CN108067244B - Method for recycling waste catalyst - Google Patents
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Abstract
The invention discloses a method for recycling a waste catalyst, which comprises the following steps: (1) extracting, drying, microwave treating and crushing the molybdenum-nickel series waste catalyst; (2) mixing the crushed catalyst with alkali, and then roasting at high temperature; (3) dipping the roasted catalyst in hot water, and filtering to obtain metaaluminate filtrate and nickel oxide solid; (4) reacting the filtrate obtained in the step (3) with an aluminum salt acid solution, filtering, preparing pseudo-boehmite, kneading the pseudo-boehmite, molding and roasting to obtain a carrier; (5) performing activated carbon adsorption on the solution filtered in the step (4) to obtain molybdenum, and desorbing the solution by using ammonia water after adsorption to obtain an ammonium molybdate solution; (6) adding acid into the solid filtered in the step (3), adjusting the pH value by adopting an alkaline solution to remove Fe and Al in the solution, and concentrating to obtain a nickel salt solution; (7) adding the nickel nitrate solution obtained in the step (6) into the solution obtained in the step (5) to obtain a molybdenum-nickel-ammonia solution; (8) and (5) impregnating, drying and roasting the carrier in the step (4) and the solution in the step (7) to prepare the catalyst. The method has the characteristics of simple process, low treatment cost and the like.
Description
Technical Field
The invention relates to a method for recycling a waste catalyst, in particular to a method for preparing a hydrogenation catalyst by using a molybdenum-nickel waste catalyst, and particularly relates to a molybdenum-nickel hydrogenation catalyst for distillate oil.
Technical Field
In modern oil refining and chemical industry, more than 90% of chemical reactions are realized through a catalytic process, and a catalyst becomes a key for developing new products of new processes for realizing oil refining and chemical industry. However, when the catalyst is changed into a waste catalyst, certain harm is caused to the environment. At present, the basic service life of a residual oil hydrogenation catalyst is 8000 hours, each set of residual oil hydrogenation device generates hundreds of tons of waste catalysts every year, more than ten sets of residual oil hydrogenation devices are in existence at home at present, and the quantity of the residual oil waste catalysts in China can reach thousands of tons every year. The molybdenum-nickel active metal content on the residual oil hydrogenation catalyst is lower than that of other catalysts, the metal recovery problem is mainly considered by catalyst recovery enterprises at present, and the utilization rate of the carrier is too low for alumina carriers which are basically used as waste residues for cement or ceramic enterprises. The recycling of active metal and alumina carrier becomes an important direction for the research of hydrogenation catalyst at present.
At present, the technology for recovering metals from aluminum-based waste catalysts is more. CN941106479.6 proposes a pyrogenic process for recovering Ni from spent catalysts, which requires higher calcination temperatures. CN200910020761.2 proposes a method for recovering metals from a molybdenum-containing spent catalyst, which comprises pulverizing the catalyst, and then reacting with soda ash to extract Mo. CN200910020761.2 discloses a method for recovering molybdenum from catalyst aluminum-based waste catalyst, which is also to extract molybdenum by crushing the catalyst, mixing with alkali and calcining. CN200410050503.6 discloses a method for producing vanadium pentoxide by using a vanadium-containing waste catalyst, which comprises the steps of firstly removing deposited oil, crushing, leaching and the like to recover sodium vanadate and sodium molybdate in sequence, roasting, leaching, recovering sodium vanadate and sodium molybdate for the second time, and finally preparing vanadium pentoxide. US4544533 discloses a process for recovering metals from spent supported hydroprocessing catalysts by calcining coke and sulphur-containing residues and then leaching the metals from the spent catalyst. US4514369 discloses obtaining metals on spent catalysts by liquid-liquid extraction separation and the like. The existing waste catalyst recycling mainly considers the recycling of metal or the recycling of a replacing device, the metal is simply recycled, so that a large amount of alumina carriers are wasted, and the waste catalyst replacing device cannot meet the recycling of all waste catalysts.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for recovering and preparing a new catalyst from a molybdenum-nickel waste catalyst, in particular to a distillate oil refining catalyst. The method has the characteristics of simple process, low treatment cost and the like.
