CN115069272A - Method for synchronously synthesizing visible light response photocatalyst by extracting lithium from anode powder of waste lithium iron phosphate battery - Google Patents
Method for synchronously synthesizing visible light response photocatalyst by extracting lithium from anode powder of waste lithium iron phosphate battery Download PDFInfo
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- iron phosphate
- lithium iron
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 87
- 239000000843 powder Substances 0.000 title claims abstract description 68
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 52
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 43
- 239000002699 waste material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- 230000004298 light response Effects 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 17
- 238000007146 photocatalysis Methods 0.000 claims abstract description 27
- 230000002195 synergetic effect Effects 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000001914 filtration Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 14
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052979 sodium sulfide 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 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 2
- 239000000975 dye Substances 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 2
- 238000005067 remediation Methods 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 26
- 229960000907 methylthioninium chloride Drugs 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 239000008367 deionised water Substances 0.000 description 18
- 229910021641 deionized water Inorganic materials 0.000 description 18
- 239000000243 solution Substances 0.000 description 18
- 238000001782 photodegradation Methods 0.000 description 12
- 229910052724 xenon Inorganic materials 0.000 description 11
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 description 9
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 229910000398 iron phosphate Inorganic materials 0.000 description 5
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000002386 leaching Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 238000000079 presaturation Methods 0.000 description 2
- 229940079101 sodium sulfide Drugs 0.000 description 2
- ZGHLCBJZQLNUAZ-UHFFFAOYSA-N sodium sulfide nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[S-2] ZGHLCBJZQLNUAZ-UHFFFAOYSA-N 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 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
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/0262—Compounds of O, S, Se, Te
- B01J20/0266—Compounds of S
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- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- 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
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Abstract
The invention relates to a method for synchronously synthesizing a visible light response photocatalyst by extracting lithium from anode powder of a waste lithium iron phosphate battery, belonging to a new solid waste resource utilization technology for environmental protection and comprehensive resource utilization. The photocatalyst with the adsorption-photocatalysis synergistic capability is successfully synthesized while lithium is recovered by taking waste lithium iron phosphate batteries as raw materials, and has the advantages of wide visible light absorption range, strong synergistic capability, high removal efficiency and the like. The excellent adsorption-photocatalysis synergistic capability overcomes the defects of the traditional photocatalyst, so that the photocatalyst has the capability of quickly removing organic dyes under visible light. The method has the advantages of simple process, mild conditions and low cost, and the prepared photocatalyst has great application potential in the aspects of wastewater treatment or organic dye polluted site remediation.
Description
Technical Field
The invention relates to a method for synchronously synthesizing visible light response photocatalyst by extracting lithium from waste lithium iron phosphate batteries, in particular to a method for preparing a photocatalyst with the capability of adsorbing and photocatalytic cooperative degradation of pollutants under visible light by using the waste lithium iron phosphate batteries, belonging to a new solid waste treatment technology for environmental protection and resource comprehensive utilization.
Background
With the rapid development of electric vehicles and energy storage power stations, the global market share and commercial yield of lithium iron phosphate batteries are increasing dramatically. Huge yield (2.5X 10 in 2021 years) 5 Ton) generates a large amount of waste lithium iron phosphate batteries, which threatens the environmental safety and also causes huge waste of precious resources. Therefore, the recovery of waste lithium iron phosphate batteries by a profitable method is urgently needed. However, due to the low content of valuable elements, most companies prefer to recover other spent lithium ion batteries (e.g., LiNi) x Mn y Co z O 2 ) Instead of recovering components (such as lithium, cobalt, nickel and manganese) with economic value from the waste lithium iron phosphate batteries, the economic infeasibility greatly hinders the development of waste lithium iron phosphate battery recovery enterprises. Therefore, besides recovering lithium, the urgent need is to make a profitable high-efficiency strategy and convert the waste lithium iron phosphate batteries into high-added-value products so as to improve the economic value of the recovery of the waste lithium iron phosphate batteries.
