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WO2022233340A1 - Catalyseur de combustion de cov préparé à partir de batteries au lithium-ion ternaire usagées recyclées, et son procédé de préparation - Google Patents

Catalyseur de combustion de cov préparé à partir de batteries au lithium-ion ternaire usagées recyclées, et son procédé de préparation Download PDF

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Publication number
WO2022233340A1
WO2022233340A1 PCT/CN2022/094388 CN2022094388W WO2022233340A1 WO 2022233340 A1 WO2022233340 A1 WO 2022233340A1 CN 2022094388 W CN2022094388 W CN 2022094388W WO 2022233340 A1 WO2022233340 A1 WO 2022233340A1
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vocs
solution
positive electrode
electrode material
combustion catalyst
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Ceased
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English (en)
Chinese (zh)
Inventor
郝郑平
黎刚刚
赵泽宇
张中申
程杰
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University of Chinese Academy of Sciences
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University of Chinese Academy of Sciences
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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
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • 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
    • 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
    • B01J35/615—100-500 m2/g
    • 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
    • B01J35/64—Pore diameter
    • B01J35/647—2-50 nm
    • 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
    • B01J35/64—Pore diameter
    • B01J35/651—50-500 nm
    • 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
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00—Specific waste
    • F23G2209/14—Gaseous waste or fumes
    • 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
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the invention relates to the technical field of catalyst preparation, in particular to a VOCs combustion catalyst prepared by recycling waste ternary lithium batteries and a preparation method thereof.
  • Ternary lithium-ion batteries are widely used in the consumer electronics market, electric vehicles and grid energy storage due to their advantages of high energy density, high storage capacity and good rate performance.
  • LTIBs lithium-ion batteries
  • 80GWh the total usage capacity of lithium-ion batteries
  • Aviconi Energy the total usage capacity of lithium-ion batteries
  • ternary lithium batteries will usher in a new wave of growth demand.
  • the safe recycling and green disposal of waste ternary lithium batteries is still a key link in the development of the lithium battery industry.
  • VOCs Volatile organic compounds
  • VOCs control technologies catalytic oxidation is considered to be a technology with a wide range of applications due to its advantages of high efficiency, energy saving, and low toxic by-products.
  • transition metal oxides such as Co 3 O 4 , MnO 2 , and NiO, have shown promising potential in the catalytic oxidation of VOCs due to their excellent redox properties and good mobility of active oxygen.
  • TLIBs have relatively high-priced Co and Ni elements, if the transition metal elements in TLIBs can be recycled to prepare composite oxide VOCs catalysts, then both the resource utilization of waste TLIBs and the pollution control of VOCs will be a problem. It has better environmental and economic benefits.
  • the technical problem to be solved by the present invention is: to overcome the deficiencies of the prior art, to provide a VOCs combustion catalyst prepared by recycling waste ternary lithium batteries and a preparation method thereof. Acid-soluble metal ions ⁇ filtration to remove insoluble impurities ⁇ salt precipitation ⁇ alkaline solution modification process to obtain CoMnNiO x composite oxides containing high oxygen defects, so as to achieve efficient catalytic purification of VOCs.
  • the present invention provides a method for reusing waste ternary lithium batteries to prepare a VOCs combustion catalyst, comprising the following steps:
  • step 2) adding the positive electrode material powder obtained in step 1) to the mixed solution of strong acid and hydrogen peroxide;
  • step 3 filtering the mixed solution obtained in step 2) to remove undissolved insoluble impurities to obtain the leachate of the positive electrode material;
  • step 4) adding carbonate solution to the leaching solution obtained in step 3) to promote the precipitation of transition metals Co 2+ , Mn 2+ and Ni 2+ , followed by filtering, washing, drying and calcining to obtain CoMnNiO x composite oxide;
  • step 5 The CoMnNiO x composite oxide obtained in step 4) is added to the alkaline solution, and after stirring treatment, a composite oxide catalyst with high oxygen deficiency is obtained.
  • the obtained composite oxide catalyst with high oxygen deficiency contains at least five metal elements of cobalt, manganese, nickel, aluminum and lithium. After the alkali treatment and modification in step 5), the three metal elements of cobalt, manganese and nickel account for all the metal elements. The molar proportion of the elements is at least 99%.
  • the Al and Li elements in the composite oxide are obtained by the one-step precipitation method of alkaline solution etching.
  • the defect-enhancing effect caused by the dissolution of Al and Li cations can greatly promote the catalytic oxidation activity of VOCs of the obtained composite oxides. Therefore, the composite oxides prepared by the alkaline solution post-treatment method have the advantages of good low-temperature activity, strong stability, and suitable for various types of VOCs reactions.
