CN112708768B - Pretreatment method of high-chromium waste material of solid oxide fuel cell - Google Patents
Pretreatment method of high-chromium waste material of solid oxide fuel cell Download PDFInfo
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/008—Disposal or recycling of fuel cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- 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
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Abstract
The invention relates to a pretreatment method of high-chromium waste materials of a solid oxide fuel cell, which comprises the following steps: 1) Crushing and grinding: crushing and grinding high-chromium waste materials of the solid oxide fuel cell; 2) Acid leaching: adding acid into the ground high-chromium waste of the solid oxide fuel cell according to a certain solid-to-liquid ratio for leaching, and filtering to obtain a pickling solution and a zirconium-rich scandium filter cake; 3) Washing: removing residual pickle liquor on the surface of the zirconium-rich scandium filter cake after pickling by using water; 4) Drying and grinding: removing residual moisture on the surface of the washed zirconium-rich scandium filter cake, and grinding by a grinder to obtain zirconium-rich scandium powder; 5) And (3) neutralization precipitation: adding alkali into the pickle liquor for neutralization and recovery. The process has the advantages of simple and safe flow, small workshop production risk, large batch processing capacity and little environmental pollution, and can realize primary separation of valuable metals in the high-chromium waste of the solid oxide fuel cell.
Description
Technical Field
The invention relates to the field of resource recovery, in particular to a pretreatment method of high-chromium waste materials of a solid oxide fuel cell.
Background
The solid oxide fuel cell (Solid Oxide Fuel Cell, SOFC for short) belongs to a third-generation fuel cell, is an important application of an advanced ceramic material, can directly convert chemical energy in fuel into electric energy through high-temperature electrochemical reaction, has the advantages of high power generation efficiency, quietness, noiselessness, low emission, wide fuel source and the like, is an effective way for realizing clean utilization of fossil energy in China, and has wide application prospect. Commercial SOFC power generation systems have been developed in developed countries, but the SOFC industry in China has a certain gap compared with the SOFC power generation systems. SOFCs are widely considered as a fuel cell which is widely used as proton exchange membrane fuel cells in the future, and in order to realize recycling of resources, it is important to recycle the used solid oxide fuel cell waste, so that research and development of a simple and rapid method for treating the solid oxide fuel cell waste is of great significance to scandium oxide use and development of the solid oxide fuel cell field.
A solid oxide fuel cell system may include one or more fuel cell stacks that generate electricity. Each stack may include fuel cells disposed between fuel cell interconnects. The fuel cell may include a solid oxide electrolyte disposed between the anode and cathode electrodes. At the end of the life cycle of the stack, each stack may be singulated to recover metal interconnects, such as ferrochrome interconnects, as described in U.S. published patent application No. 2017/024114 A1. In this process, fuel cell waste is generated as the solid fuel cells are separated from the interconnect. The solid oxide fuel cell may include scandia-stabilized zirconia electrolytes, such as scandia and ceria-stabilized zirconia electrolytes. The electrolyte may comprise an anode electrode comprising a cermet (e.g., a cermet comprising nickel and doped ceria) and a cathode electrode comprising a perovskite material (e.g., lanthanum strontium manganate). The solid oxide fuel cell is configured to withstand high temperatures. As such, the fuel cell waste may include various precious materials. For example, the fuel cell waste material may contain about 10% sc 2 O 3 About 10% La 2 O 3 About 5% CeO 2 About 70% ZrO 2 And other materials remaining such as nickel, strontium, and manganese. Scandium recovery is particularly important because of its high value.
In the current recovery process of solid oxide fuel cell waste, concentrated sulfuric acid digestion, water immersion, impurity removal, extraction, oxalic acid precipitation and calcination are mainly adopted to recover scandium, the method is not applicable to waste with high chromium content, the reaction is severe in the digestion process of the waste with high chromium content, and the workshop production is easy to overflow due to the digestion processHigh temperature, and the metallic chromium is easy to react with the concentrated sulfuric acid to generate SO 2 This results in serious safety hazards in the treatment of high-chromium waste, and the reduction of productivity affects the production efficiency of workshops.