A method for recycling a waste catalyst comprises the following steps:
(1) extracting, drying, microwave treating and crushing the molybdenum-nickel series waste catalyst;
(2) mixing the crushed catalyst with alkali, and then roasting at high temperature;
(3) dipping the roasted catalyst in hot water, and filtering to obtain metaaluminate filtrate and nickel oxide solid;
(4) reacting the filtrate obtained in the step (3) with an aluminum salt acid solution, filtering, preparing pseudo-boehmite, kneading the pseudo-boehmite, molding and roasting to obtain a carrier;
(5) performing activated carbon adsorption on the solution filtered in the step (4) to obtain molybdenum, and desorbing the solution by using ammonia water after adsorption to obtain an ammonium molybdate solution;
(6) adding acid into the solid filtered in the step (3), adjusting the pH value by adopting an alkaline solution to remove Fe and Al in the solution, and concentrating to obtain a nickel salt solution;
(7) adding the nickel nitrate solution obtained in the step (6) into the solution obtained in the step (5) to obtain a molybdenum-nickel-ammonia solution;
(8) and (5) impregnating, drying and roasting the carrier in the step (4) and the solution in the step (7) to prepare the catalyst.
In the method, the molybdenum-nickel waste hydrogenation catalyst in the step (1) contains 70-90% of catalyst solid and 10-30% of petroleum fraction by weight, wherein the weight content of nickel oxide in the extracted catalyst is 3-10% and the weight content of molybdenum oxide is 10-25%. The organic solvent adopted by the extraction is toluene, petroleum ether, ethanol and the like, and the extraction temperature is 80-110 ℃. The microwave treatment frequency is 915-2450 MHz, and the treatment time is 3-8 h. The microwave treatment is preferably carried out in a mixed atmosphere of gaseous methanol and nitrogen, and the volume ratio of the gaseous methanol to the nitrogen is 1:3-1: 5. The microwave treatment is carried out in the mixed atmosphere of gaseous methanol and nitrogen, so that the acting force between the molybdenum-nickel metal and the alumina carrier is further reduced, the subsequent efficient separation of the molybdenum-nickel metal and alumina is improved, and research results show that the process can also play a role in improving the activity of the catalyst. The crushing is carried out until the crushing granularity is 200-400 meshes, preferably 300-400 meshes.
In the method, the alkali in the step (2) can be one or more of sodium hydroxide, sodium carbonate and potassium hydroxide, and the alkali and Al contained in the waste catalyst2O3The molar ratio of (A) to (B) is 4 to 1, preferably 2.5 to 1.5; the high-temperature roasting temperature is 700-1000 ℃, preferably 850-950 ℃, the roasting time is 2-6 h, and most preferablyPreferably 3 to 5 hours.
In the method, the hot water temperature in the step (3) is 85-110 ℃, preferably 90-100 ℃, the liquid-solid ratio is 7-3, preferably 6-4, and the leaching time is 0.2-2 hours, preferably 0.5-1 hour.
In the method, the acidic solution in the step (4) is aluminum chloride, aluminum nitrate or aluminum sulfate, the pH value of the acidic solution is 1-3, the filtrate in the step (3) reacts with the acidic solution to control the pH value to be 7-9, preferably 7-7.5, the reaction temperature is controlled to be 50-80 ℃, and the roasting temperature of the carrier is 500-1000 ℃.
In the method, the granularity of the activated carbon in the step (5) is 20-200 meshes, preferably 40-80 meshes; complexing agents may be added during the adsorption process, such as: hydrochloric acid, 8-hydroxyquinoline, and the like.