  • the strong acid is nitric acid, sulfuric acid or hydrofluoric acid.
  • step 2) the mixed solution is heated to 25-90°C.
  • the carbonate solution is sodium carbonate, sodium bicarbonate, ammonium carbonate, potassium carbonate, potassium bicarbonate or ammonium bicarbonate, and the concentration is 0.1-10 mol/L.
  • the calcination temperature is 200-600°C.
  • the alkali solution is sodium hydroxide or potassium hydroxide solution, and the concentration is 0.1-5mol/L.
  • the stirring temperature is 25-95°C.
  • the present invention provides a VOCs combustion catalyst prepared by the above method.
  • the VOCs combustion catalyst has a mesoporous structure of 5-80 nm and a specific surface area of 90-200 m 2 /g.
  • the "catalytic oxidation” referred to in the present invention means that VOCs are oxidized by oxygen to carbon dioxide and water under the action of a catalyst, and do not show macroscopic flame combustion.
  • the temperature corresponding to the conversion rate of the catalytic oxidation of the target VOCs is 10%, called “light-off temperature", and denoted as T 10 ; the conversion rate of the target VOCs catalytic oxidation is 90%.
  • the corresponding temperature The temperature is called “complete transformation temperature” and is recorded as T 90 .
  • the present invention has the following beneficial effects:
  • the present invention adopts waste ternary lithium electron positive electrode material to realize CoMnNiO x composite oxide by reusing the transition metal element in it after a series of treatment processes.
  • the catalyst prepared with carbonate as precipitant is more active than oxalic acid precipitant; in addition, the alkali treatment process achieves the increase of oxygen deficiency in the composite oxide, which is in typical VOCs pollutants such as acetone, ethyl acetate and propane. It exhibits excellent catalytic activity in the catalytic combustion reaction.
  • VOCs pollutants such as acetone, ethyl acetate and propane. It exhibits excellent catalytic activity in the catalytic combustion reaction.
  • the use of waste ternary lithium battery cathode materials to prepare high-performance VOCs catalysts not only realizes the recycling of waste lithium batteries, but also has excellent application prospects for VOCs catalytic combustion.
  • Fig. 1 is the XRD pattern of the positive electrode material of ternary lithium battery and the CoMnNiO composite oxide prepared by the present invention, wherein each curve represents from bottom to top: Li( CoMnNi )O ternary obtained after mechanical disassembly, calcination and decarbonization Positive electrode material; the obtained positive electrode material was added to 1 mol/L sodium hydroxide solution, treated at 80°C for 4 h, filtered, washed and dried to obtain the positive electrode material-NaOH; the intermediate product prepared in Example 1; the product prepared in Example 2 Intermediate product; final product prepared in Example 2.
  • Example 2 is a comparison of EPR results of oxygen vacancy characterization of CoMnNiO x composite oxides before and after alkali treatment of the present invention, wherein the two curves represent the intermediate product prepared in Example 2 and the final product prepared in Example 2 from bottom to top.
  • Figure 3 shows the propane catalytic oxidation activity curves of catalysts at different treatment stages, in which the positive electrode material curve represents the Li(CoMnNi)O 2 ternary positive electrode material obtained after mechanical disassembly, calcination and decarbonization; the positive electrode material-NaOH curve represents The obtained positive electrode material was added to 1 mol/L sodium hydroxide solution, treated at 80°C for 4 h, filtered, washed and dried to obtain the positive electrode material-NaOH; the CoMnNiO x -oxalic acid curve represents the intermediate product in Example 1 ; the CoMnNiO x -sodium carbonate curve represents the intermediate product in Example 2; the CoMnNiO x -sodium carbonate-NaOH curve represents the final product in Example 2.
  • the positive electrode material curve represents the Li(CoMnNi)O 2 ternary positive electrode material obtained after mechanical disassembly, calcination and decarbonization
  • Example 4 is a graph showing the activity curves of CoMnNiO x composite oxides obtained by different precipitants for the catalytic oxidation of acetone, wherein the two curves from left to right represent the intermediate product prepared in Example 2 and the intermediate product prepared in Example 1, respectively.
  • Figure 5 shows the activity curves of the obtained CoMnNiO x composite oxide for ethyl acetate catalytic oxidation before and after alkali treatment, wherein the two curves from left to right represent the final product prepared in Example 2 and the intermediate product prepared in Example 2 respectively.
  • Figure 6 is the nitrogen adsorption and desorption curve of the catalyst, wherein the CoMnNiO x -oxalic acid curve represents the intermediate product in Example 1; the CoMnNiO x -sodium carbonate curve represents the intermediate product in Example 2; CoMnNiO x -sodium carbonate -The NaOH curve represents the final product in Example 2.
  • Fig. 7 is the pore size distribution diagram of the catalyst, wherein the CoMnNiO x -oxalic acid curve represents the intermediate product in Example 1; the CoMnNiO x -sodium carbonate curve represents the intermediate product in Example 2; CoMnNiO x -sodium carbonate-NaOH The curve represents the final product in Example 2.