Water purification, particularly the degradation and removal of organic dyes, is critical to address the growing water pollution. The organic dye is widely applied to various industries such as food, leather, textile, medical treatment, printing, aquaculture and the like, and the annual output exceeds 70 ten thousand tons. Unfortunately, about 14 million tons of organic dyes are discharged into rivers freely without any treatment every year. Due to their harmful, persistent and non-biodegradable nature, the discharged organic dyes pose extremely serious hazards to the environment and humans, such as potential carcinogenic risks to humans and death of aquatic organisms. Photocatalysis and adsorption are considered to be the most efficient and promising method for removing organic dyes due to their low cost and high removal efficiency. However, since photocatalysis is an interfacial reaction, contaminants are degraded at a faster rate only when they diffuse to the photocatalyst surface. Therefore, most photocatalysts require a long pre-saturation time before photodegradation of contaminants, which increases production costs and reduces production efficiency. Although the adsorbent can directly remove pollutants without presaturation, the poor regeneration capability and the complex desorption process limit the large-scale application of the adsorbent. However, compared with the adsorbent, the photocatalyst can be self-regenerated and recycled by free and inexhaustible sunlight, and is an energy-saving and environment-friendly method. Therefore, it is urgent to develop a novel photocatalyst having synergistic effects of adsorption and photocatalysis to improve the removal efficiency of organic dyes.
The invention successfully synthesizes a photocatalyst (NaFeS) with adsorption-photocatalysis synergistic ability by taking a lithium iron phosphate battery as a raw material 2 ) The catalyst has the advantages of wide visible light absorption range, strong synergistic capability, high removal efficiency and the like. Meanwhile, lithium and phosphorus are recovered from the waste lithium iron phosphate batteries, and the profit of recovering the low value-added batteries is greatly improved. Due to the synthesized photocatalyst NaFeS 2 Has excellent synergistic ability of adsorption and photocatalysis, overcomes the defects of the traditional photocatalyst, and can accelerate the efficiency of photocatalysis in the adsorption process so that NaFeS 2 The capability of rapidly removing organic dye under visible light. The method has the advantages of simple process, mild conditions and low cost, greatly improves the recovery profit of the waste lithium iron phosphate battery with low additional value, and prepares the NaFeS with the adsorption-photocatalysis synergistic capability 2 Has great application potential in the aspects of wastewater treatment or organic dye polluted site remediation.
Disclosure of Invention
The invention develops a method for synchronously synthesizing a visible light response photocatalyst by extracting lithium from the anode powder of waste lithium iron phosphate batteries, aiming at the problems of low pollutant removal efficiency, long pre-adsorption process, high cost, low waste lithium iron phosphate batteries and the like of the traditional photocatalyst. The method is realized by the following technical scheme:
the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the anode powder of the waste lithium iron phosphate battery specifically comprises the following steps:
(S1) adding the lithium iron phosphate battery positive electrode powder into the aqueous solution of the lithium extractant at room temperature, and stirring for 30 minutes to obtain lithium iron phosphate battery powder without lithium;
(S2) adding the lithium-removed lithium iron phosphate powder obtained in the step S1 into a sodium sulfide aqueous solution at room temperature, and stirring for 1 hour;
(S3) adjusting the pH of the suspension after the reaction of the step S2 to 6-8, filtering and drying to obtain the photocatalyst with adsorption-photocatalysis synergistic ability.