Therefore, there is a need to design a pretreatment method for high chromium waste materials of solid oxide fuel cells to solve the above-mentioned technical problems.
Disclosure of Invention
The invention aims to provide a solid oxide fuel cell high-chromium waste pretreatment method which has the advantages of simple process flow, high recovery rate, large batch processing capacity, low cost and safety.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a method for pretreating high chromium waste materials of a solid oxide fuel cell, the method comprising the steps of:
s1, crushing and grinding: crushing and grinding high-chromium waste materials of the solid oxide fuel cell;
s2 acid leaching: adding acid into the ground high-chromium waste of the solid oxide fuel cell according to a certain solid-to-liquid ratio for leaching, and filtering to obtain a pickling solution and a zirconium-rich scandium filter cake;
s3, washing: removing residual pickle liquor on the surface of the zirconium-rich scandium filter cake after pickling by using water;
s4, drying and grinding: removing residual moisture on the surface of the washed zirconium-rich scandium filter cake, and grinding by a grinder to obtain zirconium-rich scandium powder;
s5, neutralization precipitation: adding alkali into the pickle liquor for neutralization and recovery.
As a further improvement of the invention, the mass fraction of the metal chromium in the high-chromium waste material of the solid oxide fuel cell is 2% -15%.
As a further improvement of the invention, the solid oxide fuel cell high chromium waste is leached by acid leaching, and the leaching process is carried out according to a certain proportion, so that the solid oxide fuel cell high chromium waste: the solid-liquid ratio of the acid is 1:10-15. The solid-liquid ratio is too low, the leaching rate of chromium in the waste is low, the pretreatment effect is poor, and H can be generated by the reaction of metal chromium and dilute acid 2 The reaction is severe and the tank is easy to overflow, so that potential safety hazards exist in the pretreatment process of the high-chromium waste; too high a liquid-to-solid ratio increaseScandium loss is avoided, and meanwhile, the reagent consumption is large and the wastewater amount is large.
As a further improvement of the invention, the acid of the leaching process comprises one of sulfuric acid, hydrochloric acid, nitric acid.
As a further improvement of the invention, the acid concentration is controlled to be 2-6 mol/L. Too low acid concentration has low leaching rate of metal chromium in the waste, slow reaction rate and poor pretreatment effect; too high an acid concentration increases scandium losses and the high acid system is prone to corrosion in the equipment.
As a further improvement of the invention, the addition amount of the acid is 1-2 times of the stoichiometric amount.
As a further improvement of the invention, the reaction temperature of the acid leaching is controlled to be 50-100 ℃. The leaching rate of the metal chromium in the waste is low due to the too low temperature, the reaction rate is slow, and the pretreatment effect is poor; the loss of scandium is increased when the temperature is too high, the high-temperature system has high requirements on equipment, and H is generated by the reaction of metal chromium and dilute acid 2 The high-temperature reaction is severe and easy to overflow, and potential safety hazards exist.
As a further improvement of the invention, the reaction time of the acid leaching is controlled to be 4-12 hours. The reaction time is too short, so that the metal chromium reaction is incomplete, and the pretreatment effect of waste materials is poor; too long a reaction time increases scandium loss and increases production costs.
As a further improvement of the invention, the valuable metals in the high chromium waste of the solid oxide fuel cell include scandium, nickel, manganese, zirconium.