In the method, the acid in the step (6) is sulfuric acid, the alkaline solution is a sodium hydroxide solution, and the mass concentration of the sodium hydroxide solution is 2-15%, preferably 4-10%; the pH is adjusted to 5 to 6.5, preferably 5.5 to 6.2.
In the method, in the step (8), the drying temperature is 100-180 ℃, the drying time is 2-5 hours, the roasting temperature is 400-600 ℃, and the roasting time is 2-4 hours.
The method can effectively recover the active metal and the alumina in the molybdenum-nickel system waste catalyst after industrial operation, and is an environment-friendly catalyst preparation method. Compared with the prior art, the heat stress generated by microwave treatment can separate molybdenum nickel metal from aluminum oxide, thereby improving the recovery efficiency of the metal and the aluminum oxide; the waste catalyst can effectively recycle alumina to prepare a hydrogenation catalyst carrier; the molybdenum-nickel active metal can be recovered and prepared into metal solution again; the method can lead the catalyst to be recycled, improve the environmental condition and create good economic benefit.
Detailed Description
The operation and effect of the present invention will be further described with reference to the following examples.
Example 1
Extracting and deoiling the molybdenum-nickel catalyst after industrial operation, drying, and performing microwave treatment for 5 hours; weighing 100g of catalyst, and crushing to 300 meshes; weighing 166g of sodium carbonate, uniformly mixing with the waste catalyst, roasting at 850 ℃ for 4h, leaching with 500g of hot water at 90 ℃, filtering, and obtaining the residue 1. Preparing pseudo-boehmite from the filtered solution and an acidic solution (aluminum sulfate) at the temperature of 60 ℃ and the pH value of 7, and filtering to obtain a filtrate 1; mixing pseudo-boehmite with an adhesive, molding, roasting at 700 ℃ for 3 hours to obtain 86g of carrier, slowly adding hydrochloric acid into the filtrate 1, adjusting the pH value to be acidic, heating to 60 ℃, and adding 300g of 200-mesh active carbon for active carbon adsorption; after adsorbing for 3 hours, desorbing by adopting ammonia water to prepare an ammonium molybdate solution with the concentration of 0.55 g/ml; adding the filter residue 1 into a nitric acid solution until the filter residue is completely dissolved, slowly adjusting the pH value to 6.2 by adopting ammonia water, filtering, and then adjusting the concentration of a nickel nitrate solution to 0.11 g/mL; mixing a nickel nitrate solution and an ammonium molybdate solution, soaking the mixture on 80g of a carrier, drying the carrier, roasting the carrier for 3 hours at 470 ℃ to prepare 98g of a catalyst A,
example 2
Extracting and deoiling the molybdenum-nickel catalyst after industrial operation, drying, and performing microwave treatment for 8 hours; weighing 100g of catalyst, and crushing to 300 meshes; weighing 166g of sodium carbonate, uniformly mixing with the waste catalyst, roasting at 850 ℃ for 4h, leaching with 500g of hot water at 90 ℃, filtering, and obtaining the residue 1. Preparing pseudo-boehmite from the filtered solution and an acidic solution (aluminum sulfate) at the temperature of 60 ℃ and the pH value of 7, and filtering to obtain a filtrate 1; mixing pseudo-boehmite with an adhesive, molding, roasting at 700 ℃ for 3 hours to obtain 86g of carrier, slowly adding hydrochloric acid into the filtrate 1, adjusting the pH value to be acidic, heating to 60 ℃, and adding 300g of 100-mesh active carbon for active carbon adsorption; after adsorbing for 3 hours, desorbing by adopting ammonia water to prepare an ammonium molybdate solution with the concentration of 0.55 g/ml; adding the filter residue 1 into a nitric acid solution until the filter residue is completely dissolved, slowly adjusting the pH value to 6.2 by adopting ammonia water, filtering, and then adjusting the concentration of a nickel nitrate solution to 0.11 g/mL; mixing a nickel nitrate solution and an ammonium molybdate solution, soaking the mixture on 80g of a carrier, drying the carrier, roasting the carrier for 3 hours at 470 ℃ to prepare 98g of a catalyst B,