Further, in the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the cathode powder of the waste lithium iron phosphate battery, the lithium extracting agent in the step (S1) is selected from any one or a mixture of potassium persulfate, ammonium persulfate and sodium persulfate;
further, according to the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the waste lithium iron phosphate battery positive electrode powder, in the step (S1), the mass ratio of the lithium extracting agent to the lithium iron phosphate battery positive electrode powder is 1:0.6-1: 1.5;
further, according to the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the waste lithium iron phosphate battery positive electrode powder, the mass ratio of the lithium iron phosphate powder subjected to lithium removal to sodium sulfide in the step (S2) is 1:1.0-1: 1.3;
further, in the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the cathode powder of the waste lithium iron phosphate battery, in the step (S3), the mixture of any one or more of sulfuric acid, phosphoric acid, hydrochloric acid and nitric acid is used for pH adjustment;
further, in the method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the waste lithium iron phosphate battery positive electrode powder, the main component of the photocatalyst with adsorption-catalysis synergistic ability obtained in the step (S3) is NaFeS 2 。
The principle of the technical scheme of the invention is as follows:
under the action of a leaching agent and a sulfide,the photocatalyst (NaFeS) with the adsorption-catalysis synergistic ability can be successfully synthesized by utilizing the spontaneous and rapid reaction between reactants 2 )。NaFeS 2 Methylene Blue (MB) molecules are adsorbed mainly by two ways: (1) positively charged MB molecules with NaFeS 2 S of 2- /S 2 2- Electrostatic interaction between them; (2) coordination of MB molecules with Fe (II)/Fe (III). Once NaFeS is present 2 NaFeS is exposed to visible light with proton energy of more than (or equal to) 2.35eV (lambda is less than or equal to 529nm) 2 Electron-hole pairs are generated. Then, electrons are photo-generated (e) - ) Excitation from the Valence Band (VB) to the Conduction Band (CB) while in NaFeS 2 VB of (a) generates holes (h) + )。NaFeS 2 With dissolved O in CB of (2) 2 Reaction to form O 2 - It can participate in the degradation of MB. At the same time, dissolved O 2 Can react with electrons and H + Reaction to form H 2 O 2 Then H 2 O 2 Further OH degradation of MB occurs. More importantly, NaFeS 2 Accumulated h in VB of + Due to its strong oxidizing properties, it can directly participate in the degradation of MB through redox reactions. Thus, when NaFeS is used 2 When directly immersed in MB solution, due to NaFeS 2 Excellent adsorption capacity, MB molecules are rapidly adsorbed to NaFeS 2 Surface/vicinity (even without pre-adsorption process), shortening of MB molecules and active oxygen (. O) 2 - And OH) and h + The time required for contact. Therefore, since NaFeS 2 The adsorption-photocatalysis synergistic ability of the MB is greatly improved.
The method has the following outstanding advantages:
1. by adjusting the pH, the photocatalyst NaFeS with the highest yield can be obtained 2 The yield is more than 96%, and the product has good photocatalytic performance.
2. The waste lithium iron phosphate battery is converted into the photocatalyst with the adsorption-photocatalysis synergistic performance, and the economic benefit of recycling the low value-added battery is obviously improved.
3. The synthesized NaFeS is subjected to the synergistic effect of adsorption and photocatalysis 2 Has the capability of quickly removing organic dye under visible light, and overcomes the defects of the traditional photocatalyst.
4. The main elements (Li, P and Fe) in the waste lithium iron phosphate batteries are all recovered as high value-added products, so that the method is a comprehensive profit method.
5. Simple process and low cost. The method has the advantages of mild reaction conditions, high production efficiency and industrial potential.
Drawings
For further understanding of the present invention, the process flow of the present invention, and the photocatalyst NaFeS are described below with reference to the accompanying drawings 2 The performance of (A):
FIG. 1 is a graph of the rate of degradation of methylene blue light catalyzed by the product at various pH's.
FIG. 2 is a photograph of the solution after reaction at different pH.
FIG. 3 shows the difference in Na in comparative examples 5 to 7 2 S and FePO 4 pH of molar ratio and photograph after reaction.
FIG. 4 is NaFeS 2 ，TiO 2 And degrading methylene blue by lithium iron phosphate powder subjected to lithium removal under the conditions of adsorption and photocatalysis.
FIG. 5 is NaFeS 2 ，TiO 2 And degrading methylene blue by the lithium iron phosphate powder without lithium under direct photocatalysis.
FIG. 6 is NaFeS 2 ，TiO 2 And the lithium-removed lithium iron phosphate powder degrades methylene blue in three modes.
The specific implementation mode is as follows:
the following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
Example 1:
5g of lithium iron phosphate battery cathode powder and 3.018g of sodium persulfate were added to 500g of deionized water at room temperature, stirred for 30 minutes, filtered, and dried at 120 ℃ for 4 hours to obtain lithium-removed lithium iron phosphate powder. 2g of lithium-removed phosphorus are takenAdding the ferric lithium powder and 6.3652g of sodium sulfide nonahydrate into 200mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH value to 6, filtering and drying to obtain the photocatalyst NaFeS with the adsorption-photocatalysis synergistic capability 2 (1.80 g of NaFeS was obtained 2 Yield greater than 94.5%). Synthetic NaFeS 2 Under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm), the photodegradation rate of methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min is 90.4% (adsorption-photocatalysis synergistic effect).
