CN112342389A - Method for recovering valuable metal from waste chemical catalyst - Google Patents
Method for recovering valuable metal from waste chemical catalyst Download PDFInfo
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- CN112342389A CN112342389A CN202011142080.6A CN202011142080A CN112342389A CN 112342389 A CN112342389 A CN 112342389A CN 202011142080 A CN202011142080 A CN 202011142080A CN 112342389 A CN112342389 A CN 112342389A
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- molybdenum
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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
- 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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- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- 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
- C22B23/043—Sulfurated acids or salts thereof
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
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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
- C22B34/34—Obtaining molybdenum
- C22B34/345—Obtaining molybdenum from spent catalysts
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for recovering valuable metals from waste chemical catalysts, which comprises the following steps: (1) wet grinding the waste chemical catalyst; (2) acid leaching the slurry after wet grinding to obtain filter residue and leachate containing nickel, molybdenum and vanadium; (3) extracting vanadium from the leachate containing nickel, molybdenum and vanadium obtained in the step (2) to obtain a strip liquor and a vanadium raffinate; (4) extracting molybdenum from the vanadium raffinate obtained in the step (3) to obtain molybdenum raffinate and strip liquor; (5) and (4) adding sodium carbonate or sodium hydroxide into the molybdenum raffinate obtained in the step (4), adjusting the pH value to 7-8, filtering after the reaction is finished, evaporating and crystallizing to obtain a crude nickel sulfate product, and evaporating the crystallized filtrate to obtain an industrial sodium sulfate product. The process method of the invention effectively improves the recovery rate of the metal nickel vanadium molybdenum by adopting fine grinding and two-stage leaching, the recovery rate of vanadium and molybdenum is more than 97%, and the recovery rate of nickel is more than 99%.
Description
Technical Field
The invention belongs to the field of treatment of waste catalysts, and particularly relates to a method for treating a waste catalyst in the chemical industry by adopting a wet process.
Background
The technology for treating the waste catalyst in the chemical industry comprises two methods, namely a fire method and a wet method, and three processes, namely a physical separation method, a chemical regeneration method and a resource disposal method. The waste FCC catalyst is more completely, economically and effectively recycled and treated, and the difficulty of effectively treating the industrial production process and the treatment path of the waste catalyst is caused.
Publication No. CN110386616A "a method for producing aluminum sulfate by treating FCC waste catalyst" adopts a wet process to treat FCC, and adds water, FCC waste catalyst and sulfuric acid solution into a reaction kettle, and then stirs and reacts to obtain a reaction mixture containing aluminum sulfate and nickel sulfate. The publication No. CN109821859A 'treatment method of waste FCC catalyst', realizes the reconstruction of the structure of the waste FCC catalyst by a hydrothermal method, thereby reducing the leaching toxicity of nickel element and vanadium element. Publication No. CN106552680A "a method for demetallizing and reactivating FCC spent catalyst" is to contact the FCC spent catalyst with small molecular substances containing halogen to perform demetallization reaction at medium temperature to obtain the reaction product of the FCC spent catalyst.
The above methods for treating the spent FCC catalyst cannot sufficiently recover valuable metals contained in the spent FCC catalyst.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background technology and provide a method for treating the waste catalyst in the chemical industry by adopting a wet process.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for recovering valuable metals from waste chemical catalysts comprises the following steps:
(1) wet grinding the waste chemical catalyst;
(2) acid leaching the slurry after wet grinding to obtain filter residue and leachate containing nickel, molybdenum and vanadium;
(3) extracting vanadium from the leachate containing nickel, molybdenum and vanadium obtained in the step (2) to obtain a strip liquor and a vanadium raffinate;
(4) extracting molybdenum from the vanadium raffinate obtained in the step (3) to obtain molybdenum raffinate and strip liquor;
(5) and (4) adding sodium carbonate or sodium hydroxide into the molybdenum raffinate obtained in the step (4), adjusting the pH value to 7-8, filtering after the reaction is finished, evaporating and crystallizing to obtain a crude nickel sulfate product, and evaporating the crystallized filtrate to obtain an industrial sodium sulfate product.
Preferably, in the step (1), the waste chemical industry catalyst is a filter cake of filter residue after FCC incineration, and contains nickel, vanadium, molybdenum, sulfur and ash.
The above method, preferably, in the step (1), the wet milling is carried out in an ultrafine mill, and the ratio of liquid to solid mass is 1.5 to 3: 1, the particle size of the material after wet grinding is not higher than 320 meshes.
