CN113713828A - VOCs combustion catalyst prepared by recycling waste ternary lithium batteries and preparation method thereof - Google Patents
VOCs combustion catalyst prepared by recycling waste ternary lithium batteries and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 42
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 28
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000002699 waste material Substances 0.000 title claims abstract description 20
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 15
- 238000004064 recycling Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000002131 composite material Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 31
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- 239000007774 positive electrode material Substances 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- 239000010405 anode material Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 230000007547 defect Effects 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
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- 239000002244 precipitate Substances 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 208000028659 discharge Diseases 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical class Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 28
- 230000004048 modification Effects 0.000 abstract description 5
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- 206010058490 Hyperoxia Diseases 0.000 abstract 1
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 32
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 22
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 10
- 239000013067 intermediate product Substances 0.000 description 10
- 229910044991 metal oxide Inorganic materials 0.000 description 10
- 150000004706 metal oxides Chemical class 0.000 description 10
- 235000006408 oxalic acid Nutrition 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 239000001294 propane Substances 0.000 description 7
- 230000010718 Oxidation Activity Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000012467 final product Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
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- 230000000052 comparative effect Effects 0.000 description 5
- 238000000643 oven drying Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 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 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 but Co Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- B01J35/64—Pore diameter
- B01J35/651—50-500 nm
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
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- F23G2209/00—Specific waste
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Abstract
The invention discloses a VOCs (volatile organic compounds) combustion catalyst prepared by recycling waste ternary lithium batteries and a preparation method thereof, belonging to the technical field of catalyst preparation. Discharging → disassembling → mechanical stripping → acid soluble metal ion → filtering to remove insoluble impurities → salifying precipitation → alkali solution modification process is carried out on the waste ternary lithium battery to obtain the CoMnNiO containing hyperoxia defectxThe oxides are compounded, so that the high-efficiency catalytic purification of VOCs is realized.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a VOCs (volatile organic compounds) combustion catalyst prepared by recycling waste ternary lithium batteries and a preparation method thereof.
Background
Ternary lithium-ion batteries (TLIBs) are widely applied to the fields of consumer electronics product markets, electric vehicles, power grid energy storage and the like because of the advantages of high energy density, high storage capacity, good rate capability and the like. According to the statistics of Avermenni energy company, the total using capacity of 2016 global lithium batteries (LIBs) reaches 80GWh, which is about six million single batteries. With the further increase of the demand of electric automobiles, the ternary lithium battery will meet a new increasing demand. However, the safe recovery and green disposal of the waste ternary lithium battery are still key links for the development of the lithium battery industry.
Volatile Organic Compounds (VOCs) have received widespread attention by governments and the public due to significant pollution emissions, adverse environmental effects and serious health risks to humans. Among the technologies for controlling VOCs, the catalytic oxidation method is considered to be a technology having a wide application range due to its advantages of high efficiency, energy saving, low toxic by-products, and the like. In recent years, such as Co3O4、MnO2And the transition metal oxides such as NiO and the like have excellent oxidation-reduction performance and good active oxygen mobility, so that the transition metal oxides have good catalytic performance potential in the catalytic oxidation reaction of VOCs. Because TLIBs have Co and Ni elements with relatively high price, if the transition metal elements in TLIBs can be recycled to prepare the composite oxide type VOCs catalyst, the environmental and economic benefits can be better in both the resource utilization of waste TLIBs and the pollution control of VOCs.
Although Chinese patent CN107694559B discloses a similar method for preparing toluene degradation catalyst by recycling waste TLIBs anode material, only MnO with lower economic value is recycled in the method2Co and Ni elements are not effectively used. In general, the recycled TLIBs positive electrode material also contains metal elements such as Li and Al which have an inert effect on catalytic oxidation reactions, and oxygen vacancy defects are considered to be important factors capable of effectively promoting the catalytic activity of the composite oxide. Therefore, the simple and rapid removal of inert metal elements and the improvement of the content of defects on the composite oxide in the process of recycling and preparing the catalyst from the waste LIBs cathode material have important significance in improving the catalytic oxidation activity of VOCs.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and providesA VOCs combustion catalyst prepared by recycling waste ternary lithium batteries and a preparation method thereof are disclosed, wherein the waste ternary lithium batteries are subjected to the process of discharging → disassembling → mechanical stripping → acid soluble metal ions → filtering to remove insoluble impurities → salifying precipitation → alkali solution modification to obtain CoMnNiO containing high oxygen defectsxThe oxides are compounded, so that the high-efficiency catalytic purification of VOCs is realized.