Example 2:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 4g of lithium-removed lithium iron phosphate powder and 15.913g of sodium sulfide nonahydrate into 400mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH value to 6, filtering and drying to obtain the photocatalyst NaFeS with adsorption-photocatalysis synergistic ability 2 (3.696 g NaFeS was obtained 2 Yield greater than 96%). Synthetic NaFeS 2 Under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm), the photodegradation rate of methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min is 99.2% (adsorption-photocatalysis synergistic effect).
Example 3:
adding 5g of lithium iron phosphate battery positive electrode powder and 7.544g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 3g of lithium-removed lithium iron phosphate powder and 9.5478g of sodium sulfide nonahydrate into 300mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH value to 8, filtering and drying to obtain the photocatalyst NaFeS with adsorption-photocatalysis synergistic capability 2 (2.748 g NaFeS was obtained 2 Yield greater than 96%). Synthetic NaFeS 2 Under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm), the photodegradation rate of methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min is more than 98.1 percent (adsorption-photocatalysis synergistic effect).
Example 4:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 2g of lithium-removed lithium iron phosphate powder and 7.9565g of sodium sulfide nonahydrate into 200mL of deionized water, stirring for 1 hour, adding sulfuric acid to adjust the pH value to 8, filtering and drying to obtain the photocatalyst NaFeS with adsorption-photocatalysis synergistic capability 2 (1.860 g NaFeS was obtained 2 Yield greater than 96%). Synthetic NaFeS 2 Under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm), the photodegradation rate of methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min is more than 92.5 percent (adsorption-photocatalysis synergistic effect).
Example 5:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 4g of lithium-removed lithium iron phosphate powder and 15.913g of sodium sulfide nonahydrate into 400mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH value to 8, filtering and drying to obtain the photocatalyst NaFeS with adsorption-photocatalysis synergistic ability 2 (1.808 g of NaFeS was obtained 2 Yield greater than 95%). Synthetic NaFeS 2 Under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm), the photodegradation rate of methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min is more than 90.8 percent (adsorption-photocatalysis synergistic effect).
Comparative example 1:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 2g of lithium-removed lithium iron phosphate powder and 7.9565g of sodium sulfide nonahydrate into 200mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH to 12, and finding that the solution after reaction cannot be filtered, cannot be subjected to solid-liquid separation, and cannot obtain the photocatalyst NaFeS 2 After standing for 72 hours, filtration was possible, but only 0.184g of NaFeS was obtained 2 In a yield of9.7%, about 10% of the maximum yield (NaFeS) 2 The highest yield of (d) is obtained when the pH of the solution is between 6 and 8). The photodegradation rate of the synthesized product to methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm) is 75.3% (adsorption-photocatalysis synergistic effect).
Comparative example 2:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. Adding 2g of lithium-removed lithium iron phosphate powder and 7.9565g of sodium sulfide nonahydrate into 200mL of deionized water, stirring for 1 hour, adding phosphoric acid to adjust the pH to 10 (as shown in figure 2), and finding that the product after the reaction is in a gel state, cannot be subjected to solid-liquid separation, and cannot obtain the photocatalyst NaFeS 2 And still standing for 72 hours, and still failing to filter.
Comparative example 3:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. 2g of lithium-removed iron phosphate powder and 7.9565g of sodium sulfide nonahydrate were added to 200mL of deionized water, and after stirring for 1 hour, phosphoric acid was added to adjust the pH to 4 (see FIG. 2), and the solution after the reaction was found to be milky white, and 0.616g of a white solid (NaFeS) was obtained after filtration 2 Black solid), no photocatalyst NaFeS can be obtained 2 . The photodegradation rate of the synthesized white product to methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm) is 24.0%.
Comparative example 4:
adding 5g of lithium iron phosphate battery positive electrode powder and 6.035g of sodium persulfate into 500g of deionized water at room temperature, stirring for 30 minutes, filtering, and drying at 120 ℃ for 4 hours to obtain the lithium-removed lithium iron phosphate powder. 2g of lithium-removed iron phosphate powder and 7.9565g of sodium sulfide nonahydrate were added to 200mL of deionized water, and after stirring for 1 hour, phosphoric acid was added to adjust the pH to 2 (see FIG. 2), and the reaction was found to have been completedThe solution appeared milky white and after filtration a small amount of solid was obtained as white (NaFeS) 2 Black solid), about 0.249g, no photocatalyst NaFeS could be obtained 2 . The photodegradation rate of the synthesized white product to methylene blue (the initial concentration is 20mg/L, and the volume is 100mL) after 20min under the irradiation of a 300W xenon lamp (the wavelength of light is more than 420nm) is 6.1%.
