CN104815703A - Method for resuscitating spent catalytic cracking catalyst through gas-solid reaction with SiCl4 - Google Patents
Method for resuscitating spent catalytic cracking catalyst through gas-solid reaction with SiCl4 Download PDFInfo
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Abstract
The invention discloses a method for resuscitating spent catalytic cracking catalyst through gas-solid reaction with SiCl4 and relates to the solid waste disposal and application field. The resuscitating method includes steps of doing mixing roasted spent catalytic cracking catalyst material with gaseous SiCl4, and reacting to obtain catalyst product; using de-ionized water to wash the catalyst product till the pH value of filtered water is constant, and using organic acid to carry out acid pickling treatment on the washed catalyst; using de-ionized water to wash the catalyst subjected to acid pickling, filtering, mixing the obtained catalyst with rare earth chloride solution, stirring to obtain mixed size, filtering the mixed size, and drying to obtain the resuscitated catalyst. The resuscitating method uses gas-solid hybrid reaction between SiCl4 and spent catalyst and uses acid pickling treatment and rare earth deposition, the resuscitating method is simple, the heavy metal content of the resuscitated catalyst is low, the specific surface area is high, and the activity stability is good.
Description
Technical field:
The present invention relates to one and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, belongs to solid waste process and application.
Background technology:
Catalytic cracking catalyst is a kind of catalyst that in oil refining process, application quantity is maximum.Catalytic cracking catalyst is the inactivation through reasons such as cracking reaction green coke, high-temperature water hot recycling and heavy metal pollutions in use.Slightly high for activity, the poising agent that tenor is relatively very low can be applied to some catalytic cracking unit or use as the agent that goes into operation, and then becomes useless agent for activity very low (specific surface is lower), poising agent that content of beary metal is higher.
For the processing method of waste acetic acid, method relatively more conventional is at present buried, but bury and can pollute soil and groundwater resource; Therefore, lot of domestic and international researcher does a lot of work to reuse waste acetic acid, replaces fresh catalyst after especially carrying out resurrection process to it.As ChemCat company of the U.S. uses H
2s and Cl
2gas and dead catalyst react and remove Ni, V, Fe, then with hydrogen peroxide with containing SO
2water catalyst is oxidized, reduces washing, then ammonium exchanges, and makes revivification of catalyst.CCTI company of the U.S. develops ACT treatment system on the basis of Demet technique, with Demet resemble process.This processing step is various, not easy to operate.Shah utilizes chelating agent (second phthalein acetone, ethylenediamine tetra-acetic acid, ammonium citrate etc.) to process the FCC catalyst of metal poisoning.Result shows, closes the catalyst of reaction treatment, H through huge legendary turtle
2obviously decline with the productive rate of dry gas, but the activity change of catalyst is little.Flvin utilizes ammonium salt and rare earth compound solution to carry out ion-exchange to the FCC equilibrium catalyst (the Y zeolite containing USY and rare earth exchanged) after superchlorination, sulfuration and other method process, compares the catalyst activity after distinct methods process, selective and partially catalyzed agent demetalization degree.From the result of the test of Flvin, sulfuration and chlorination process are to removing heavy metal, and particularly nickel is very effective; The ion-exchange of ammonium salt and rare earth is helpful to the activity improving catalyst.Domestic Zheng Lian justice waits and adopts the method for oxidation acid leaching washing to be studied, but the activity of demetalization rear catalyst do not have be improved significantly, for this reason, they also adopt the method for ammonium salt activation process to improve catalyst activity.The kindheartedness tinkling of pieces of jade etc. adopt oxalic acid and liquor potassic permanganate process spent FCC catalyst, and nickel removal rate is the highest can close to 50%; Be 1: 7 in solid-to-liquid ratio, temperature is the NH merely with 1.5% under 80 ~ 100 DEG C of conditions
4nO
3solution-treated catalyst 0.5h, just can remove the nickel of more than 50%; With the HClO of 33%
4process, catalyst nickel removal rate just can reach 50%, and with 100% HClO
4process catalyst, nickel removal efficiency reaches as high as 66.7%.Li Chunyi etc. adopt HCl, HNO
3, H
2sO
4and HClO
4deng inorganic acid pickling and oxidation and pickling (hydrogen peroxide and oxalic acid) composite algorithm to FCC dead catalyst carry out demetalization bring back to life study, result shows, inorganic acid all has vanadium removal effect, and does not have nickel removal effect, and the nickel removal effect of oxidation and pickling composite algorithm is then better.CN101219396A adopts inorganic acid and organic acid to process FCC dead catalyst, makes the heavy metal partial removal of dead catalyst, and specific area increases and active raising.
The rejuvenation method of existing FCC dead catalyst mostly processing step more complicated, operates cumbersome above, although some method is relatively simple, be difficult to reach desirable effect, especially the removal efficiency of heavy metal is lower.