In a first aspect, the invention provides a method for preparing VOCs combustion catalyst by recycling waste ternary lithium batteries, which comprises the following steps:
1) carrying out complete discharge treatment on the waste ternary lithium battery, and carrying out shearing, screening and mechanical stripping treatment to realize separation and crushing of the positive electrode material;
2) adding the anode material powder obtained in the step 1) into a mixed solution of strong acid and hydrogen peroxide;
3) filtering the mixed solution obtained in the step 2) to remove undissolved insoluble impurities to obtain a leachate of the anode material;
4) adding carbonate solution into the leaching solution obtained in the step 3) to promote transition metal Co2+、Mn2+And Ni2+Precipitate is generated, and then the CoMnNiO is obtained after filtration, washing, drying and calcinationxA composite oxide;
5) the CoMnNiO obtained in the step 4) is treatedxAdding the composite oxide into an alkali solution, and stirring to obtain the composite oxide catalyst with high oxygen defect.
The obtained composite oxide catalyst with high oxygen defect at least comprises five metal elements of cobalt, manganese, nickel, aluminum and lithium, and after the alkali treatment modification in the step 5), the molar ratio of the three metal elements of cobalt, manganese and nickel in all the metal elements is at least 99%.
Considering that Al and Li can be dissolved by alkali solution, but Co, Mn and Ni oxides can not react with the alkali solution, Al and Li elements in the composite oxide are obtained by adopting an alkali solution etching one-step precipitation method, and further defect enhancement effect caused by dissolution of Al and Li cations can greatly promote VOCs catalytic oxidation activity of the obtained composite oxide. Therefore, the composite oxide prepared by the alkali solution post-treatment method has the advantages of good low-temperature activity, strong stability, suitability for reactions of various VOCs of different types and the like.
Preferably, in step 2), the strong acid is nitric acid, sulfuric acid, or hydrofluoric acid.
Preferably, in step 2), the mixed solution is heated to 25 to 90 ℃.
Preferably, in the step 4), the carbonate solution is sodium carbonate, sodium bicarbonate, ammonium carbonate, potassium bicarbonate or ammonium bicarbonate, and the concentration is 0.1-10 mol/L.
Preferably, in step 4), the calcination temperature is 200-600 ℃.
Preferably, in the step 5), the alkali solution is sodium hydroxide or potassium hydroxide solution, and the concentration is 0.1-5 mol/L.
Preferably, in step 5), the stirring temperature is 25-95 ℃.
In a second aspect, the present invention provides a VOCs combustion catalyst prepared by the above method.
Preferably, the VOCs combustion catalyst is of a mesoporous structure of 5-80nm and has a specific surface area of 90-200m2/g。
The term "catalytic oxidation" as used herein means that VOCs are oxidized by oxygen to carbon dioxide and water under the action of a catalyst and do not exhibit macroscopic flame combustion. In the catalytic oxidation of VOCs, the temperature at which the conversion of the target VOCs is 10% is referred to as "light-off temperature" and denoted as T10(ii) a The temperature at which the conversion of the target VOCs by catalytic oxidation is 90%, referred to as the "complete conversion temperature", is denoted as T90。
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts the waste ternary lithium electron anode material to realize the recycling of transition metal elements in the ternary lithium electron anode material after a series of treatment processes to obtain the CoMnNiOxA composite oxide. Wherein, the catalyst prepared by taking carbonate as a precipitator is better in activity than the catalyst prepared by oxalic acid precipitator; in addition, the alkaline treatment process achieves increased oxygen defects in the composite oxide that catalyze the combustion of typical VOCs contaminants such as acetone, ethyl acetate, and propaneExhibits excellent catalytic activity in the firing reaction. The high-performance VOCs catalyst prepared by using the anode material of the waste ternary lithium battery not only realizes resource recovery of the waste lithium battery, but also has excellent VOCs catalytic combustion application prospect.
Drawings
FIG. 1 shows a ternary lithium battery anode material and CoMnNiO prepared by the inventionxAn XRD pattern of the composite oxide, wherein each curve represents from bottom to top in sequence: mechanical dismantling, calcining and decarburizing to obtain Li (CoMnNi) O2A ternary positive electrode material; adding the obtained positive electrode material into 1mol/L sodium hydroxide solution, processing for 4h at 80 ℃, filtering, washing and drying to obtain a positive electrode material-NaOH; the intermediate prepared in example 1; the intermediate prepared in example 2; example 2 final product prepared.