Comparative example 5:
5g of waste lithium iron phosphate powder is added into an aqueous solution of ammonium persulfate, the molar ratio of the lithium iron phosphate to the sodium persulfate is 4:3 (the mass ratio is 1:1.13), the reaction is carried out for 1.5 hours, and the removal rate of lithium is 96%. Filtering and drying the lithium iron phosphate powder after removing lithium, and adding 2g of the lithium iron phosphate powder into Na 2 In an aqueous solution of S, Na 2 The molar ratio of S to the lithium iron phosphate powder (namely, iron phosphate) without lithium is 2:1 (the mass ratio is 1.03:1), the reaction is carried out for 5 hours, the pH of the solution after the reaction is measured to be 12.14 (as shown in figure 3), and the solution after the reaction cannot be filtered, cannot be subjected to solid-liquid separation, and cannot obtain the photocatalyst NaFeS 2 (as shown in FIG. 2), filtration was possible after 72 hours of standing, but only 0.190g of NaFeS was obtained 2 The yield was 10.02% and was about 10% of the maximum yield (NaFeS) 2 The highest yield was obtained when the pH of the solution was between 6 and 8), the leaching rate of phosphorus was 92.4%. The synthesized product is irradiated by a 300W xenon lamp (the wavelength of light is more than 420nm) and NaFeS is obtained after 20min 2 The photodegradation rate of methylene blue (initial concentration of 20mg/L, volume of 100mL) was 75.8% (adsorption-photocatalytic synergy).
Comparative example 6:
5g of waste lithium iron phosphate powder is added into an aqueous solution of ammonium persulfate, the molar ratio of the lithium iron phosphate to the sodium persulfate is 4:3 (the mass ratio is 1:1.13), the reaction is carried out for 1.5 hours, and the removal rate of lithium is 96%. Filtering and drying the lithium iron phosphate powder after removing lithium, and adding 2g of the lithium iron phosphate powder into Na 2 In an aqueous solution of S, Na 2 The molar ratio of S to the lithium iron phosphate powder (namely, iron phosphate) without lithium is 2.2:1 (the mass ratio is 1.14:1), the reaction is carried out for 5 hours, the pH of the solution after the reaction is measured to be 12.26 (as shown in figure 3), and the solution after the reaction cannot be filtered, cannot be subjected to solid-liquid separation, and cannot obtain the photocatalyst NaFeS 2 (as shown in FIG. 2)After standing for 72 hours, filtration was possible, but only 0.181g of NaFeS was obtained 2 The yield was 9.55%, which was about 9.5% of the highest yield (NaFeS) 2 The highest yield was obtained when the pH of the solution was at 6-8), the leaching rate of phosphorus was 93.4%. The synthesized product is irradiated by a 300W xenon lamp (the wavelength of light is more than 420nm) and NaFeS is obtained after 20min 2 The photodegradation rate of methylene blue (initial concentration of 20mg/L, volume of 100mL) was 72.7% (adsorption-photocatalytic synergy).
Comparative example 7:
5g of waste lithium iron phosphate powder is added into an aqueous solution of ammonium persulfate, the molar ratio of the lithium iron phosphate to the sodium persulfate is 4:3 (the mass ratio is 1:1.13), the reaction is carried out for 1.5 hours, and the removal rate of lithium is 96%. Filtering and drying the lithium iron phosphate powder after removing lithium, and adding 2g of the lithium iron phosphate powder into Na 2 In an aqueous solution of S, Na 2 The molar ratio of S to the lithium iron phosphate powder (namely, iron phosphate) without lithium is 4:1 (the mass ratio is 2.06:1), the reaction is carried out for 5 hours, the pH of the solution after the reaction is measured to be 12.77 (as shown in figure 3), and the solution after the reaction cannot be filtered, cannot be subjected to solid-liquid separation, and cannot obtain the photocatalyst NaFeS 2 After standing for 72 hours, filtration was possible, but only 0.175g of NaFeS was obtained 2 The yield was 9.23%, which was about 9.23% of the highest yield (NaFeS) 2 The highest yield was obtained when the pH of the solution was between 6 and 8), the leaching rate of phosphorus was 92.0%. The synthesized product is irradiated by a 300W xenon lamp (the wavelength of light is more than 420nm) and NaFeS is obtained after 20min 2 The photodegradation rate of methylene blue (initial concentration of 20mg/L, volume of 100mL) was 75.9% (adsorption-photocatalytic synergy).
