipitation removes ammonium unit 6.
Embodiment 2
Discarded vanadium titanium tungsten system's denitrating catalyst carries out deashing in pretreatment unit 1, is crushed and grinds and be sieved and is made
Partial size is no more than 100 mesh powders, is sent into the reaction chamber of the alkali leaching unit 2 using sodium hydroxide；It is 30% that mass fraction, which is added,
NaOH solution, wherein the solid-to-liquid ratio of catalyst fines and NaOH solution is 1g:4mL, is then heated to 100 DEG C, constant temperature stirring
Reaction 6 hours；Reaction product is obtained after filtering containing TiO2Sediment and alkaline filtrate containing vanadium and tungsten；By filtrate
It is sent into the reaction chamber for adjusting unit 3 using the pH of sulfuric acid, the H that mass fraction is 40% is added2SO4Solution adjusting pH value is quiet to 8
It is filtered after setting 12h, removes crystalline solid, after filtrate is adjusted to pH=12, be delivered to the reaction of ammonium sulfate precipitation unit 4
(NH is added in room4)2SO4 solution, wherein V:NH4 +Molar ratio be 1:2, stand, be obtained by filtration containing tungsten after being stirred to react 1.5h
The filtrate of acid ion and ammonium ion and contain NH4VO3Sediment；It again will be containing tungstate ion and ammonium ion
Filtrate, which is sent to sulfuric acid, sinks the reaction chamber of tungsten unit 5, the concentrated sulfuric acid is added, wherein W:SO4 2+Molar ratio be 1:2, be stirred to react 1.5h
After stand, the filtrate containing ammonium ion and the solid containing wolframic acid is obtained by filtration；Filtrate containing ammonium ion is sent to change
The heavy reaction chamber except ammonium unit 6 is learned, 30% NaOH solution adjustment pH to 6 is added, MgSO is added4And Na2HPO4, so that Mg:N:
P=1:1:1, be stirred to react be added after 3h 5% polyaluminium sulfate, be stirred to react 20min, precipitate 60min, obtain sediment with
And supernatant；The supernatant is sent into the reaction chamber of sodium sulphate electrolysis cells 7, adjusting current density is 1000A/m2, electrolysis
Time 12 hours, sulfuric acid solution reuse in sour tank to pH adjusted unit 3 and sulfuric acid sinks tungsten unit 5, the NaOH solution in alkali tank
Reuse to alkali soaks unit 2 and chemical precipitation removes ammonium unit 6.
Embodiment 3
Discarded vanadium titanium tungsten system's denitrating catalyst carries out deashing in pretreatment unit 1, is crushed and grinds and be sieved and is made
Partial size is no more than 100 mesh powders, is sent into the reaction chamber of the alkali leaching unit 2 using sodium hydroxide；It is 50% that mass fraction, which is added,
NaOH solution, wherein the solid-to-liquid ratio of catalyst fines and NaOH solution is 1g:10mL, is then heated to 90 DEG C, constant temperature stirring
Reaction 2 hours；Reaction product is obtained after filtering containing TiO2Sediment and alkaline filtrate containing vanadium and tungsten；By filtrate
It is sent into the reaction chamber for adjusting unit 3 using the pH of sulfuric acid, the H that mass fraction is 50% is added2SO4Solution adjusting pH value is quiet to 12
It is filtered after setting 12h, removes crystalline solid, after filtrate is adjusted to pH=11, be delivered to the reaction of ammonium sulfate precipitation unit 4
(NH is added in room4)2SO4 solution, wherein V:NH4 +Molar ratio be 1:6, stood after being stirred to react 1.5h, tungstate radicle be obtained by filtration
The filtrate of ion and ammonium ion and contain NH4VO3Sediment；Again by the filtrate of tungstate ion and ammonium ion send to
The reaction chamber of the heavy tungsten unit 5 of sulfuric acid, is added the concentrated sulfuric acid, wherein W:SO4 2+Molar ratio be 1:6, stood after being stirred to react 1.5h,
The filtrate containing ammonium ion and the solid containing wolframic acid is obtained by filtration；It is heavy except ammonium unit to chemistry that the filtrate of ammonium ion is sent
6 reaction chamber is added 50% NaOH solution adjustment pH to 9, MgSO is added4And Na2HPO4, so that Mg:N:P=1:1:1, is stirred
The polyaluminium sulfate for mixing addition 15% after reacting 3h is stirred to react 15min, precipitates 45min, obtains sediment and supernatant；
The supernatant is sent into the reaction chamber of sodium sulphate electrolysis cells 7, adjusting current density is 1800A/m2, electrolysis time 6 hours,
Sulfuric acid solution reuse in sour tank adjusts unit 3 and the heavy tungsten unit 5 of sulfuric acid to pH, and NaOH solution reuse to the alkali in alkali tank soaks single
Member 2 and chemical precipitation remove ammonium unit 6.
