CN1098130A - A kind of cracking catalyst and preparation method thereof - Google Patents
A kind of cracking catalyst and preparation method thereof Download PDFInfo
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- CN1098130A CN1098130A CN 93109101 CN93109101A CN1098130A CN 1098130 A CN1098130 A CN 1098130A CN 93109101 CN93109101 CN 93109101 CN 93109101 A CN93109101 A CN 93109101A CN 1098130 A CN1098130 A CN 1098130A
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Abstract
A kind of catalytic cracking catalyst that contains the composite aluminum base binding agent, oxide compound, the 5-40m% that is selected from elements such as Sn, Ti, Mg by clay, the composite aluminum base binding agent of 5-40m%, the 0-5m% of 20-80m% are selected from faujusite that lattice constant is 2.432-2.472nm, ZSM-5 zeolite, β zeolite and composition thereof and form.Its preparation method is that clay is mixed making beating with deionized water, adds hcl acidifying, adds pseudo-boehmite, aluminium colloidal sol, zeolite molecular sieve making beating, and drying, washing or roasting promptly get product.This catalyzer all has improvement at aspects such as activity, intensity, gasoline yields, and simultaneously, the coke in the reaction product obviously reduces.
Description
The present invention relates to the cracking catalyst technical field, specifically about a kind of catalytic cracking catalyst that contains the composite aluminum base binding agent and preparation method thereof.
Continuous heaviness, poor qualityization along with catalytically cracked material, and environment friendly system is to the increase day by day of unleaded stop bracket gasoline demand, catalyzer trends towards the ultra-steady Y molecular sieve cracking catalyst development to polymer sieve content, simultaneously, because the change of raw material is heavy, the macromolecular ability of catalytic cracking catalyst cracking has also been proposed new requirement, and the matrix of catalyzer is to wear resisting property, the activity of catalyzer, and selectivity particularly cracking macromole ability very significant effects is arranged.It is that binding agent the fluidized catalytic cracking catalyst wear resistance and the hydrothermal stability that make are all fine that United States Patent (USP) 4010116 proposes with the peptization pseudo-boehmite, and United States Patent (USP) 4325845 thinks that the activated alumina that is made by pseudo-boehmite impels the coke generation easily.Though the peptization pseudo-boehmite has adhesive property and certain activity preferably, but, the employing of the high silica alumina ratio molecular sieve little along with structure cell, that the acid sites number is few, hydrogen transfer activity is low, the add-on of molecular sieve obviously increases in the catalyzer, thereby the viscosifying power requirement to binding agent is higher, and the peptization pseudo-boehmite can not satisfy this requirement fully.Use the better aluminium colloidal sol of adhesive property can improve the wear resisting property (GB2109696, USP4542118) of catalyzer, but be that the support of the catalyst cracking activity of adhesive preparation is low, cracking is macromolecular limited in one's ability with aluminium colloidal sol as the binding agent of cracking catalyst.1979, Filtrol company has mentioned in United States Patent (USP) 4206085 and used two kinds of thin water aluminum oxide of plan that flowing property is different, and was wherein a kind of as binding agent, in order to improve the intensity of catalyzer, another kind of in order to regulate activity of such catalysts.Nineteen eighty-two, Filtrol company proposes in United States Patent (USP) 4325847, adds aluminum oxide in cracking catalyst, can improve the stability of zeolite, in this catalyzer, except that intending thin water aluminum oxide, has also introduced the aluminium source gel of anionization.
The purpose of this invention is to provide a kind of catalytic cracking catalyst that contains the composite aluminum base binding agent and preparation method thereof.The composite aluminum base binding agent that adopts the peptization pseudo-boehmite to combine with aluminium colloidal sol can integrate that the peptization pseudo-boehmite has the characteristics of certain cracking activity and the sol bonded performance of aluminium is good, the few advantage of reaction product generation coke, improves the selectivity of wear resistance, activity and the STRENGTH ON COKE of catalyzer.
The said catalyzer of the present invention is made up of following component:
(1) 20-80m%, the preferably clay of 30-70m%;
(2) 5-40m%, preferably the composite aluminum base binding agent of 10-30m% is (with Al
2O
3Burn base for calculating benchmark);
(3) 0-5m% is selected from the oxide compound of Sn, Ti, Mg, Zr, P, Mn, Cr;
(4) 5-40m%, preferably 10-40m% is selected from faujusite that lattice constant is 2.432-2.472, ZSM-5 zeolite, β zeolite and composition thereof.