In the method, preferably, the filter residue obtained in the step (2) is subjected to low-acid leaching, and 1-5g/l of hydrogen peroxide is added as an oxidant to obtain a filtrate and filter residue; conditions of low acid leaching: acidity of 15-25 g/l, liquid-solid mass ratio of 1.5-2.5: 1. the temperature is 80-90 ℃ and the time is 4-6 hours; and (3) returning the filtrate to the acid leaching process in the step (2), washing filter residues, piling the filter residues for producing building materials such as cement or environment-friendly bricks, and returning the filter residue washing liquor to the step (1).
In the above method, preferably, in the step (2), the acid leaching conditions are: acidity of 120-: 1, the temperature is 80-90 ℃, and the time is 2-3 hours.
In the method, preferably, in the step (3), the process conditions for extracting vanadium include: pH value is 1.5-3, extracting agent is composed of 20% P204, 10% TBP and 70% sulfonated kerosene, compared with O/A2, extracting time is 5-6min, diluting agent is No. 260 sulfonated kerosene, organic phase is back-extracted by 1.5mol/L sulfuric acid, the back-extraction liquid containing vanadium is directly precipitated to obtain V2O5And (5) producing the product.
In the method, preferably, in the step (4), the process conditions for extracting molybdenum include: the method adopts a P204 and N235 combined extracting agent, wherein the P204 accounts for 20-50%, the N235 accounts for 80-50%, the diluent is 260# sulfonated kerosene, the initial pH is 3, the final pH is 5, and the organic phase is subjected to back extraction of molybdenum by using 4mol/l ammonia water.
In the above method, preferably, in the step (4), the strip liquor is purified to remove impurities, then ammonium bicarbonate is added, and evaporation and crystallization are carried out to produce ammonium molybdate crystals.
Preferably, in the step (5), the crude nickel sulfate is purified to produce refined nickel sulfate or battery-grade nickel sulfate.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts two-stage extraction process, and metal is separated in a step manner, so that effective separation of vanadium, molybdenum and nickel is realized.
(2) The process method of the invention effectively improves the recovery rate of the metal nickel vanadium molybdenum by adopting fine grinding, two-stage leaching and adding the oxidant, wherein the recovery rate of vanadium and molybdenum is more than 97 percent, and the recovery rate of nickel is more than 99 percent.
(3) The chemical waste catalyst is treated by a wet process, so that dust is reduced, gas in the reaction process can be directly pumped into an absorption tower for absorption treatment, liquid generated in the treatment process can be returned to the process for recycling, and no process wastewater is generated.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention discloses a method for recovering valuable metals from waste chemical catalysts, which has a process flow diagram shown in figure 1 and comprises the following steps:
(1) fine grinding:
mixing the washing liquid of the leaching filter press with the filter residue filter cake after the incineration of the waste catalyst in the chemical industry, and carrying out wet-type fine grinding in a superfine grinding machine, wherein the liquid-solid mass ratio of the fine grinding is controlled to be 2.5: 1, enabling the granularity of the material to reach-320 meshes;
(2) leaching:
leaching the filter cake of the filter residue obtained in the step (1) after fine grinding by using sulfuric acid (acid leaching condition: acidity 130g/l, liquid-solid mass ratio 2.5: 1, temperature 85 ℃, time 2.5 hours), and performing filter pressing treatment on the leached ore pulp to obtain filter residue and leaching solution; the leachate enters the following step (3); circularly collected flue gas generated in the acid leaching process is discharged into a washing and collecting tower through a draught fan, absorbed by alkali liquor and finally discharged through a chimney;
carrying out low-acid leaching on filter residues by using sulfuric acid (the conditions of low-acid leaching are that the acidity is 18g/L, the liquid-solid mass ratio is 2.0: 1, the temperature is 85 ℃, and the time is 5 hours), adding 2g/L hydrogen peroxide while carrying out low-acid leaching, carrying out filter pressing treatment, washing the filter residues for producing building materials, returning washing water to the step (1) for preparing a solution, and returning the filtrate to the sulfuric acid leaching process;
(3) vanadium extraction procedure:
extracting the leachate obtained in the step (2), and separating vanadium: diluting agent is 260# sulfonated kerosene, pH value is 1.5-3, extracting agent is composed of 20% P204+ 10% TBP + 70% sulfonated kerosene, compared with O/A2, the extraction time is 5min, 1.5mol/L sulfuric acid is used for back extraction for 6min, the back extraction liquor is directly precipitated with vanadium, and V is prepared2O5Product (alum tablet);
(4) molybdenum extraction:
sending the vanadium raffinate obtained in the step (3) to a molybdenum extraction process: adopting a P204 and N235 combined extracting agent (P204 accounts for 40 percent and N235 accounts for 60 percent), using 260# sulfonated kerosene as a diluent, extracting molybdenum with initial pH of 3 and end pH of 5, back-extracting molybdenum from an organic phase by using 4mol/L ammonia water, adding ammonium bicarbonate into the obtained back-extraction solution after purifying and removing impurities, and evaporating and crystallizing to produce ammonium molybdate crystals; sending raffinate after molybdenum extraction to a nickel precipitation process;
(5) a nickel deposition process:
and (3) introducing the raffinate obtained in the step (4) into a nickel precipitation process: adding caustic soda flakes into raffinate after molybdenum extraction, adjusting the pH value to 7-8, precipitating nickel, filtering, evaporating and crystallizing to obtain a crude nickel sulfate product, and evaporating saline water after nickel precipitation to obtain industrial sodium sulfate. The crude nickel sulfate can be purified to remove impurities to produce refined nickel sulfate or battery-grade nickel sulfate. According to the metal content in the product, the recovery rate of vanadium is 97.5%, the recovery rate of molybdenum is 97.2%, and the recovery rate of nickel is 99.3%.