FIG. 2 shows CoMnNiO before and after the alkali treatment according to the present inventionxThe EPR results of oxygen vacancy characterization of the composite oxide were compared, wherein two curves represent the intermediate product prepared in example 2 and the final product prepared in example 2 in order from bottom to top.
FIG. 3 is a graph showing the catalytic oxidation activity of propane in the catalyst at various stages of treatment, wherein the positive electrode material curve represents Li (CoMnNi) O obtained after mechanical dismantling and calcination for carbon removal2A ternary positive electrode material; the curve of the positive electrode material-NaOH represents that the obtained positive electrode material is added into 1mol/L sodium hydroxide solution, treated for 4 hours at 80 ℃, filtered, washed and dried to obtain the positive electrode material-NaOH; CoMnNiOxThe oxalic acid profile represents the intermediate product of example 1; CoMnNiOxThe sodium carbonate curve represents the intermediate product of example 2; CoMnNiOxThe sodium carbonate-NaOH curve represents the final product in example 2.
FIG. 4 shows CoMnNiO obtained by different precipitantsxThe catalytic oxidation activity curves of the composite oxide on acetone are shown, wherein two curves represent the intermediate product prepared in example 2 and the intermediate product prepared in example 1 from left to right respectively.
FIG. 5 shows CoMnNiO obtained before and after the alkali treatmentxThe catalytic oxidation activity curve of the composite oxide to ethyl acetate is shown in the specification, wherein two curves are from leftTo the right represent the final product prepared in example 2, the intermediate product prepared in example 2, respectively.
FIG. 6 is a nitrogen desorption curve of a catalyst in which CoMnNiOxThe oxalic acid profile represents the intermediate product of example 1; CoMnNiOxThe sodium carbonate curve represents the intermediate product of example 2; CoMnNiOxThe sodium carbonate-NaOH curve represents the final product in example 2.
FIG. 7 is a pore size distribution diagram of a catalyst in which CoMnNiOxThe oxalic acid profile represents the intermediate product of example 1; CoMnNiOxThe sodium carbonate curve represents the intermediate product of example 2; CoMnNiOxThe sodium carbonate-NaOH curve represents the final product in example 2.
FIG. 8 is a schematic view showing the structure of a small fixed-bed continuous flow reaction evaluating apparatus according to the present invention.
Detailed Description
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Catalyst evaluation methods used in the following examples:
when the catalytic oxidation performance of the VOCs is evaluated, a small fixed bed continuous flow reaction evaluation device shown in fig. 8 is adopted, VOCs gas and oxygen respectively enter a gas mixing device, the mixed gas enters a quartz tube of a reaction furnace (model SK2-1-10K) and is in contact reaction with a catalyst in the quartz tube, and the reacted gas enters a gas chromatograph for detection so as to obtain the catalytic oxidation conversion rate of the VOCs gas.
During testing, 0.1g of catalyst with 40-60 meshes obtained by tabletting and sieving is filled into a quartz tube (the diameter is 6mm), the reaction temperature is controlled by a temperature programming reaction furnace, three gases of propane, acetone or ethyl acetate are selected as VOCs gas, the concentration is 2000ppm, 1000ppm and 1000ppm respectively, and the oxygen concentration is 20%. The space velocity is 18000 g/ml/h-1。
Example 1
Carrying out complete discharge treatment on the waste ternary lithium battery, and carrying out shearing, screening and mechanical stripping treatment to realize separation and crushing of the positive electrode material; adding the anode material powder into a mixed solution of strong acid (nitric acid, sulfuric acid or hydrofluoric acid) and hydrogen peroxide, and heating to 25-90 ℃ to promote the dissolution of metal ions in the anode material; and filtering the mixed solution to remove undissolved insoluble impurities (conductive graphite and the like) to obtain the leachate of the cathode material.
5mol/L oxalic acid solution is continuously and dropwise added into 150mL of the positive electrode material leaching solution until flocculent precipitate is generated. Stirring vigorously for 30min, standing, aging for 12 hr, filtering the obtained precipitate, washing to neutrality, and oven drying at 100 deg.C overnight. Finally, the obtained powder is placed in a muffle furnace to be calcined for 3 hours at 300 ℃ under the air atmosphere to obtain CoMnNiOxA composite metal oxide.