example 3
Extracting and deoiling the molybdenum-nickel catalyst after industrial operation, drying, and performing microwave treatment for 5 hours; weighing 100g of catalyst, and crushing to 300 meshes; weighing 166g of sodium carbonate, uniformly mixing with the waste catalyst, roasting at 850 ℃ for 4h, leaching with 500g of hot water at 90 ℃, filtering, and obtaining the residue 1. Preparing pseudo-boehmite from the filtered solution and an acidic solution (aluminum sulfate) at the temperature of 60 ℃ and the pH value of 7, and filtering to obtain a filtrate 1; slowly adding hydrochloric acid into the filtrate 1, adjusting the filtrate to be acidic, heating to 60 ℃, adding 300g of 200 meshes of active carbon for active carbon adsorption, and adding a complexing agent of octahydroxyquinoline during the active carbon adsorption; after adsorbing for 2 hours, desorbing by adopting ammonia water to prepare an ammonium molybdate solution with the concentration of 0.55 g/ml; adding the filter residue 1 into a nitric acid solution until the filter residue is completely dissolved, slowly adjusting the pH value to 6.2 by adopting ammonia water, filtering, and then adjusting the concentration of a nickel nitrate solution to 0.11 g/mL; mixing a nickel nitrate solution and an ammonium molybdate solution, soaking the mixture on 80g of a carrier, drying the carrier, roasting the carrier for 3 hours at 470 ℃ to prepare 98g of a catalyst C,
example 4
Extracting and deoiling a molybdenum-nickel catalyst after industrial operation, drying, performing microwave treatment for 5 hours, wherein the microwave treatment is performed in a mixed atmosphere of gaseous methanol and nitrogen, and the volume ratio of the gaseous methanol to the nitrogen is 1: 3. (ii) a Weighing 100g of catalyst, and crushing to 300 meshes; weighing 166g of sodium carbonate, uniformly mixing with the waste catalyst, roasting at 850 ℃ for 4h, leaching with 500g of hot water at 90 ℃, filtering, and obtaining the residue 1. Preparing pseudo-boehmite from the filtered solution and an acidic solution (aluminum sulfate) at the temperature of 60 ℃ and the pH value of 7, and filtering to obtain a filtrate 1; mixing pseudo-boehmite with an adhesive, molding, roasting at 700 ℃ for 3 hours to obtain 86g of carrier, slowly adding hydrochloric acid into the filtrate 1, adjusting the pH value to be acidic, heating to 60 ℃, and adding 300g of 200-mesh active carbon for active carbon adsorption; after adsorbing for 3 hours, desorbing by adopting ammonia water to prepare an ammonium molybdate solution with the concentration of 0.55 g/ml; adding the filter residue 1 into a nitric acid solution until the filter residue is completely dissolved, slowly adjusting the pH value to 6.5 by adopting ammonia water, filtering, and then adjusting the concentration of a nickel nitrate solution to 0.11 g/mL; mixing a nickel nitrate solution and an ammonium molybdate solution, soaking the mixture on 80g of a carrier, drying the carrier, roasting the carrier for 3 hours at 470 ℃ to prepare 98g of a catalyst D,
example 5