Each component concentration of the said catalyzer of the present invention all is meant at 1 hour bright basic content of 800 ℃ of roastings, this Preparation of catalysts method is that clay is mixed making beating with deionized water, add hcl acidifying, add pseudo-boehmite, aluminium colloidal sol, zeolite molecular sieve making beating again, steps such as drying, washing or roasting promptly get the said catalyzer of the present invention, and its preparation process comprises:
(1) according to the proportion of composing of the said catalyzer of the present invention, clay is mixed making beating 25-35 minute with deionized water, added hcl acidifying 0.5-1 hour, added the pseudo-boehmite stirring to pulp 25-35 minute, wherein the add-on of water is that 20-55m% is as the criterion to keep solid content, and the add-on of hydrochloric acid accounts for pseudo-boehmite Al
2O
315～50m% of the base unit weight of burning;
(2) at 50-80 ℃ of aging 0.5-2 hour;
(3) adding aluminium colloidal sol stirred 10-20 minute;
(4) add ground zeolite molecular sieve, continue making beating 25-35 minute;
(5) drying and moulding;
(6) through washing, being drying to obtain product, also can obtain product at 500-700 ℃ of roasting 1-3 hour.
The mixture that the said composite aluminum base binding agent of the present invention is peptization pseudo-boehmite and aluminium colloidal sol, its mixed weight ratio is 9: 1-1: 9, preferably 7: 3-3: 7(is with Al
2O
3Burn base for calculating benchmark).
The said lattice constant of the present invention is the Y zeolite that the faujusite of 2.432-2.472nm is meant REY, REHY, USY, REUSY and various high silica alumina ratios.
The said clay of the present invention is meant that kaolin, wilkinite, rectorite leng, sepiolite etc. can be used as the various clays of support of the catalyst.
The present invention compared with prior art has following advantage:
1, the said catalytic cracking catalyst that contains the composite aluminum base binding agent of the present invention, the catalyzer that it is binding agent that its wear resisting property is better than with single peptization pseudo-boehmite is 2.0-2.5% hour as the abrasion index of catalyzer of the present invention
-1, the latter is 2.5-5.0% hour
-1; When carrying out cracking reaction, the former makes moderate progress than the latter's coke selectivity.
2, the activity of such catalysts of the present invention catalyzer that to be better than with single aluminium colloidal sol be binding agent, when carrying out cracking reaction, under the identical situation of catalystoil ratio, the productive rate of gasoline the former than the high 2-5 of the latter percentage point, heavy oil conversion performance improves 1-3 percentage point.
The following examples will the invention will be further described.
(1) the used analysis test method of the present invention:
1, Na
2O content: measure with flame atomic absorption spectrometry.
2, Fe content: atomic absorption spectrometry.
3, RE
2O
3Content: XRF spectrometry.
4, the catalyst abrasion exponential is measured: with a certain amount of catalyzer, put into the abrasion index determinator, under constant gas, blew mill 5 hours, except that first hour, the fine powder less than 15 microns that the back was produced in four hours accounts for sample is called catalyzer greater than the weight percentage of 15 microns catalyzer wear rate, claim abrasion index again, unit is % hour
1
(2) the used places of origin of raw materials and specification in the example of the present invention:
1, kaolin: the Suzhou machine selects 2#, and china clay company in Suzhou produces.
2, hydrochloric acid: chemical pure, Beijing chemical reagent two factories.
Technical pure, Beijing Organic Chemical Plant.
3, pseudo-boehmite: Shandong Aluminum Plant, wherein β three water Al
2O
3＜5m%.
4, aluminium colloidal sol: Zhou village catalyst plant, Al
2O
3Content is 21.5-23.5m%, Al/Cl(m) is 1.15-1.25, and Fe content is 0.025-0.07m%.
5, NH
4Y molecular sieve: the Zhou village catalyst plant is that a kind of lattice constant is the high silicon Y molecular sieve of 2.450nm.
6, REY molecular sieve: Zhou village catalyst plant, lattice constant are 2.470nm, RE
2O
318.0m%, Na
2O 1.6m%.
7, ZSM-5 molecular sieve: the Zhou village catalyst plant is produced, SiO
2/ Al
2O
3＞50, Na
2O＜0.1m%.