Compared with the prior art, firstly, the Mn/Ni/Cr in the high-chromium waste material of the solid oxide fuel cell is selectively leached by acid leaching, SO that the phenomenon that the reaction is severe in the digestion process in the traditional process and the production of a workshop is easy to cause the overflow of the workshop is effectively avoided, and because the temperature of the digestion process is high, the metallic chromium is easy to react with concentrated sulfuric acid to generate SO 2 This results in serious safety hazards in the treatment of high-chromium waste, and the reduction of productivity affects the production efficiency of workshops. Secondly, in the pretreatment process, the primary separation of most impurities and zirconium/scandium is realized, and the subsequent purification of zirconium scandium is simplified. Third, solid oxide fuelScandium content in the pickle liquor after the pretreatment of the battery high-chromium waste is less than 100ppm, scandium loss is less than 1%, and scandium loss is effectively controlled. The whole process is simple to operate, the equipment investment is low, the efficiency is high, the produced zirconium-rich scandium powder is subjected to the next purification process, the safety risk of concentrated sulfuric acid digestion is reduced, and the treatment efficiency of the concentrated sulfuric acid digestion is improved.
Detailed Description
The invention provides a pretreatment method of high-chromium waste materials of a solid oxide fuel cell, which comprises the following steps:
s1, crushing and grinding: crushing and grinding high-chromium waste materials of the solid oxide fuel cell;
s2 acid leaching: adding acid into the ground high-chromium waste of the solid oxide fuel cell according to a certain solid-to-liquid ratio for leaching, and filtering to obtain a pickling solution and a zirconium-rich scandium filter cake;
s3, washing: removing residual pickle liquor on the surface of the zirconium-rich scandium filter cake after pickling by using water;
s4, drying and grinding: removing residual moisture on the surface of the washed zirconium-rich scandium filter cake, and grinding by a grinder to obtain zirconium-rich scandium powder;
s5, neutralization precipitation: adding alkali into the pickle liquor for neutralization and recovery.
Example 1.
A method for pretreating high-chromium waste materials of solid oxide fuel cells, comprising the following steps: crushing and grinding solid oxide fuel cell waste with 13% chromium, and then mixing according to a solid-to-liquid ratio of 1:10 adding 400g/L sulfuric acid, heating to 85 ℃, and reacting for 4 hours at a temperature of between the temperature of the mixture to obtain a zirconium-rich scandium filter cake and an acid leaching filter cake, wherein Sc in the filtrate is less than 100ppm; tap water is used according to the solid-liquid ratio of 1: and 5, removing residual acid liquor and impurities on the surface of the zirconium-rich scandium filter cake obtained after acid leaching. And (3) drying the zirconium-rich scandium filter cake after water washing, removing residual moisture on the surface, and grinding by a grinder to obtain zirconium-rich scandium powder, wherein the removal rate of Mn/Ni/Cr in the zirconium-rich scandium powder can reach 99%, the loss of scandium is less than 2%, and the mass is reduced by 35%. Adding alkali liquor into the acid leaching filtrate for neutralization precipitation, heating to 65 ℃, adjusting the pH to 9, carrying out heat preservation reaction for 3 hours, filtering, and neutralizing to recover Mn, ni and Cr hydroxide precipitates.
Example 2.
A method for pretreating high-chromium waste materials of solid oxide fuel cells, comprising the following steps: crushing and grinding solid oxide fuel cell waste with 13% chromium, and then mixing according to a solid-to-liquid ratio of 1:10 adding 6mol/L hydrochloric acid, heating to 78 ℃, and reacting for 4 hours at a temperature maintaining condition to obtain a zirconium-rich scandium filter cake and an acid leaching filter cake, wherein Sc in the filtrate is less than 100ppm; tap water is used according to the solid-liquid ratio of 1: and 4, removing residual acid liquor and impurities on the surface of the zirconium-rich scandium filter cake obtained after acid leaching. And (3) drying the zirconium-rich scandium filter cake after water washing, removing residual moisture on the surface, and grinding by a grinder to obtain zirconium-rich scandium powder, wherein the removal rate of Mn/Ni/Cr in the zirconium-rich scandium powder can reach 99%, the loss of scandium is less than 2%, and the mass is reduced by 32%. Adding alkali liquor into the acid leaching filtrate for neutralization precipitation, heating to 55 ℃, adjusting the pH to 9.5, carrying out heat preservation reaction for 3 hours, filtering, and neutralizing to recover Mn, ni and Cr hydroxide precipitates.