Example 2
The invention discloses a method for recovering valuable metals from waste chemical catalysts, which has a process flow diagram shown in figure 1 and comprises the following steps:
(1) fine grinding:
mixing the washing liquid of the leaching filter press with the filter residue filter cake after the incineration of the waste catalyst in the chemical industry, and carrying out wet-type fine grinding in a superfine grinding machine, wherein the liquid-solid mass ratio of the fine grinding is controlled to be 2: 1, enabling the granularity of the material to reach-320 meshes;
(2) leaching:
leaching the filter cake of the filter residue obtained in the step (1) after fine grinding by using sulfuric acid (acid leaching condition: acidity 140g/l, liquid-solid mass ratio is 2.5: 1, temperature is 90 ℃, time is 2.5 hours), and performing filter pressing treatment on the leached ore pulp to obtain filter residue and leaching solution; the leachate enters the following step (3); circularly collected flue gas generated in the acid leaching process is discharged into a washing and collecting tower through a draught fan, absorbed by alkali liquor and finally discharged through a chimney;
carrying out low-acid leaching on filter residues by using sulfuric acid (the conditions of low-acid leaching are that the acidity is 20g/L, the liquid-solid ratio is 2.5: 1, the temperature is 890 ℃, and the time is 6 hours), adding 2g/L hydrogen peroxide while carrying out low-acid leaching, carrying out filter pressing treatment, washing the filter residues for producing building materials, returning washing water to the step (1) for preparing a solution, and returning the filtrate to the sulfuric acid leaching process;
(3) vanadium extraction procedure:
extracting the leachate obtained in the step (2), and separating vanadium: diluting agent is 260# sulfonated kerosene, pH value is 1.5-3, extracting agent is composed of 20% P204+ 10% TBP + 70% sulfonated kerosene, compared with O/A2, the extraction time is 5min, 1.5mol/L sulfuric acid is used for back extraction for 6min, the back extraction liquor is directly precipitated with vanadium, and V is prepared2O5Product (alum tablet);
(4) molybdenum extraction:
sending the vanadium raffinate obtained in the step (3) to a molybdenum extraction process: adopting a P204 and N235 combined extracting agent (P204 accounts for 35 percent and N235 accounts for 65 percent), using 260# sulfonated kerosene as a diluent, extracting molybdenum with initial pH of 3 and end pH of 5, back-extracting molybdenum from an organic phase by using 4mol/l ammonia water, adding ammonium bicarbonate into the obtained back-extraction solution after purifying and removing impurities, evaporating and crystallizing to produce ammonium molybdate crystals; sending raffinate after molybdenum extraction to a nickel precipitation process;
(5) a nickel deposition process:
and (3) introducing the raffinate obtained in the step (4) into a nickel precipitation process: adding caustic soda flakes into raffinate after molybdenum extraction, adjusting the pH value to 7-8, precipitating nickel, filtering, evaporating and crystallizing to obtain a crude nickel sulfate product, and evaporating salt water after nickel precipitation to obtain industrial sodium sulfate. The crude nickel sulfate can be purified to remove impurities to produce refined nickel sulfate or battery-grade nickel sulfate. According to the metal content in the product, the recovery rate of vanadium is 97.2%, the recovery rate of molybdenum is 97.5%, and the recovery rate of nickel is 99.4%.