The obtained CoMnNiOxAdding the composite metal oxide into 1mol/L sodium hydroxide solution, stirring and processing for 4 hours at 80 ℃, filtering, washing and drying to obtain the oxygen-deficient composite oxide, which is marked as catalyst A. Catalyst a was used in the catalytic activity tests for propane, acetone and ethyl acetate, respectively.
Example 2
The leachate of the positive electrode material was prepared in the same manner as in example 1.
5mol/L sodium carbonate solution is continuously added dropwise into 150mL of the positive electrode material leaching solution until the pH value is increased to 10. Stirring vigorously for 30min, standing, aging for 12 hr, filtering the obtained precipitate, washing to neutrality, and oven drying at 100 deg.C overnight. Finally, the obtained powder is placed in a muffle furnace to be calcined for 3 hours at 300 ℃ under the air atmosphere to obtain CoMnNiOxA composite metal oxide.
The obtained CoMnNiOxAdding the composite metal oxide into 1mol/L sodium hydroxide solution, stirring and processing for 8 hours at 50 ℃, filtering, washing and drying to obtain the oxygen-deficient composite oxide, which is marked as catalyst B. Catalyst B was used in the catalytic activity tests for propane, acetone and ethyl acetate, respectively.
Example 3
The leachate of the positive electrode material was prepared in the same manner as in example 1.
5mol/L ammonium carbonate solution is continuously added dropwise into 150mL of the positive electrode material leaching solution until the pH value is increased to 10. Drama (E)Stirring vigorously for 30min, standing, aging for 12 hr, filtering the obtained precipitate, washing to neutrality, and oven drying at 100 deg.C overnight. Finally, the obtained powder is placed in a muffle furnace to be calcined for 3 hours at 300 ℃ under the air atmosphere to obtain CoMnNiOxA composite metal oxide.
The obtained CoMnNiOxAdding the composite metal oxide into 1mol/L potassium hydroxide solution, stirring and processing for 4 hours at 80 ℃, filtering, washing and drying to obtain the oxygen-deficient composite oxide which is marked as catalyst C. Catalyst C was used in the catalytic activity tests for propane, acetone and ethyl acetate, respectively.
Comparative example 1
The leachate of the positive electrode material was prepared in the same manner as in example 1.
5mol/L oxalic acid solution is continuously and dropwise added into 150mL of the positive electrode material leaching solution until flocculent precipitate is generated. Stirring vigorously for 30min, standing, aging for 12 hr, filtering the obtained precipitate, washing to neutrality, and oven drying at 100 deg.C overnight. Finally, the obtained powder is placed in a muffle furnace to be calcined for 3 hours at 300 ℃ under the air atmosphere to obtain CoMnNiOxThe composite metal oxide is marked as catalyst R1. Catalyst R1 was used in the catalytic activity tests for propane, acetone and ethyl acetate, respectively.
Comparative example 2
The leachate of the positive electrode material was prepared in the same manner as in example 1.
5mol/L sodium carbonate solution is continuously added dropwise into 150mL of the positive electrode material leaching solution until the pH value is increased to 10. Stirring vigorously for 30min, standing, aging for 12 hr, filtering the obtained precipitate, washing to neutrality, and oven drying at 100 deg.C overnight. Finally, the obtained powder is placed in a muffle furnace to be calcined for 3 hours at 300 ℃ under the air atmosphere to obtain CoMnNiOxThe composite metal oxide is marked as catalyst R2. Catalyst R2 was used in the catalytic activity tests for propane, acetone and ethyl acetate, respectively.
The following table shows the catalytic degradation activity of VOCs for the catalysts prepared in examples 1-3 and comparative examples 1-2
TABLE 1
As can be seen from the catalytic oxidation results of examples 1-3 and comparative examples 1-2, the use of carbonate as a precipitant has higher catalytic oxidation activity and a lower complete conversion temperature of VOCs than the use of expensive oxalic acid. Meanwhile, the obtained composite metal oxide is modified by the alkali solution to remove metal cations such as Al and Li in the crystal, so that the oxygen defect content in the composite metal oxide can be greatly increased (as proved by an EPR result in figure 2), the catalytic activity of the VOCs of the catalyst is further promoted, and the complete degradation temperature of the VOCs can be further reduced by 10-20 ℃. Therefore, the high-performance VOCs catalytic purification catalyst is obtained by resource utilization of the waste ternary lithium battery anode material through creative preparation steps of modifying with carbonate and alkali solution.