Example 1-2
Get 56.3 gram kaolin, add deionized water and mix the half an hour of pulling an oar for 110 milliliters, add 2.5 milliliters of acidifyings of HCl and pull an oar half an hour, add and contain 13 gram Al
2O
3Pseudo-boehmite stir half an hour, 55 ± 5 ℃ aging 2 hours, add and contain 5.7 gram Al
2O
3Aluminium colloidal sol stirred 15 minutes, add 25 grams ground, lattice constant is that (this molecular sieve is by high silicon NH for the REUSY molecular sieve of 2.450nm
4Y molecular sieve is through RECl
3Make its RE after the exchange
2O
33.1m%, Na
2O 1.0m%), continue the half an hour of pulling an oar, transfer to then in the enamel tray of 15cm * 30cm, place 110 ℃ of baking oven inner dryings, dried sample is through pulverizing, get 20-40 order particle, promptly getting sample 1 in 1 hour through 600 ℃ of roastings, and the composition proportioning of this catalyzer sees Table 1.
The preparation method of sample 2 is with example 1, and it is formed proportioning and sees Table 1.
Comparative Examples 1
Get 56.3 gram kaolin, add 170 milliliters of deionized waters and mix making beating half an hour, adds 3 milliliters of hcl acidifying half an hour, add and contain 18.7 and restrain Al
2O
3Pseudo-boehmite continue to stir half an hour, be warming up to 55 ± 5 ℃ aging 2 hours, add the ground molecular sieve identical of 25 grams with example 1, continue making beating half an hour, other preparation process promptly get sample A-1 with example 1, its composition proportioning sees Table 1.
Example 3-5
Press the proportioning of sample 3 in the table 1, get 52.5 gram kaolin, add 100 milliliters of deionized waters, mix making beating 0.5 hour, added 2 milliliters of hcl acidifyings 0.5 hour, add and contain 5.3 gram Al
2O
3Pseudo-boehmite stir half an hour, 55 ± 5 ℃ aging 2 hours, add again and contain 12.2 gram Al
2O
3Aluminium colloidal sol stirred 15 minutes, add the molecular sieve of the ground same example 1 of 30 grams then, other preparation process promptly gets sample 3 with example 1.The preparation process of sample 4,5 is the proportioning difference with example 3, and it is formed proportioning and sees Table 1.
Comparative Examples 2
Press the proportioning of sample B in the table 1, get 52.5 the gram kaolin, join while stirring contain 17.5 the gram Al
2O
3Aluminium colloidal sol in, stirring to pulp 1 hour adds then with the molecular sieve of example 1 and continues making beating 0.5 hour, other preparation process promptly gets sample B with example 1.
Annotate: 1, the total Al of *
2O
3M% is with Al
2O
3Bright base for calculating benchmark, down with.
2, * * pseudo-boehmite: aluminium colloidal sol is weight ratio, down together.
3, each components contents of catalyzer is meant at 1 hour bright basic content of 800 ℃ of roastings in the table, down together.
Example 6
With catalyst sample 1,2 of the present invention and Comparative Examples 1 sample A-1, behind 800 ℃, 4 hours, 100% hydrothermal treatment consists, on MAT-II type heavy oil microreactor, estimate, stock oil is 227-478 ℃ triumph wax oil, 482 ℃ of temperature of reaction, catalystoil ratio=3.5 of sample 1,2, catalystoil ratio=3 of Comparative Examples 1 sample A-1 the results are shown in table 2.
As can be seen from Table 2, the catalyst sample 1 that the present invention is said to contain the composite aluminum base binding agent and 2 is a binding agent with single peptization pseudo-boehmite, and sample A-1 compares, under the close situation of transformation efficiency, the selectivity of the former coke is 3.09-3.15%, and the latter reaches 4.0%, illustrates that the former obviously reduces than the coke that the latter produces.
Example 7
Catalyst sample 4,5 of the present invention and Comparative Examples 2 sample B after handle down 800 ℃, 4 hours, 100% water vapour, are estimated on MAT-II type heavy oil microreactor, and stock oil and temperature of reaction are with example 6, and catalystoil ratio=6 the results are shown in Table 3.
As can be seen from Table 3: the catalyst sample 4,5 that the present invention is said to contain the composite aluminum base binding agent is compared with the sample B that single aluminium colloidal sol is binding agent, under the identical situation of catalystoil ratio, the former increases 2-5 percentage point than the latter gasoline yield, and heavy oil conversion performance improves 1-3 percentage point.
