CN104801353B - Roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst - Google Patents
Roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000004523 catalytic cracking Methods 0.000 title claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 23
- 230000003716 rejuvenation Effects 0.000 title claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 28
- 229910003910 SiCl4 Inorganic materials 0.000 claims abstract description 25
- 239000000047 product Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000012467 final product Substances 0.000 claims abstract description 4
- 239000012071 phase Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 8
- 230000004044 response Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- -1 rare earth compound Chemical class 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 150000002910 rare earth metals Chemical group 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 206010027439 Metal poisoning Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- BWKOZPVPARTQIV-UHFFFAOYSA-N azanium;hydron;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [NH4+].OC(=O)CC(O)(C(O)=O)CC([O-])=O BWKOZPVPARTQIV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002010 green coke Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention discloses roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst, it are related to solid waste and process and applied technical field.Its rejuvenation method comprises the following steps：(1) by the catalytic cracking spent catalyst material after fired process and gas phase SiCl4Mixing is reacted, and obtains catalyst product, and the temperature of the material of this catalytic cracking spent catalyst is 250 450 DEG C；(2) deionized water keeps constant to the pH value that the catalyst product of step (1) gained carries out being washed to filter water, process is dried again, the temperature of dried is 100 350 DEG C, and drying time is 0.25 4 hours, obtains final product resurrection catalyst.It adopts SiCl4Gas-solid mixing reaction and washing process are carried out with catalytic cracking spent catalyst, rejuvenation method is fairly simple, flexible operation, the resurrection catalyst content of beary metal of gained is low, specific surface area is high, activity stability is good.
Description
Technical field：
The present invention relates to roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst, belongs to solid waste
Thing process and applied technical field.
Background technology：
Catalytic cracking catalyst is the maximum a kind of catalyst of application amount in oil refining process.Catalytic cracking catalyst is being used
During the reason such as cracked reaction green coke, high-temperature water hot recycling and heavy metal pollution and inactivate.For active slightly higher, metal
The relatively very low poising agent of content can apply to some catalytic cracking units or use as the agent that goes into operation, and for active very low
The higher poising agent of (specific surface is relatively low), content of beary metal then becomes useless agent.
For the processing method of waste acetic acid, method the more commonly used at present is to bury, can be right but bury
Soil and groundwater resource is polluted；Therefore, lot of domestic and international researcher is done a lot of work to the useless catalytic cracking of reuse
Catalyst, especially carries out replacing fresh catalyst after resurrection process to which.As ChemCat companies of the U.S. use H2S and Cl2Gas
Ni, V, Fe are removed with dead catalyst reaction, then with hydrogen peroxide and contains SO2Water catalyst is carried out aoxidizing, reduces washing, then
Ammonium is exchanged, and makes revivification of catalyst.CCTI companies of the U.S. develop ACT processing systems on the basis of Demet techniques, with Demet
Technique is similar.The processing step is various, not easy to operate.Shah utilizes chelating agen (second phthalein acetone, ethylenediaminetetraacetic acid, citric acid
Ammonium etc.) process metal poisoning FCC catalyst.As a result show, through the catalyst of sequestration reaction treatment, H2Yield with dry gas
It is decreased obviously, but the activity change of catalyst is little.Elvin is using ammonium salt and rare earth compound solution to through superchlorination, sulfuration
And the FCC equilibrium catalysts (Y zeolite containing USY and rare earth exchanged) after other methods process have carried out ion exchange, compare
Catalyst activity, selectivity and partial catalyst demetalization degree after distinct methods process.From in terms of the result of the test of Elvin,
Sulfuration and chloridized are very effective to removing heavy metal, particularly nickel；The ion exchange of ammonium salt and rare earth is to improving catalyst
Activity is helpful.Domestic Zheng Lian justice etc. is studied using the method that oxidation acid leaching is washed, but demetalization rear catalyst
Activity not be improved significantly, for this purpose, they are also adopted by the method for ammonium salt activation processing to improve catalyst activity.Kindheartedness
Tinkling of pieces of jade etc. processes spent FCC catalyst, nickel removal rate highest accessible 50% using oxalic acid and potassium permanganate solution；It is 1: 7 in solid-to-liquid ratio,
Temperature be under the conditions of 80～100 DEG C simple with 1.5% NH4NO3Solution processes catalyst 0.5h, it is possible to remove more than 50%
Nickel；With 33% HClO4Process, catalyst nickel removal rate can just reach 50%, and use 100% HClO4Process catalyst,
Nickel removal efficiency reaches as high as 66.7%.Li Chunyi etc. adopts HCl, HNO3, H2SO4And HClO4Deng mineral acid pickling and oxidation and
Pickling (hydrogen peroxide and oxalic acid) composite algorithm carries out demetalization and brings back to life research to FCC dead catalyst, as a result shows, mineral acid all has
Vanadium removal effect, and there is no nickel removal effect, the nickel removal effect of oxidation and pickling composite algorithm is then more preferably.CN101219396A adopts nothing
Machine acid and organic acid are processed to FCC dead catalyst, the heavy metal partial removal of dead catalyst, specific surface area is increased and living
Property improve.