Claims (9)
1. A method for recovering valuable metals from waste chemical catalysts is characterized by comprising the following steps:
(1) wet grinding the waste chemical catalyst;
(2) acid leaching the slurry after wet grinding to obtain filter residue and leachate containing nickel, molybdenum and vanadium;
(3) extracting vanadium from the leachate containing nickel, molybdenum and vanadium obtained in the step (2) to obtain a strip liquor and a vanadium raffinate;
(4) extracting molybdenum from the vanadium raffinate obtained in the step (3) to obtain molybdenum raffinate and strip liquor;
(5) and (4) adding sodium carbonate or sodium hydroxide into the molybdenum raffinate obtained in the step (4), adjusting the pH value to 7-8, filtering after the reaction is finished, evaporating and crystallizing to obtain a crude nickel sulfate product, and evaporating the crystallized filtrate to obtain an industrial sodium sulfate product.
2. The method according to claim 1, wherein in the step (1), the waste chemical industry catalyst is filter cake after FCC incineration.
3. The method according to claim 1, wherein in the step (1), the wet milling is performed in an ultra-fine mill, and the ratio of liquid to solid mass is 1.5 to 3: 1, the particle size of the material after wet grinding is not higher than 320 meshes.
4. The method as claimed in claim 1, wherein the filter residue obtained in step (2) is subjected to low acid leaching while adding hydrogen peroxide, and is subjected to pressure filtration to obtain a filtrate and a filter residue; conditions of low acid leaching: acidity of 15 < -25 > g/l, liquid-solid mass ratio of 1.5-2.5: 1. the temperature is 80-90 ℃ and the time is 4-6 hours; and (3) returning the filtrate to the acid leaching process in the step (2), washing filter residues, piling up the filter residues for producing building materials, and returning the filter residue washing liquor to the step (1).
5. The method of claim 1, wherein in step (2), the acid leaching conditions are: acidity of 120-: 1, the temperature is 80-90 ℃, and the time is 2-3 hours.
6. The method of claim 1, wherein in step (3), the process conditions for extracting vanadium comprise: pH value is 1.5-3, extracting agent is composed of 20% P204, 10% TBP and 70% sulfonated kerosene, compared with O/A2, extracting time is 5-6min, diluting agent is No. 260 sulfonated kerosene, organic phase is back-extracted by 1.5mol/L sulfuric acid, the back-extraction liquid containing vanadium is directly precipitated to obtain V2O5And (5) producing the product.
7. The method of claim 1, wherein in step (4), the process conditions for extracting molybdenum comprise: the method adopts a P204 and N235 combined extracting agent, wherein the P204 accounts for 20-50%, the N235 accounts for 80-50%, the diluent is 260# sulfonated kerosene, the initial pH is 3, the final pH is 5, and the organic phase is subjected to back extraction of molybdenum by using 4mol/l ammonia water.
8. The method of claim 1, wherein in step (4), ammonium bicarbonate is added to the strip liquor after purifying and removing impurities, and ammonium molybdate crystals are produced by evaporation and crystallization.
9. The method of claim 1, wherein in step (5), the crude nickel sulfate is purified to produce refined nickel sulfate or battery grade nickel sulfate.
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Cited By (9)
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| CN114015882A (en) * | 2021-10-29 | 2022-02-08 | 苏州博萃循环科技有限公司 | Method for recovering vanadium and nickel from POX carbon black |
| CN114134331A (en) * | 2021-11-25 | 2022-03-04 | 苏州博萃循环科技有限公司 | Method for preparing vanadyl sulfate and nickel sulfate from petroleum POX slag |
| CN114959261A (en) * | 2022-04-29 | 2022-08-30 | 北京科技大学 | Method for recovering tungsten, molybdenum, nickel and cobalt from multi-metal alloy in full-wet process |
| CN115198118A (en) * | 2022-06-29 | 2022-10-18 | 安庆市月铜钼业有限公司 | Process for producing sodium molybdate by using vanadium-molybdenum-containing calcine |
| CN115216649A (en) * | 2022-07-25 | 2022-10-21 | 中国石油大学(北京) | Method for preparing vanadium dioxide battery material by using waste vanadium titanium-based SCR catalyst |
| CN115478177A (en) * | 2022-08-30 | 2022-12-16 | 广东省科学院资源利用与稀土开发研究所 | Method for efficiently extracting vanadium, molybdenum and nickel from multi-metal vanadium shale |
| CN115491513A (en) * | 2022-09-08 | 2022-12-20 | 西北矿冶研究院 | Process for comprehensively recovering copper, cobalt and nickel from copper-cobalt-nickel-containing solid hazardous waste |
| CN116162803A (en) * | 2022-12-09 | 2023-05-26 | 成都虹波钼业有限责任公司 | Process for extracting valuable metals from alloy powder |
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Cited By (10)
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| CN114015882A (en) * | 2021-10-29 | 2022-02-08 | 苏州博萃循环科技有限公司 | Method for recovering vanadium and nickel from POX carbon black |
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