Summary of the invention:
For the problems referred to above, the technical problem to be solved in the present invention is to provide one and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst.
The present invention and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, it comprises the following steps: (1) by the catalytic cracking spent catalyst material after calcination process and gas phase SiCl
4mixing is reacted, and the reaction time, at 0.5-40 minute, obtains catalyst product;
(2) remain unchanged by the pH value that the catalyst product of deionized water to step (1) gained is washed to filtered water, then with organic acid, pickling processes is carried out to the catalyst after washing;
(3) wash with the catalyst of deionized water to step (2) gained and filter, wherein the mass ratio of deionized water and catalyst is 6-12: 1;
(4) catalyst step (3) obtained and re chloride mix and blend, in slurries, the ratio of water and catalyst butt is 6-10: 1, ratio 0.005-0.04: 1 of rare earth (in rare earth oxide) and catalyst butt;
(5) after being filtered by the mixed serum of step (4) gained, then within 0.25-4 hour, catalyst must be brought back to life in 120-400 DEG C of dry process.
As preferably, in described step (1), catalytic cracking spent catalyst temperature of charge is 250-450 DEG C, SiCl
4with mass ratio 0.05-0.5: 1 of the butt of catalytic cracking spent catalyst material.
As preferably, the organic acid in described step (2) can be the one or several arbitrarily in formic acid, oxalic acid, citric acid and tartaric acid.
As preferably, in described step (2), the time of pickling is 0.25-6 hour, and pickling pH value is 1-5, and pickling temperature is 60-120 DEG C.
As preferably, in described step (4), mixing time is 0.3-1.5 hour, and slurry pH value controls at 3.3-4.5.
Beneficial effect of the present invention: it can overcome the drawback of prior art, it adopts SiCl
4react with dead catalyst gas-solid mixing, pickling processes and rare earth deposit, its rejuvenation method is simple, and flexible operation, the catalyst content of beary metal after resurrection is low, and specific area is high, and activity stability is good.
Accompanying drawing illustrates:
For ease of illustrating, the present invention is described in detail by following concrete enforcement and accompanying drawing.
Fig. 1 is the physico-chemical property schematic diagram of catalytic cracking spent catalyst raw material used in each embodiment of the present invention;
The physico-chemical property schematic diagram of the resurrection catalyst that Fig. 2 obtains for each embodiment in the present invention;
The resurrection catalyst that Fig. 3 the present invention obtains carries out the physico-chemical property figure that Catalytic Cracking Performance evaluates feedstock oil used on small fixed flowing bed-tion reacting device;
Fig. 4 brings back to life catalyst on small fixed flowing bed-tion reacting device, carry out Catalytic Cracking Performance evaluation result analysis chart in the present invention.
Detailed description of the invention:
This detailed description of the invention is by the following technical solutions: it comprises the following steps: (1) by the catalytic cracking spent catalyst material after calcination process and gas phase SiCl
4mixing is reacted, and the reaction time, at 0.5-40 minute, obtains catalyst product;
(2) remain unchanged by the pH value that the catalyst product of deionized water to step (1) gained is washed to filtered water, then with organic acid, pickling processes is carried out to the catalyst after washing;
(3) wash with the catalyst of deionized water to step (2) gained and filter, wherein the mass ratio of deionized water and catalyst is 6-12: 1;
(4) catalyst step (3) obtained and re chloride mix and blend, in slurries, the ratio of water and catalyst butt is 6-10: 1, ratio 0.005-0.04: 1 of rare earth (in rare earth oxide) and catalyst butt;
(5) after being filtered by the mixed serum of step (4) gained, then within 0.25-4 hour, catalyst must be brought back to life in 120-400 DEG C of dry process.
As preferably, in described step (1), catalytic cracking spent catalyst temperature of charge is 250-450 DEG C, SiCl
4with mass ratio 0.05-0.5: 1 of the butt of catalytic cracking spent catalyst material.
As preferably, the organic acid in described step (2) can be the one or several arbitrarily in formic acid, oxalic acid, citric acid and tartaric acid.
As preferably, in described step (2), the time of pickling is 0.25-6 hour, and pickling pH value is 1-5, and pickling temperature is 60-120 DEG C.