Example 8-9
Press the proportioning of sample 6 in the table 4,8.8 kilograms of kaolin are joined in 17 kilograms of deionized waters, stirring to pulp 1 hour adds 0.7 kilogram of technical-grade hydrochloric acid and stirs acidifying 0.5 hour, adds and contains 2.6 kilograms of Al
2O
3Pseudo-boehmite making beating 0.5 hour, be warming up to 60 ± 5 ℃ aging 1 hour, add and contain 0.3 kilogram of Al
2O
3Aluminium colloidal sol making beating 0.5 hour, add 3.3 kilograms of ground REY molecular sieves again, intermittently pulled an oar 0.5 hour, spray drying forming through washing, drying, promptly gets sample 6.
The preparation method of sample 7 is with sample 6, and it is formed proportioning and sees Table 4.
Comparative Examples 3-4
Press the proportioning of sample A-2 in the table 4,8.8 kilograms of kaolin are joined in 27 kilograms of deionized waters making beating 1 hour, adds 0.6 kilogram of technical-grade hydrochloric acid and stir acidifying half an hour, adding contains 2.9 kilograms of Al
2O
3Pseudo-boehmite, continue making beating 0.5 hour, be warming up to 60 ± 5 ℃, aging 1 hour, add 3.3 kilograms ground, with the molecular sieve of example 8, continue making beating 0.5 hour, spray drying forming through washing drying, promptly gets sample A-2 then, the same A-2 of preparation method of the sample A-3 of Comparative Examples 4, it is formed proportioning and sees Table 4.
As can be seen from Table 4, the said abrasion index that contains the catalyst sample 6,7 of composite aluminum base binding agent of the present invention is 2.0-2.2% hour
-1, be 2.5-3.0% hour with single peptization pseudo-boehmite sample A-2 that is binding agent and the abrasion index of A-3
-1, illustrate that the composite aluminum base binding agent has improved the intensity of catalyzer.
Example 10-11
Press the proportioning of sample 8 in the table 5,7.9 kilograms of kaolin are joined in 15 kilograms of deionized waters pulled an oar 1 hour, add 0.35 kilogram of technical-grade hydrochloric acid, stir acidifying 0.5 hour, add and contain 1.3 kilograms of Al
2O
3Pseudo-boehmite, continue making beating 0.5 hour, be warming up to 60 ℃, aging 1 hour, add and contain 1.3 kilograms of Al
2O
3Aluminium colloidal sol, continue making beating 0.5 hour, add 4.5 kilograms of ground molecular sieves (this molecular sieve is the mixture of REY and ZSM-5, and its mixed weight ratio is 6: 1) then, pulled an oar 0.5 hour, spray drying forming, through wash, drying, promptly get sample 8.The preparation method of sample 9 is with sample 8, and it is formed proportioning and sees Table 5.
Comparative Examples 5
Press the proportioning of sample A-4 in the table 5,7.9 kilograms of kaolin are joined in 24 kilograms of deionized waters, pulled an oar 1 hour, add 0.6 kilogram of technical-grade hydrochloric acid acidifying 0.5 hour, add and contain 2.6 kilograms of Al
2O
3Pseudo-boehmite, continue making beating 0.5 hour, be warming up to 60 ℃, aging 1 hour, adds the molecular sieve making beating 0.5 hour of 4.5 kilograms of ground same examples 10, spray drying forming, through wash, drying, promptly get sample A-4.
As can be seen from Table 5: the said abrasion index that contains the catalyst sample 8,9 of composite aluminum base binding agent of the present invention is 1.8-2.2% hour
-1, and reach 4.0% hour with the abrasion index of the single peptization pseudo-boehmite sample A-4 that is binding agent
-1, catalyzer of the present invention is described, the catalyzer that it is binding agent that its wear resisting property is better than with single peptization pseudo-boehmite.
Claims (9)
1, a kind of catalytic cracking catalyst is characterized in that this catalyzer is that composite aluminum base binding agent by the clay of 20-80m%, 5-40m% is (with Al
2O
3Burn base for calculating benchmark), 0-5m% is selected from the oxide compound of Sn, Ti, Mg, Zr, P, Mn, Cr and 5-40m% and is selected from faujusite that lattice constant is 2.432-2.472nm, ZSM-5 zeolite, β zeolite and composition thereof and forms.