  • FIG. 8 is a schematic structural diagram of a small-scale fixed-bed continuous flow reaction evaluation device of the present invention.
  • VOCs gas and oxygen entered the gas mixing device respectively, and then entered the quartz tube of the reaction furnace (model SK2-1-10K) after mixing. In the process, it contacts and reacts with the catalyst in the quartz tube, and the reacted gas enters the gas chromatograph for detection to obtain the catalytic oxidation conversion rate of VOCs gas.
  • the 40-60 mesh catalyst obtained by sieving 0.1g of tablets was put into a quartz tube (diameter 6mm), the reaction temperature was controlled by a temperature-programmed reaction furnace, and the VOCs gas was selected from three gases of propane, acetone or ethyl acetate.
  • the concentrations were 2000 ppm, 1000 ppm and 1000 ppm, respectively, and the oxygen concentration was 20%.
  • the space velocity was 18000 g ⁇ ml ⁇ h ⁇ 1 .
  • the waste ternary lithium battery is completely discharged, and the positive electrode material is separated and pulverized through shearing, screening and mechanical stripping treatment; the positive electrode material powder is added to the mixed solution of strong acid (nitric acid, sulfuric acid or hydrofluoric acid) and hydrogen peroxide and heated to 25-90° C. to promote the dissolution of metal ions in the positive electrode material; filter the mixed solution to remove undissolved insoluble impurities (conductive graphite, etc.) to obtain the leaching solution of the positive electrode material.
  • strong acid nitric acid, sulfuric acid or hydrofluoric acid
  • hydrogen peroxide hydrogen peroxide
  • a 5 mol/L oxalic acid solution was continuously added dropwise to 150 mL of the positive electrode material leaching solution until flocculent precipitation occurred. Stir vigorously for 30 min, and then stand still for aging for 12 h. The obtained precipitate is filtered with suction, washed until neutral, and dried at 100°C overnight. Finally, the obtained powder was calcined in a muffle furnace at 300° C. for 3 hours in an air atmosphere to obtain a CoMnNiO x composite metal oxide.
  • CoMnNiO x composite metal oxide was added to a 1 mol/L sodium hydroxide solution, stirred at 80° C. for 4 hours, filtered, washed and dried to obtain an oxygen-deficient composite oxide, denoted as catalyst A.
  • Catalyst A was used in the catalytic activity test of propane, acetone and ethyl acetate, respectively.
  • the preparation method of the leaching solution of the positive electrode material is the same as that in Example 1.
  • CoMnNiO x composite metal oxide was added to a 1 mol/L sodium hydroxide solution, stirred at 50°C for 8 hours, filtered, washed and dried to obtain an oxygen-deficient composite oxide, denoted as catalyst B.
  • Catalyst B was used in the catalytic activity test of propane, acetone and ethyl acetate, respectively.
  • the preparation method of the leaching solution of the positive electrode material is the same as that in Example 1.
  • a 5 mol/L ammonium carbonate solution was continuously added dropwise to 150 mL of the positive electrode material leaching solution until the pH rose to 10. Stir vigorously for 30 min, and then stand still for aging for 12 h. The obtained precipitate is filtered with suction, washed until neutral, and dried at 100°C overnight. Finally, the obtained powder was calcined in a muffle furnace at 300° C. for 3 hours in an air atmosphere to obtain a CoMnNiO x composite metal oxide.
  • CoMnNiOx composite metal oxide was added to a 1 mol/L potassium hydroxide solution, stirred at 80°C for 4 hours, filtered, washed and dried to obtain an oxygen-deficient composite oxide, denoted as catalyst C.
  • Catalyst C was used in the catalytic activity test of propane, acetone and ethyl acetate, respectively.
  • the preparation method of the leaching solution of the positive electrode material is the same as that in Example 1.
  • a 5 mol/L oxalic acid solution was continuously added dropwise to 150 mL of the positive electrode material leaching solution until flocculent precipitation occurred. Stir vigorously for 30 min, and then stand still for aging for 12 h. The obtained precipitate is filtered with suction, washed until neutral, and dried at 100°C overnight. Finally, the obtained powder was calcined in a muffle furnace at 300° C. for 3 hours in an air atmosphere to obtain a CoMnNiO x composite metal oxide, which was denoted as catalyst R1.
  • the catalyst R1 was used in the catalytic activity test of propane, acetone and ethyl acetate, respectively.
  • the preparation method of the leaching solution of the positive electrode material is the same as that in Example 1.
  • Example 2 the CoMnNiO x composite oxide prepared by using sodium carbonate as a precipitant has a higher diffraction peak than the CoMnNiO x composite oxide prepared by using oxalic acid as a precipitant in Example 1. It can be explained that the crystallinity of CoMnNiO x -sodium carbonate prepared in Example 2 is lower, and it contains more oxygen vacancy defects. Similarly, CoMnNiO x -sodium carbonate-NaOH after alkali treatment also has broad diffraction peaks, indicating that there are abundant oxygen vacancy defects.
  • Figure 4 further confirms that the catalyst prepared using carbonate as precipitant is more active than oxalic acid precipitant.
  • Figure 5 also further confirms that the alkali treatment can further improve the activity of the catalyst.
  • Figure 6 shows that the specific surface area of the VOCs combustion catalyst is 90-200 m 2 /g
  • Figure 7 shows that the catalyst has a mesoporous structure of 5-80 nm.