The rejuvenation method mostly processing step of existing FCC dead catalyst is more complicated above, operates cumbersome, some sides
Method is although relatively easy, but is extremely difficult to preferable effect, and especially the removal efficiency of heavy metal is relatively low.
Content of the invention：
For the problems referred to above, the technical problem to be solved in the present invention is to provide roasting and SiCl4Hybrid reaction catalytic cracking
The rejuvenation method of dead catalyst.
Roasting of the present invention and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst comprises the following steps：(1) will
Catalytic cracking spent catalyst material after fired process and gas phase SiCl4Mixing is reacted, and obtains catalyst product, this
The temperature of charge of catalytic cracking spent catalyst is 250-450 DEG C；
(2) deionized water keeps constant to the pH value that the catalyst product of step (1) gained carries out being washed to filter water,
Process is dried again, and the temperature of dried is 100-350 DEG C, and drying time is 0.25-4 hours, obtains final product resurrection catalyst.
Preferably, gas phase SiCl in described step (1)4It is by the SiCl of liquid4Carry out gasification to be formed, then
It is passed through in the solid phase of catalytic cracking spent catalyst again.
Preferably, SiCl in described step (1)4Mass ratio with the butt of catalytic cracking spent catalyst material
0.05-0.5: 1, the response time is 0.5-40 minutes.
Beneficial effects of the present invention：The drawbacks of it can overcome prior art, using SiCl4Enter with catalytic cracking spent catalyst
The solid hybrid reaction of circulation of qi promoting and washing process, rejuvenation method are fairly simple, flexible operation, the resurrection catalyst content of beary metal of gained
Low, specific surface area is high, and activity stability is good.
Description of the drawings：
For ease of explanation, the present invention is embodied as and accompanying drawing is described in detail by following.
Fig. 1 is the physico-chemical property schematic diagram of catalytic cracking spent catalyst raw material used in each embodiment of the invention；
Fig. 2 is the physico-chemical property schematic diagram of the resurrection catalyst in the present invention obtained by each embodiment；
The resurrection catalyst that Fig. 3 present invention is obtained carries out Catalytic Cracking Performance on small fixed flowing bed-tion reacting device and comments
The physico-chemical property figure of the raw oil used by valency；
Fig. 4 carries out Catalytic Cracking Performance evaluation on small fixed flowing bed-tion reacting device for bringing back to life catalyst in the present invention
Interpretation of result figure.
Specific embodiment：
This specific embodiment is employed the following technical solutions：(1) by the catalytic cracking spent catalyst thing after fired process
Material and gas phase SiCl4Mixing is reacted, and obtains catalyst product, and the temperature of charge of this catalytic cracking spent catalyst is 250-
450℃；
(2) deionized water keeps constant to the pH value that the catalyst product of step (1) gained carries out being washed to filter water,
Process is dried again, and the temperature of dried is 100-350 DEG C, and drying time is 0.25-4 hours, obtains final product resurrection catalyst.
Preferably, gas phase SiCl in described step (1)4It is by the SiCl of liquid4Carry out gasification to be formed, then
It is passed through in the solid phase of catalytic cracking spent catalyst again.
Preferably, SiCl in described step (1)4Mass ratio with the butt of catalytic cracking spent catalyst material
0.05-0.5: 1, the response time is 0.5-40 minutes.
The ultimate principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not restricted to the described embodiments, simply explanation described in above-described embodiment and description this
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Embodiment 1：By the catalytic cracking spent catalyst (400 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, (in this embodiment, catalytic cracking spent catalyst raw material is designated as former agent, and its physical and chemical performance parameter is as shown in Figure 1),
SiCl4Mass ratio with the butt of catalytic cracking spent catalyst is 0.25: 1, and the response time is 10 minutes.By reacted catalysis
Agent sample carries out washing and filtering with 10 times of deionized waters, is then dried process to catalyst sample, and baking temperature is 200
DEG C, drying time is 2 hours, finally must bring back to life catalyst sample, be designated as sample 1.The physico-chemical property of products therefrom is shown in Fig. 2.Fig. 2
In, specific surface area and pore volume are determined using BET method.
Embodiment 2：By the catalytic cracking spent catalyst (350 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, (catalytic cracking spent catalyst raw material is with embodiment 1 in this embodiment) SiCl4Dry with catalytic cracking spent catalyst
The mass ratio of base is 0.35: 1, and the response time is 20 minutes.Reacted catalyst sample is washed with 11 times of deionized waters
Filtration being washed, process being then dried to catalyst sample, baking temperature is 250 DEG C, and drying time is 1.5 hours, finally
Catalyst sample is brought back to life, sample 2 is designated as.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 3：By the catalytic cracking spent catalyst (250 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, (catalytic cracking spent catalyst raw material is with embodiment 1 in this embodiment) SiCl4Dry with catalytic cracking spent catalyst
The mass ratio of base is 0.15: 1, and the response time is 40 minutes.Reacted catalyst sample is washed with 8 times of deionized waters
Filtering, process being then dried to catalyst sample, baking temperature is 150 DEG C, and drying time is 3 hours, must finally 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 the catalytic cracking spent catalyst (450 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, (catalytic cracking spent catalyst raw material is with embodiment 1 in this embodiment) SiCl4Dry with catalytic cracking spent catalyst
The mass ratio of base is 0.05: 1, and the response time is 0.5 minute.Reacted catalyst sample is washed with 5 times of deionized waters
Filtration being washed, process being then dried to catalyst sample, baking temperature is 120 DEG C, and drying time is 4 hours, must finally answer
Catalyst sample living, is designated as sample 4.The physico-chemical property of products therefrom is shown in Fig. 2.