Extracting and deoiling a molybdenum-nickel catalyst after industrial operation, drying, performing microwave treatment for 5 hours, wherein the microwave treatment is performed in a mixed atmosphere of gaseous methanol and nitrogen, and the volume ratio of the gaseous methanol to the nitrogen is 1: 5. (ii) a Weighing 100g of catalyst, and crushing to 300 meshes; weighing 166g of sodium carbonate, uniformly mixing with the waste catalyst, roasting at 850 ℃ for 4h, leaching with 500g of hot water at 90 ℃, filtering, and obtaining the residue 1. Preparing pseudo-boehmite from the filtered solution and an acidic solution (aluminum sulfate) at the temperature of 60 ℃ and the pH value of 7, and filtering to obtain a filtrate 1; slowly adding hydrochloric acid into the filtrate 1, adjusting the filtrate to be acidic, heating to 60 ℃, adding 300g of 200 meshes of active carbon for active carbon adsorption, and adding a complexing agent of octahydroxyquinoline during the active carbon adsorption; after adsorbing for 2 hours, desorbing by adopting ammonia water to prepare an ammonium molybdate solution with the concentration of 0.55 g/ml; adding the filter residue 1 into a nitric acid solution until the filter residue is completely dissolved, slowly adjusting the pH value to 6.5 by adopting ammonia water, filtering, and then adjusting the concentration of a nickel nitrate solution to 0.11 g/mL; mixing a nickel nitrate solution and an ammonium molybdate solution, soaking the mixture on 80g of a carrier, drying the carrier, roasting the carrier for 3 hours at 470 ℃ to prepare 98g of a catalyst E,
comparative example 1
Preparing a catalyst by adopting an industrial alumina carrier, preparing a molybdenum-nickel-ammonia solution by adopting ammonium molybdate, nickel nitrate and ammonia water, spraying and soaking the catalyst according to the water absorption rate of 1.0, and roasting at 470 ℃ for 3 hours to prepare a catalyst F
Comparative example 2
The molybdenum-nickel catalyst obtained in example 1 after the industrial operation was subjected to extraction and deoiling, dried, and calcined to obtain catalyst G.
The catalysts prepared in examples 1 to 5 and comparative examples 1 and 2 were evaluated on a 200ml fixed bed hydrogenation test apparatus at a reaction pressure of 15.7 MPa, a reaction temperature of 380 ℃ and a hydrogen-oil volume ratio of 800(v), the properties of the feed oil are shown in Table 1, and the 500-hour test results are shown in Table 2.
TABLE 1
TABLE 2
| Catalyst and process for preparing same | A | B | C | D | E | F | G |
| Demetallization rate,% | 61 | 63 | 62 | 67 | 69 | 68 | 40 |
Claims (11)
1. A method for recycling a waste catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) extracting, drying, microwave treating and crushing the molybdenum-nickel series waste catalyst;
(2) mixing the crushed catalyst with alkali, and then roasting at high temperature;
(3) dipping the roasted catalyst in hot water, and filtering to obtain metaaluminate filtrate and nickel oxide solid;
(4) reacting the filtrate obtained in the step (3) with an aluminum salt acid solution, filtering, preparing pseudo-boehmite, kneading the pseudo-boehmite, molding and roasting to obtain a carrier;
(5) performing activated carbon adsorption on the solution filtered in the step (4) to obtain molybdenum, and desorbing the solution by using ammonia water after adsorption to obtain an ammonium molybdate solution;
(6) adding acid into the solid filtered in the step (3), adjusting the pH value by adopting an alkaline solution to remove Fe and Al in the solution, and concentrating to obtain a nickel salt solution;
(7) adding the nickel nitrate solution obtained in the step (6) into the solution obtained in the step (5) to obtain a molybdenum-nickel-ammonia solution;
(8) and (5) impregnating, drying and roasting the carrier in the step (4) and the solution in the step (7) to prepare the catalyst.
2. The method of claim 1, wherein: the molybdenum-nickel spent hydrogenation catalyst in the step (1) contains 70-90% of catalyst solid and 10-30% of petroleum fraction by weight, and the weight content of nickel oxide and molybdenum oxide in the extracted catalyst is 3-10% and 10-25% respectively.
3. The method of claim 1, wherein: the organic solvent adopted in the extraction in the step (1) is one or more of toluene, petroleum ether and ethanol, and the extraction temperature is 80-110 ℃.