TABLE 1 examples 1-5 and comparative examples 1-7
In conclusion, the photocatalyst NaFeS with adsorption-catalysis synergy is successfully synthesized by taking the waste lithium iron phosphate battery as the raw material 2 It can rapidly degrade organic dyes. Not only can greatly improve the recovery value of the waste lithium iron phosphate battery, but also can greatly improve the recovery value of the waste lithium iron phosphate batterySynthetic NaFeS 2 Also has great advantages in the aspects of wastewater treatment and organic dye removal. In addition, as shown in table 1, pH can significantly affect NaFeS 2 Synthesis of (2) and NaFeS 2 Only when the pH of the solution after the reaction is 6-8, the solid and the liquid can be quickly separated, and high yield of NaFeS is obtained 2 Although part of the NaFeS is obtained when the pH is 12-13 2 However, the yield is only 10% of the maximum yield (pH 6-8), and it is required to be left for 72 hours, which is not suitable for industrial application.
pH vs. NaFeS 2 The influence of (b) mainly includes the following aspects: (1) NaFeS 2 Has a small particle diameter (several tens to several hundreds nanometers), cannot form aggregates at a high pH, and therefore cannot separate solids from liquids by filtration or the like, and at a pH of 6 to 8, NaFeS 2 Agglomerates can be formed so that they can be separated from the liquid more easily and with maximum yield (in stoichiometric terms); (2) at pH below 6, NaFeS 2 Is unstable in an acid environment, and may further react to generate sodium sulfate, so that NaFeS cannot be synthesized 2 。
It should be noted that the above examples and test examples are only for further illustration and understanding of the technical solutions of the present invention, and are not to be construed as further limitations of the technical solutions of the present invention, and the invention which does not highlight essential features and significant advances made by those skilled in the art still belongs to the protection scope of the present invention.
Claims (6)
1. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the anode powder of the waste lithium iron phosphate battery specifically comprises the following steps:
(S1) adding the lithium iron phosphate battery positive electrode powder into the aqueous solution of the lithium extractant at room temperature, and stirring for 30 minutes to obtain lithium iron phosphate powder without lithium;
(S2) adding the lithium-removed lithium iron phosphate powder obtained in the step S1 into a sodium sulfide aqueous solution at room temperature, and stirring for 1 hour;
(S3) adjusting the pH of the suspension after the reaction in the step S2 to 6-8, filtering and drying to obtain the photocatalyst with adsorption-photocatalysis synergistic ability.
2. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the cathode powder of the waste lithium iron phosphate batteries according to claim 1, wherein the lithium extracting agent in the step (S1) is selected from any one or a mixture of potassium persulfate, ammonium persulfate and sodium persulfate.
3. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the cathode powder of the waste lithium iron phosphate batteries according to claim 1, wherein the mass ratio of the lithium extracting agent to the cathode powder of the lithium iron phosphate batteries in the step (S1) is 1:0.6-1: 1.5.
4. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the positive electrode powder of the waste lithium iron phosphate battery according to claim 1, wherein the mass ratio of the lithium iron phosphate powder subjected to lithium removal to sodium sulfide in the step (S2) is 1:1.0-1: 1.3.
5. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the cathode powder of the waste lithium iron phosphate batteries according to claim 1, wherein the mixture of any one or more of sulfuric acid, phosphoric acid, hydrochloric acid and nitric acid is used for adjusting the pH in the step (S3).
6. The method for synchronously synthesizing the visible light response photocatalyst by extracting lithium from the positive electrode powder of the waste lithium iron phosphate battery according to claim 1, wherein the main component of the photocatalyst with the adsorption-catalysis synergistic ability obtained in the step (S3) is NaFeS 2 。
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