Embodiment 5：By the catalytic cracking spent catalyst (300 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, (catalytic cracking spent catalyst raw material is with embodiment 1 in this embodiment) SiCl4With catalytic cracking spent catalyst butt
Mass ratio be 0.5: 1, the response time be 30 minutes.Reacted catalyst sample is washed with 13 times of deionized waters
Filtering, process being then dried to catalyst sample, baking temperature is 300 DEG C, and drying time is 45 minutes, must finally 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 the catalytic cracking spent catalyst (280 DEG C of temperature of charge) of fired process and gas phase SiCl4Carry out
Hybrid reaction, SiCl4Mass ratio with the butt of catalytic cracking spent catalyst is 0.2: 1, and the response time is 35 minutes.Will reaction
Catalyst sample afterwards carries out washing and filtering with 9 times of deionized waters, is then dried process, baking temperature to catalyst sample
For 350 DEG C, drying time is 15 minutes, finally must bring back to life catalyst sample, be 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 in the catalyst after resurrection,
Ni, V, the content of beary metal such as Ca and Na low, specific surface area and micro anti-active index are significantly improved.
The resurrection catalyst of above-described embodiment gained is carried out catalytic cracking on small fixed flowing bed-tion reacting device
Can evaluate.It is former agent and the mixing (mixed catalyst is labeled as embodiment numbering) for bringing back to life catalyst, its Central Plains to evaluate catalyst
Agent accounts for the 30% of mixed catalyst, brings back to life catalyst and accounts for the 70% of mixed catalyst.Reaction condition is as follows：Reaction temperature is 500
DEG C, oil ratio is 4.0, and mass space velocity is 20h-1；Raw materials used oil nature as shown in figure 3, cracking reaction Evaluation results such as
Shown in Fig. 4.Can be drawn by Fig. 4：Bring back to life catalyst and be applied in catalytic cracking unit the coke yield that can reduce device, while
The yield of gasoline and liquefied gas can be improved.
Claims (3)
1. roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst, it is characterised in that：Described rejuvenation method
Comprise the following steps：(1) by the catalytic cracking spent catalyst material after fired process and gas phase SiCl4Mixing is reacted,
Catalyst product is obtained, the temperature of the material of this catalytic cracking spent catalyst is 250-450 DEG C；
(2) deionized water keeps constant to the pH value that the catalyst product of step (1) gained carries out being washed to filter water, then enters
Row dried, the temperature of dried is 100-350 DEG C, and drying time is 0.25-4 hours, obtains final product resurrection catalyst.
2. roasting according to claim 1 and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst, its feature
It is：Gas phase SiCl in described step (1)4It is by the SiCl of liquid4Carry out gasification to be formed, be then passed through catalysis again and split
Change in the solid phase of dead catalyst.
3. roasting according to claim 1 and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst, its feature
It is：SiCl in described step (1)4With mass ratio 0.05-0.5: 1 of the butt of catalytic cracking spent catalyst material, instead
It is 0.5-40 minutes between seasonable.
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| CN201510178636.XA CN104801353B (en) | 2015-04-15 | 2015-04-15 | Roasting and SiCl4The rejuvenation method of hybrid reaction catalytic cracking spent catalyst |
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| CN112973804A (en) * | 2019-12-12 | 2021-06-18 | 青岛惠城环保科技股份有限公司 | Method for reactivating waste catalytic cracking catalyst |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4784749A (en) * | 1986-05-13 | 1988-11-15 | Mobil Oil Corporation | Cracking/dewaxing |
| CN1035104C (en) * | 1991-11-27 | 1997-06-11 | 中国科学院化工冶金研究所 | Regenerating method for waste molecular sieve cracking catalyzer |
| CN1051029C (en) * | 1995-01-16 | 2000-04-05 | 中国石油化工总公司石油化工科学研究院 | Preparation of rare earth-containing rich silicon ultra stabilization Y-type molecular sieve |
| CN102049315B (en) * | 2009-10-30 | 2013-01-09 | 中国石油化工股份有限公司 | Method for preparing catalytic cracking catalyst |
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Address after: 266500 Huaihe East Road, Qingdao economic and Technological Development Zone, Shandong, China, No. 57, No. Patentee after: QINGDAO HUI CHENG ENVIRONMENTAL TECHNOLOGY Co.,Ltd. Address before: 266500 Huaihe East Road, Qingdao economic and Technological Development Zone, Shandong, China, No. 57, No. Patentee before: QINGDAO HUICHENG PETROCHEMICAL TECHNOLOGY Co.,Ltd. |
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