Further, as is clear from FIG. 1, in example 2, CoMnNiO produced using sodium carbonate as a precipitantxComposite oxide having diffraction peak higher than that of CoMnNiO prepared in example 1 using oxalic acid as precipitantxThe diffraction peak of the complex oxide is broader, and it can be shown that CoMnNiO prepared in example 2 is widerxThe crystallinity of sodium carbonate is lower and the oxygen vacancy defects contained therein will therefore be more. CoMnNiO treated by homological alkalixSodium carbonate-NaOH also has broad diffraction peaks, indicating the abundance of oxygen vacancy defects.
As can be seen from fig. 3: firstly, the activity of the catalyst treated by the NaOH alkaline solution is obviously improved by comparing the activities of the anode material and the anode material-NaOH. Next, the CoMnNiO of comparative example 1 was passed throughxOxalic acid, CoMnNiO of example 2xSodium carbonate and CoMnNiOxSodium carbonate-NaOH it was found that when sodium carbonate is used as a precipitant, the catalyst activity is better than when conventional oxalic acid precipitant is used, and the NaOH alkali treatment also generates further promoting benefits on the catalyst activity.
Figure 4 further demonstrates that the catalyst prepared using carbonate as a precipitant is more active than oxalic acid precipitant. While figure 5 also demonstrates that the alkaline treatment can further enhance the activity of the catalyst.
FIG. 6 shows that the specific surface area of the combustion catalyst for VOCs is 90 to 200m2The catalyst has a mesoporous structure of 5-80nm as shown in figure 7.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. The method for preparing the VOCs combustion catalyst by recycling the waste ternary lithium battery is characterized by comprising the following steps of:
1) carrying out complete discharge treatment on the waste ternary lithium battery, and carrying out shearing, screening and mechanical stripping treatment to realize separation and crushing of the positive electrode material;
2) adding the anode material powder obtained in the step 1) into a mixed solution of strong acid and hydrogen peroxide;
3) filtering the mixed solution obtained in the step 2) to remove undissolved insoluble impurities to obtain a leachate of the anode material;
4) adding carbonate solution into the leaching solution obtained in the step 3) to promote transition metal Co2+、Mn2+And Ni2+Precipitate is generated, and then the CoMnNiO is obtained after filtration, washing, drying and calcinationxA composite oxide;
5) the CoMnNiO obtained in the step 4) is treatedxAdding the composite oxide into an alkali solution, and stirring to obtain the composite oxide catalyst with high oxygen defect.
2. The method of claim 1, wherein in step 2), the strong acid is nitric acid, sulfuric acid, or hydrofluoric acid.
3. The method of claim 1, wherein in step 2), the mixed solution is heated to 25 to 90 ℃.
4. The method of claim 1, wherein in step 4), the carbonate solution is sodium carbonate, sodium bicarbonate, ammonium carbonate, potassium bicarbonate, or ammonium bicarbonate with a concentration of 0.1 to 10 mol/L.
5. The method as claimed in claim 1, wherein the calcination temperature in step 4) is 200-600 ℃.
6. The method according to claim 1, wherein in the step 5), the alkali solution is a sodium hydroxide or potassium hydroxide solution with a concentration of 0.1 to 5 mol/L.
7. The method of claim 1, wherein in step 5), the stirring temperature is from 25 ℃ to 95 ℃.
8. A combustion catalyst for VOCs prepared by the method of any one of claims 1 to 7.
9. The VOCs combustion catalyst of claim 8, wherein the VOCs combustion catalyst has a mesoporous structure of 5-80nm and a specific surface area of 90-200m2/g。
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| PCT/CN2022/094388 WO2022233340A1 (en) | 2021-09-16 | 2022-05-23 | Vocs combustion catalyst prepared from recycled waste ternary lithium-ion batteries, and preparation method therefor |
| ZA2022/12438A ZA202212438B (en) | 2021-09-16 | 2022-11-15 | Vocs combustion catalyst prepared by recycling ternary lithium-ion batteries and preparation method thereof |
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| CN114832845A (en) * | 2022-05-23 | 2022-08-02 | 濮阳天地人环保科技股份有限公司 | Composite catalyst prepared by utilizing recycled lithium battery material and preparation method thereof |
| WO2022233340A1 (en) * | 2021-09-16 | 2022-11-10 | 中国科学院大学 | Vocs combustion catalyst prepared from recycled waste ternary lithium-ion batteries, and preparation method therefor |
| CN115716660A (en) * | 2022-10-14 | 2023-02-28 | 东南大学 | Composite ternary metal oxide oxygen carrier material and preparation method and application thereof |
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