As shown in Fig. 2, a kind of vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation utilization system, including successively connect
Logical pretreatment unit 1, alkali leaching unit 2, pH adjust unit 3, ammonium sulfate precipitation unit 4, sulfuric acid and sink tungsten unit 5, chemical precipitation
Except ammonium unit 6 and sodium sulphate electrolysis cells 7；Alkali soaks unit 2, pH adjusts the heavy tungsten list of unit 3, ammonium sulfate precipitation unit 4, sulfuric acid
Member 5, chemical precipitation remove 6 sodium sulphate electrolysis cells 7 of ammonium unit and are provided with independent reaction chamber；And lead between adjacent reaction chamber
Process pipe connection is crossed, the acid solution outlet connection pH of sodium sulphate electrolysis cells 7 adjusts unit 3 and the heavy tungsten unit 5 of sulfuric acid, sulfuric acid
The lye export connection alkali leaching unit 2 of sodium electrolysis cells 7 and chemical precipitation remove ammonium unit 6；Pretreatment unit 1 includes soot cleaning system
And grinding system, wherein soot cleaning system has heating device inside the reaction chamber of alkali leaching unit 2 for removing dust in catalyst；
Agitating device is provided with inside reaction chamber；PH adjusts unit 3 and chemical precipitation except the interior pH that is equipped with of the reaction chamber of ammonium unit 6 is monitored
Device；Reaction chamber top opens up feed inlet and dosing mouth；The discharge gate of the feed inlet connection alkali leaching unit 2 of pH adjusting unit 3,
The discharge gate connection pH of ammonium sulfate precipitation unit 4 adjusts the discharge gate of unit 3, and the feed inlet of the heavy tungsten unit 5 of sulfuric acid is connected to sulfuric acid
The discharge gate of ammonia-sinking vanadium unit 4, chemical precipitation are connected to the discharge gate of the heavy tungsten unit 5 of sulfuric acid except the feed inlet of ammonium unit 6, and chemistry is heavy
The feed inlet to form sediment except the discharge gate connection sodium sulphate electrolysis cells 7 of ammonium unit 6.
Medium flow direction is provided with valve, flowmeter and liquid delivery pump on each segment process pipeline.
The reaction chamber of sodium sulphate electrolysis cells 7 includes acid compartment, salt room, alkaline chamber, sour tank, brine tank and alkali tank；Acid compartment and
Sour tank, salt room and brine tank, alkaline chamber are connected to by pipeline respectively with alkali tank；Brine tank be connected to chemical precipitation remove ammonium unit 6, acid compartment and
It is provided with anion-exchange membrane between salt room, cation-exchange membrane is set between salt room and alkaline chamber, anode plate, alkali are set in acid compartment
Indoor setting cathode plate, alkaline chamber and alkali tank diconnected, sour tank and acid compartment diconnected, brine tank and salt room diconnected, acid
Tank, which leads to, is provided with liquid delivery pump on the pipeline of acid compartment, brine tank, which is led on the pipeline of salt room, is provided with liquid delivery pump, alkali
Tank, which leads to, is provided with liquid delivery pump on the pipeline of alkaline chamber；Alkali tank is also connected with alkali leaching unit 2 and chemical precipitation except ammonium unit 6；Acid
Tank connects pH and adjusts unit 3 and the heavy tungsten unit 5 of sulfuric acid.
Although inventions have been a degree of descriptions, it will be apparent that, do not departing from the spirit and scope of the present invention
Under conditions of, the appropriate variation of each condition can be carried out.It is appreciated that the present invention is not limited to the embodiments, and it is attributed to power
The range that benefit requires comprising the equivalent replacement of each factor.