As preferably, in described step (4), mixing time is 0.3-1.5 hour, and slurry pH value controls at 3.3-4.5.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Embodiment 1: by catalytic cracking spent catalyst (temperature of charge 400 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is designated as former dose, and its physical and chemical performance parameter as shown in Figure 1), SiCl
4be 0.25 with the mass ratio of catalytic cracking spent catalyst butt, the reaction time is 10 minutes.Reacted catalyst sample 10 times of deionized waters are carried out washing and filtering, then catalyst and oxalic acid solution is carried out mix and blend 1 hour, controlling solution ph is 3.0, and solution temperature remains on 90 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 10 used is doubly to catalyst butt quality, then after filtering catalyst and lanthanum chloride solution are carried out mix and blend, mixing time is 45 minutes, lanthanum chloride (in lanthana) is 0.015: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 8: 1, and it is 3.7 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 300 DEG C, and drying time is 45 minutes, finally must bring back to life catalyst sample, is designated as sample 1.The physico-chemical property of products therefrom is shown in Fig. 2.In Fig. 2, specific area and pore volume adopt BET method to measure.
Embodiment 2: by catalytic cracking spent catalyst (temperature of charge 350 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is with embodiment 1), SiCl
4be 0.35 with the mass ratio of catalytic cracking spent catalyst butt, the reaction time is 20 minutes.Reacted catalyst sample 10 times of deionized waters are carried out washing and filtering, then catalyst and citric acid solution is carried out mix and blend 1.5 hours, controlling solution ph is 3.5, and solution temperature remains on 95 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 9 used is doubly to catalyst butt quality, then after filtering catalyst and rare earth chloride (lanthanum chloride: cerium chloride mass ratio is 6: 4) solution are carried out mix and blend, mixing time is 60 minutes, rare earth chloride (in rare earth oxide) is 0.025: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 9: 1, and it is 3.6 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 350 DEG C, and drying time is 30 minutes, finally must bring back to life catalyst sample, is designated as sample 2.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 3: by catalytic cracking spent catalyst (temperature of charge 250 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is with embodiment 1), SiCl
4be 0.15 with the mass ratio of the butt of catalytic cracking spent catalyst, the reaction time is 40 minutes.Reacted catalyst sample 8 times of deionized waters are carried out washing and filtering, then catalyst and tartaric acid solution is carried out mix and blend 3 hours, controlling solution ph is 5.0, and solution temperature remains on 60 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 7 used is doubly to catalyst butt quality, then after filtering catalyst and rare earth chloride (lanthanum chloride: cerium chloride mass ratio is 7: 3) solution are carried out mix and blend, mixing time is 50 minutes, rare earth chloride (in rare earth oxide) is 0.01: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 7: 1, and it is 3.8 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 250 DEG C, and drying time is 1 hour, finally must bring back to life catalyst sample, is designated as sample 3.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 4: by catalytic cracking spent catalyst (temperature of charge 450 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is designated as former dose, and its physical and chemical performance parameter as shown in Figure 1), SiCl
4be 0.05 with the mass ratio of catalytic cracking spent catalyst butt, the reaction time is 0.5 minute.Reacted catalyst sample 5 times of deionized waters are carried out washing and filtering, then catalyst and oxalic acid and citric acid mixed solution (mass ratio of oxalic acid and citric acid is 1: 1) are carried out mix and blend 15 minutes, controlling solution ph is 1.0, and solution temperature remains on 70 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 12 used is doubly to catalyst butt quality, then after filtering catalyst and solution of cerium chloride by oxidation are carried out mix and blend, mixing time is 18 minutes, cerium chloride (in cerium oxide) is 0.005: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 6: 1, and it is 4.5 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 200 DEG C, and drying time is 1.5 hours, finally must bring back to life catalyst sample, is designated as sample 4.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 5: by catalytic cracking spent catalyst (temperature of charge 300 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is designated as former dose, and its physical and chemical performance parameter as shown in Figure 1), SiCl
4be 0.5 with the mass ratio of catalytic cracking spent catalyst butt, the reaction time is 30 minutes.Reacted catalyst sample 12 times of deionized waters are carried out washing and filtering, then catalyst and oxalic acid and tartaric mixed solution (oxalic acid and tartaric acid mass ratio are 1: 1) are carried out mix and blend 2 hours, controlling solution ph is 4.0, and solution temperature remains on 100 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 8 used is doubly to catalyst butt quality, then after filtering catalyst and lanthanum chloride solution are carried out mix and blend, mixing time is 1.5 hours, lanthanum chloride (in lanthana) is 0.04: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 10: 1, and it is 4.0 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 150 DEG C, and drying time is 2.5 hours, finally must bring back to life catalyst sample, is designated as sample 5.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 6: by catalytic cracking spent catalyst (temperature of charge 280 DEG C) and gas phase SiCl through calcination process
4carry out hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is designated as former dose, and its physical and chemical performance parameter as shown in Figure 1), SiCl
4be 0.2 with the mass ratio of catalytic cracking spent catalyst butt, the reaction time is 35 minutes.Reacted catalyst sample 9 times of deionized waters are carried out washing and filtering, then catalyst and oxalic acid, citric acid and tartaric mixed solution (oxalic acid, citric acid and tartaric mass ratio are 1: 1: 1) are carried out mix and blend 1 hour, controlling solution ph is 2.5, and solution temperature remains on 80 DEG C.Catalyst sample after pickling is being washed, the deionized water water yield 11 used is doubly to catalyst butt quality, then after filtering catalyst and lanthanum chloride solution are carried out mix and blend, mixing time is 35 hours, lanthanum chloride (in lanthana) is 0.012: 1 with the mass ratio of catalyst butt, in slurries, water and catalyst butt mass ratio are 8: 1, and it is 3.9 that slurry pH value controls.After being filtered by above-mentioned slurries, then carry out drying process to the catalyst sample obtained, baking temperature is 120 DEG C, and drying time is 4 hours, finally must bring back to life catalyst sample, is designated as sample 6.The physico-chemical property of products therefrom is shown in Fig. 2.In Fig. 2, * MAT is expressed as the micro anti-active index of catalytic cracking catalyst, as shown in Figure 2, Fe, Ni, V in the catalyst after resurrection, the content of beary metal such as Ca and Na is low, specific area and micro anti-active index significantly improve.