Example 3.
A method for pretreating high-chromium waste materials of solid oxide fuel cells, comprising the following steps: crushing solid oxide fuel cell waste containing 5% of chromium, and then mixing the crushed solid oxide fuel cell waste with the solid-to-liquid ratio of 1:8, adding 250g/L sulfuric acid, heating to 80 ℃, and reacting for 10 hours at a temperature maintaining condition to obtain a zirconium-rich scandium filter cake and an acid leaching filter cake, wherein Sc in the filtrate is less than 50ppm; tap water is used according to the solid-liquid ratio of 1: and 5, removing residual acid liquor and impurities on the surface of the zirconium-rich scandium filter cake obtained after acid leaching. And (3) drying the zirconium-rich scandium filter cake after water washing, removing residual moisture on the surface, and grinding by a grinder to obtain 200-300 mesh powder, wherein the Mn/Ni/Cr removal rate in the zirconium-rich scandium powder can reach 99%, the scandium loss is less than 1%, and the mass is reduced by 16%. Adding alkali liquor into the acid leaching filtrate for neutralization precipitation, heating to 60 ℃, adjusting the pH to 8.5, carrying out heat preservation reaction for 2.5 hours, filtering, and neutralizing to recover Mn, ni and Cr hydroxide precipitates.
The invention has the beneficial effects that: the method is used for preprocessing the high-chromium waste of the solid oxide fuel cell, can efficiently and quickly process the high-chromium solid oxide fuel cell waste, has low loss rate of scandium in the process, and performs primary separation on scandium and other metals, thereby having important significance for scandium recovery. The method also reduces the risk of scandium recovery process production of the solid oxide fuel cell waste and solves the problem of difficult wastewater treatment. The process has the advantages of simple technical flow, high recovery rate, large batch processing capacity, low cost, safety and the like.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (1)
1. A pretreatment method of high-chromium waste materials of solid oxide fuel cells is characterized in that: the method comprises the following steps:
s1, crushing and grinding: crushing and grinding high-chromium waste materials of the solid oxide fuel cell, wherein the mass fraction of metal chromium in the high-chromium waste materials of the solid oxide fuel cell is 1-15%, and valuable metals in the high-chromium waste materials of the solid oxide fuel cell comprise scandium, nickel, manganese and zirconium;
s2 acid leaching: leaching the ground high-chromium waste of the solid oxide fuel cell with acid according to the solid-to-liquid ratio of 1:10-15, wherein the acid comprises sulfuric acid, hydrochloric acid or nitric acid, the concentration of the acid is controlled to be 2-6 mol/L, the reaction temperature of the acid leaching is controlled to be 50-100 ℃, the reaction time of the acid leaching is controlled to be 4-12 h, and the acid leaching solution and the zirconium-enriched scandium filter cake are obtained through filtration;
s3, washing: removing residual pickle liquor on the surface of the zirconium-rich scandium filter cake after pickling by using water;
s4, drying and grinding: removing residual moisture on the surface of the washed zirconium-rich scandium filter cake, and grinding by a grinder to obtain zirconium-rich scandium powder;
s5, neutralization precipitation: adding alkali liquor into the pickle liquor to adjust the pH value to 8.5-9.5, heating to 55-65 ℃ to perform neutralization precipitation, reacting for 2.5-3 hours while preserving heat, filtering, and recovering Mn, ni and Cr hydroxide precipitates.
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Effective date of registration: 20230927 Address after: 221100 No.1, Xianxian South Road, Tongchuang Road West, High tech Industrial Development Zone, Xuzhou City, Jiangsu Province Patentee after: Pioneer Electronic Technology Co.,Ltd. Address before: 511500 Heyun Town Industrial Zone, Qingxin District, Qingyuan City, Guangdong Province (beside Yuba highway) Patentee before: FIRST RARE MATERIALS Co.,Ltd. |