Claims (10)
1. vanadium titanium tungsten system denitrating catalyst resource utilization and water circulation use method, which comprises the following steps:
Step 1, catalyst fines of the partial size less than 100 mesh are obtained after denitrating catalyst being pre-processed；
Step 2, step 1 gained catalyst fines are mixed with sodium hydroxide solution, heats and stirs, sufficiently carried out after reaction
Filter obtains the sediment A containing titanium dioxide and containing alkaline filtrate B, collects sediment A；
Step 3, sulphur acid for adjusting pH value is added into step 2 gained alkaline filtrate B to clean, products therefrom is stood, crystalline substance is precipitated
Body C, then be filtered removal crystal C and obtain filtrate, the pH value of the filtrate is adjusted, is obtained containing metavanadic acid radical ion and wolframic acid
The filtrate D of radical ion；
Step 4, step 3 gained filtrate D is mixed with ammonium sulfate, is stirred to react after stablizing, is obtained by filtration containing ammonium metavanadate
Sediment E and filtrate F containing tungstate ion and ammonium ion collects sediment E；
Step 5, sulfuric acid is added into step 4 gained filtrate F, is stirred to react, generate sediment, consolidating containing wolframic acid is obtained by filtration
Body G and filtrate H containing ammonium ion collects sediment G；
Step 6, sodium hydroxide solution is added into step 5 gained filtrate H and adjusts pH, add MgSO4And Na2HPO4Generate Mg
(NH4)PO4Then precipitating is added the suspended matter in coagulant removal water body, staticly settles after reaction, realize and be separated by solid-liquid separation, obtain
Supernatant I and sediment J；
Step 7, step 6 gained supernatant I progress cell reaction is obtained into sulfuric acid solution and sodium hydroxide solution, recycling sulfuric acid is molten
Liquid and sodium hydroxide solution；
Step 8, the sulfuric acid solution recycled in step 7 is back to step 3 and step 5, sodium hydroxide solution is back to step 2
With step 6.
2. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, sodium hydroxide solution used in step 2 is that concentration is 30wt%-50wt%, catalyst fines and sodium hydroxide solution
The ratio between be 1g:(4mL-10mL).
3. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, the concentration of sulfuric acid solution is 30wt%-50wt%, pH adjustable range 8-12 in step 3.
4. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, the additional amount of ammonium salt is 1:(2-6 according to the molar ratio of vanadium and ammonium ion in step 4).
5. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, the additional amount of sulfuric acid is 1:(2-6 according to the molar ratio of tungsten and sulfate ion in step 5).
6. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, pH is adjusted to 6-9 using sodium hydroxide solution in step 6, MgSO is added4And Na2HPO4So that the molar ratio of Mg:N:P
For 1:1:1.
7. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, coagulant is the polyaluminum sulfate aluminum solutions that mass concentration is 5%-15% in step 6.
8. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation use method, feature
It is, is electrolysed in step 7 using constant current.
9. a kind of for realizing vanadium titanium tungsten system denitrating catalyst resource utilization described in claim 1 and water circulation use method
System, which is characterized in that pretreatment unit (1), alkali leaching unit (2), pH including being sequentially communicated adjust unit (3), ammonium sulfate
Precipitation unit (4), sulfuric acid sink tungsten unit (5), chemical precipitation removes ammonium unit (6) and sodium sulphate electrolysis cells (7)；Alkali soaks unit
(2), pH adjusts unit (3), ammonium sulfate precipitation unit (4), sulfuric acid heavy tungsten unit (5), chemical precipitation except ammonium unit (6) sodium sulphate
Electrolysis cells (7) are provided with independent reaction chamber；And it is connected between adjacent reaction chamber by process pipe, sodium sulphate electrolysis
The acid solution outlet connection pH of unit (7) adjusts unit (3) and sulfuric acid sinks tungsten unit (5), the lye of sodium sulphate electrolysis cells (7)
Outlet connection alkali leaching unit (2) and chemical precipitation remove ammonium unit (6)；Pretreatment unit (1) includes soot cleaning system and grinding system,
Wherein soot cleaning system soaks unit (2) for removing dust in catalyst, discharge port connection alkali leaching unit (2) of grinding system, alkali
Reaction chamber inside have heating device.
10. vanadium titanium tungsten according to claim 1 system denitrating catalyst resource utilization and water circulation utilization system, feature
It is, medium flow direction is provided with valve, flowmeter and liquid delivery pump on the process pipe between the reaction chamber；Alkali leaching
Unit (2), pH adjust unit (3), ammonium sulfate precipitation unit (4) and sulfuric acid sink tungsten unit (5) reaction chamber inside be respectively provided with
There is agitating device.
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