4. The method of claim 1, wherein: in the step (1), the microwave treatment frequency is 915-2450 MHz, and the treatment time is 3-8 h.
5. The method of claim 1, wherein: the microwave treatment in the step (1) is carried out in a mixed atmosphere of gaseous methanol and nitrogen, and the volume ratio of the gaseous methanol to the nitrogen is 1:3-1: 5.
6. The method of claim 1, wherein: in the step (2), the alkali is one or more of sodium hydroxide, sodium carbonate and potassium hydroxide, and the alkali and Al contained in the waste catalyst2O3The molar ratio of (A) to (B) is 4-1; the high-temperature roasting temperature is 700-1000 ℃, and the roasting time is 2-6 h.
7. The method of claim 1, wherein: in the step (3), the temperature of the hot water is 85-110 ℃, the liquid-solid volume ratio is 7-3, and the dipping time is 0.2-2 h.
8. The method of claim 1, wherein: the acidic solution in the step (4) is aluminum chloride, aluminum nitrate or aluminum sulfate, the pH value of the acidic solution is 1-3, the filtrate in the step (3) reacts with the acidic solution to control the pH value to be 7-9, the reaction temperature is controlled to be 50-80 ℃, and the roasting temperature of the carrier is 500-1000 ℃.
9. The method of claim 1, wherein: in the step (5), the granularity of the activated carbon is 20-200 meshes; and adding a complexing agent in the adsorption process.
10. The method of claim 1, wherein: the acid in the step (6) is sulfuric acid, the alkaline solution is a sodium hydroxide solution, the mass concentration of the sodium hydroxide solution is 2-15%, and the pH value is adjusted to be 5-6.5.
11. The method of claim 1, wherein: in the step (8), the drying temperature is 100-180 ℃, the drying time is 2-5 h, the roasting temperature is 400-600 ℃, and the roasting time is 2-4 h.
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| CN108893594A (en) * | 2018-06-12 | 2018-11-27 | 昆明冶金高等专科学校 | A kind of method of carbon distribution and sulphur in quick abjection failure platinum-rhenium catalyst |
| CN108751241B (en) * | 2018-07-31 | 2019-07-26 | 菏泽华立新材料有限公司 | A kind of alkali treatment method and its processing unit of aluminium isopropoxide dead catalyst |
| CN111821992B (en) * | 2019-04-18 | 2022-08-12 | 中国石油化工股份有限公司 | Preparation method of high-activity hydrodemetallization catalyst |
| CN112619658A (en) * | 2019-09-24 | 2021-04-09 | 中国石油化工股份有限公司 | Method for recycling waste hydrogenation catalyst |
| CN113694932B (en) * | 2020-05-22 | 2024-01-09 | 中国石油化工股份有限公司 | Residual oil hydrotreating catalyst, preparation method and recycling thereof |
| CN114427029B (en) * | 2020-10-29 | 2024-07-09 | 中国石油化工股份有限公司 | Heavy oil treatment method for realizing metal separation and recovery |
| CN112645372B (en) * | 2021-01-19 | 2023-05-05 | 广西化工研究院有限公司 | Method for recycling waste activated alumina regenerant for hydrogen peroxide |
| CN113564386B (en) * | 2021-07-23 | 2022-11-29 | 中国科学院过程工程研究所 | Method for recovering molybdenum from waste nickel-molybdenum catalyst |
| CN113789446A (en) * | 2021-08-23 | 2021-12-14 | 常州大学 | Method for recovering molybdenum, vanadium and nickel metals from waste catalyst |
| CN115957770B (en) * | 2021-10-08 | 2024-06-28 | 中国石油化工股份有限公司 | Preparation method of boiling bed residual oil hydrogenation catalyst |
| CN117324046A (en) * | 2023-09-25 | 2024-01-02 | 青岛金牛油脂科技有限公司 | Regeneration method of nickel catalyst for grease hydrogenation |
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