2,, it is characterized in that this catalyzer contains the clay of 30-70m% according to the said catalyzer of claim 1.
3,, it is characterized in that this catalyzer contains the composite aluminum base binding agent of 10-30m% according to the said catalyzer of claim 1.
4,, it is characterized in that this catalyzer contains 10-40m% and is selected from faujusite that lattice constant is 2.432-2.472nm, ZSM-5 zeolite, β zeolite and composition thereof according to the said catalyzer of claim 1.
5, according to claim 1 or 3 said catalyzer, it is characterized in that said composite aluminum base binding agent is the mixture of peptization pseudo-boehmite and aluminium colloidal sol, its mixed weight ratio is with Al
2O
3The base that burns is 9 for calculating benchmark: 1-1: 9.
6, according to the said catalyzer of claim 5, it is characterized in that said composite aluminum base binding agent is the mixture of peptization pseudo-boehmite and aluminium colloidal sol, its mixed weight ratio is with Al
2O
3The base that burns is 7 for calculating benchmark: 3-3: 7.
7,, it is characterized in that said lattice constant is the Y zeolite that the faujusite of 2.432-2.472nm is meant REY, REHY, USY, REUSY and various high silica alumina ratios according to claim 1 or 4 said catalyzer.
8, the said Preparation of catalysts method of claim 1 is characterized in that:
(1) according to the proportion of composing of the said catalyzer of claim 1, clay is mixed making beating 25-35 minute with deionized water, added hcl acidifying 0.5-1 hour, added the pseudo-boehmite stirring to pulp 25-35 minute, wherein the add-on of water is that 20-55m% is as the criterion to keep solid content, and the add-on of hydrochloric acid accounts for Al in the pseudo-boehmite
2O
315～50m% of the base unit weight of burning;
(2) at 50-80 ℃ of aging 0.5-2 hour;
(3) adding aluminium colloidal sol stirred 10-20 minute;
(4) add ground zeolite molecular sieve, continue making beating 25-35 minute;
(5) drying and moulding;
(6) through washing, be drying to obtain product.
9, said according to Claim 8 preparation method is characterized in that (6) money was promptly to get product at 500-700 ℃ of roasting 1-3 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93109101A CN1034718C (en) | 1993-07-29 | 1993-07-29 | Cracking catalyst and preparing process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93109101A CN1034718C (en) | 1993-07-29 | 1993-07-29 | Cracking catalyst and preparing process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1098130A true CN1098130A (en) | 1995-02-01 |
| CN1034718C CN1034718C (en) | 1997-04-30 |
Family
ID=4987455
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|---|---|---|---|
| CN93109101A Expired - Lifetime CN1034718C (en) | 1993-07-29 | 1993-07-29 | Cracking catalyst and preparing process thereof |
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| CN1055301C (en) * | 1996-02-08 | 2000-08-09 | 中国石油化工总公司 | Cracking catalyst for producing isomeric olefine and gasoline with high yield |
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| CN1072030C (en) * | 1997-11-11 | 2001-10-03 | 中国石油化工总公司 | Phosphorus-contained octahedro zeolite hydrocarbons cracking catalyst and preparation method therefor |
| CN1081218C (en) * | 1998-09-17 | 2002-03-20 | 中国石油化工集团公司 | Preparation of petroleum cracking catalyst |
| CN1081219C (en) * | 1998-09-03 | 2002-03-20 | 中国石油化工集团公司 | Process for preparing catalyst for catalytic cracking |
| CN1100846C (en) * | 1999-07-10 | 2003-02-05 | 巴陵石化长岭炼油化工总厂 | Cracking catalyst and its preparing process |
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| US4206085A (en) * | 1979-01-15 | 1980-06-03 | Filtrol Corporation | Balanced alumina matrix in zeolite containing catalyst |
| US4325847A (en) * | 1980-06-19 | 1982-04-20 | Filtrol Corporation | Use of additional alumina for extra zeolite stability in FCC catalyst |
| US4542118A (en) * | 1984-02-02 | 1985-09-17 | W. R. Grace & Co. | Catalyst manufacture |
| US4987110A (en) * | 1987-05-07 | 1991-01-22 | Union Oil Company Of California | Attrition resistant cracking catalyst |
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