The resurrection catalyst of above-described embodiment gained is carried out Catalytic Cracking Performance evaluation on small fixed flowing bed-tion reacting device (FFB).Evaluate catalysts is the mixing (mixed catalyst is labeled as embodiment numbering) of former dose and resurrection catalyst, and its Central Plains agent accounts for 30% of mixed catalyst, brings back to life catalyst and accounts for 70% of mixed catalyst.Reaction condition is as follows: reaction temperature is 500 DEG C, and oil ratio is 4.0, and mass space velocity is 20h
-1.As shown in Figure 3, cracking reaction Evaluation results as shown in Figure 4, can be drawn by Fig. 4 raw materials used oil nature: bring back to life the coke yield that can reduce device in catalyst application to catalytic cracking unit, can improve the yield of gasoline and liquefied gas simultaneously.
Claims (5)
1. one kind and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, is characterized in that: its rejuvenation method comprises the following steps: that (1) is by the catalytic cracking spent catalyst material after calcination process and gas phase SiCl
4mixing is reacted, and the reaction time, at 0.5-40 minute, obtains catalyst product;
(2) remain unchanged by the pH value that the catalyst product of deionized water to step (1) gained is washed to filtered water, then with organic acid, pickling processes is carried out to the catalyst after washing;
(3) wash with the catalyst of deionized water to step (2) gained and filter, wherein the mass ratio of deionized water and catalyst is 6-12: 1;
(4) catalyst step (3) obtained and re chloride mix and blend, in slurries, the ratio of water and catalyst butt is 6-10: 1, rare earth, in rare earth oxide, and ratio 0.005-0.04: 1 of catalyst butt;
(5) after being filtered by the mixed serum of step (4) gained, then within 0.25-4 hour, catalyst must be brought back to life in 120-400 DEG C of dry process.
2. one according to claim 1 and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, is characterized in that: in described step (1), catalytic cracking spent catalyst temperature of charge is 250-450 DEG C, SiCl
4with mass ratio 0.05-0.5: 1 of the butt of catalytic cracking spent catalyst material.
3. one according to claim 1 and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, is characterized in that: the organic acid in described step (2) can be the one in formic acid, oxalic acid, citric acid and tartaric acid and several arbitrarily.
4. one according to claim 1 and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, is characterized in that: in described step (2), the time of pickling is 0.25-6 hour, and pickling pH value is 1-5, and pickling temperature is 60-120 DEG C.
5. one according to claim 1 and SiCl
4the rejuvenation method of gas-solid reaction catalytic cracking spent catalyst, is characterized in that: in described step (4), mixing time is 0.3-1.5 hour, and slurry pH value controls at 3.3-4.5.
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Cited By (3)
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|---|---|---|---|---|
| CN106552680A (en) * | 2016-12-07 | 2017-04-05 | 四川润和催化新材料股份有限公司 | A kind of method of FCC dead catalyst Demetalizing reactivating |
| CN106622395A (en) * | 2015-10-29 | 2017-05-10 | 中国石油化工股份有限公司 | Method for modifying catalytic cracking equilibrium agent |
| CN115999650A (en) * | 2021-10-22 | 2023-04-25 | 中国石油化工股份有限公司 | Reactivating method of catalytic cracking dead catalyst |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106622395A (en) * | 2015-10-29 | 2017-05-10 | 中国石油化工股份有限公司 | Method for modifying catalytic cracking equilibrium agent |
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| CN115999650A (en) * | 2021-10-22 | 2023-04-25 | 中国石油化工股份有限公司 | Reactivating method of catalytic cracking dead catalyst |
| CN115999650B (en) * | 2021-10-22 | 2024-07-09 | 中国石油化工股份有限公司 | Reactivating method of catalytic cracking dead catalyst |
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