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Abstract

La présente invention divulgue un catalyseur de combustion de COV préparé à partir de batteries au lithium-ion ternaire usagées recyclées, et son procédé de préparation, qui appartiennent au domaine technique de la préparation de catalyseurs. Un oxyde composite de CoMnNiOx contenant des défauts d'oxygène élevés est obtenu par soumission de batteries au lithium-ion ternaire usagées au processus suivant : décharge → désassemblage → exfoliation mécanique → dissolution d'acide d'ions métalliques → filtration pour éliminer les impuretés insolubles → formation de sel et précipitation → modification de solution alcaline, de telle sorte qu'une purification catalytique efficace des COV est obtenue.
PCT/CN2022/094388 2021-09-16 2022-05-23 Catalyseur de combustion de cov préparé à partir de batteries au lithium-ion ternaire usagées recyclées, et son procédé de préparation Ceased WO2022233340A1 (fr)

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CN202111086649.6A CN113713828B (zh) 2021-09-16 2021-09-16 回用废旧三元锂电池制备的VOCs燃烧催化剂及其制备方法
CN202111086649.6 2021-09-16

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CN115970738A (zh) * 2022-12-28 2023-04-18 上海第二工业大学 基于废旧锂离子电池正极材料的分子筛基催化剂在微波催化氧化VOCs中的应用
CN117548116A (zh) * 2023-11-15 2024-02-13 中国科学院山西煤炭化学研究所 一种催化湿式氧化四溴双酚a废水的催化剂及其制备方法和应用
CN117548097A (zh) * 2023-09-26 2024-02-13 中山大学 一种利用废旧锰酸锂电池制备整体式催化剂及其制备方法与应用
CN117654534A (zh) * 2023-11-01 2024-03-08 华南理工大学 一种用于去除短链烃的复合过渡金属氧化物催化剂及其制备方法与应用

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CN113713828B (zh) * 2021-09-16 2023-08-08 中国科学院大学 回用废旧三元锂电池制备的VOCs燃烧催化剂及其制备方法
CN114832845B (zh) * 2022-05-23 2024-05-10 濮阳天地人环保科技股份有限公司 一种利用回收锂电池材料制备的复合催化剂及其制备方法
CN115716660A (zh) * 2022-10-14 2023-02-28 东南大学 一种复合三元金属氧化物载氧体材料及其制备方法和用途
CN117531515A (zh) * 2023-09-26 2024-02-09 中山大学 一种利用废旧钴酸锂电池制备掺杂-多孔型-钴基纳米材料的方法与应用

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