CN1194072C - RE-containing Si-base partially-synthesized hydrocarbon converting catalyst - Google Patents
RE-containing Si-base partially-synthesized hydrocarbon converting catalyst Download PDFInfo
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- CN1194072C CN1194072C CNB021534187A CN02153418A CN1194072C CN 1194072 C CN1194072 C CN 1194072C CN B021534187 A CNB021534187 A CN B021534187A CN 02153418 A CN02153418 A CN 02153418A CN 1194072 C CN1194072 C CN 1194072C
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- molecular sieve
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Abstract
The present invention relates to a silicon based semi-synthesized hydrocarbon converting catalyst with rare earth. The present invention is characterized in that the hydrocarbon converting catalyst is made by silica sol binding agents with 0.1 to 20% of rare earth salts (rare earth oxides), natural aluminium silicate slime and artificially synthesized molecular sieves. The catalyst of the present invention utilizes rare earth activation silicon oxide, and thereby, the present invention enhances the heavy oil cracking activity and the anti heavy metal pollution capability, and lowers the contents of catalytically cracked gasoline alkene and sulfur.
Description
Technical field
The invention belongs to hydrocarbon cracking catalyzer, more particularly, is a kind of semisynthetic hydrocarbon cracking catalyzer of silicon sol that contains rare earth.
Background technology
Oil is irreplaceable transport fuel, and petroleum resources are limited, therefore develops the heavy oil degree of depth and transforms, and increases light-end products, will be the significant development strategy of 21st century oil refining industry.Product yield, quality and the economic target etc. of heavy oil degree of depth conversion process are all closely related with catalyst performance.The cracking catalyst that relevant heavy oil deep processing is used, China has carried out a large amount of research and development.The cracking catalyst that the heavy oil deep processing is used has multiple by the solid support material classification.Silicon sol is the silica-based semi-synthetic Hydrocarban coversion catalysts of binding agent, and except that binding agent, carrier also comprises specific natural rich hole silicate minerals material; Molecular sieve then is the very flourishing synthetic crystallization catalytic material of active surface, is the main active element of catalyzer.With sial base or alumina-base material is that the semi-synthetic Hydrocarban coversion catalysts material of binding agent is compared, and silicon sol has the relatively low advantage of cost, widely accepts industrial.Yet, concerning the heavy hydrocarbon conversion, its molecular dimension is big, to silicon sol as molecular sieve catalyst carrier integral part, it has been cohesive action, because its non-activity certainly heavy oil molecules is not had the cracking ability, and molecular sieve is because of intrinsic pore structure, having limited the macromole hydrocarbon enters, can't therefore provide the aperture bigger support of the catalyst directly near the active internal surface that molecular sieve provided, just very necessary to improve the catalyzer heavy oil cracking ability.
In addition, also have the application of rare earth in catalytic cracking catalyst, people have done extensive and deep research.Rare earth has increased the acid active centre of catalyzer as the composition of catalyzer, has improved the cracking activity of molecular sieve catalyst, has also improved active stability, thereby improves the heavy oil hydrocarbon conversion activity and the selectivity of catalyzer; Rare earth is again the functional component of catalyzer preventing from heavy metal pollution, because rare earth oxide and vanadic anhydride are under catalytic cracking condition, can form resistant to elevated temperatures vanadate, prevented that vanadium from moving on the molecular sieve lattice, the crystalline structure of unlikely saboteur's sieve, simultaneously, rare earth oxide combines with nickel oxide, can prevent the formation of metallic nickel, passivation the dehydrogenation green coke ability of nickel, this and V that rare earth had and Ni bonded ability help improving the preventing from heavy metal pollution performance of molecular sieve catalyst for heavy oil catalytic cracking, distribute thereby improve product.In the recent period, people require to use clean fuel in order to protect environment, and market presses for the cracking catalyst that can reduce alkene and sulphur content in the catalytically cracked gasoline, and the research of using rare earth in this respect also has a large amount of reports.
CN1284403A is a kind of improved rare earth Y type zeolite and preparation method thereof: CN1330981A is about a kind of P-contained Y-zeolite and preparation method thereof.In these two kinds of prepare zeolite methods, all useful silicon solution, it mainly is the process of two kinds of zeolites of silicon sol dipping, purpose is in the hydrothermal treatment consists process, the part Siliciumatom can migrate in the hole of y-type zeolite dealuminzation formation, zeolite is mended silicon, make skeleton structure of zeolite avoid destroying, keep the degree of crystallinity of zeolite.Catalyzer with these two kinds of zeolite preparations has stronger heavy oil conversion performance and better products distribution.
Disclose a kind of composite aluminum base binding agent in the CN1098130A patent application, this binding agent has improved the wear resistance and the coke selectivity of semi-synthetic carrier cracking catalyst.
CN1143666A reports a kind of voluminous isomeric olefine of rare-earth five-membered ring supersiliceous zeolite and cracking catalyst of gasoline of containing.When vanadiumcontent in the stock oil was 5.2ppm, the productive rate of isomeric olefine and gasoline was still very high.
USP5173174 is fluid catalytic cracking (FCC) catalyzer about a kind of anti-vanadium and nickel.Catalyzer is made up of molecular sieve, macropore boehmite and aluminum oxide and rare earth component.This catalyst formulation has reduced sedimentary Ni and V to catalyst activity and harmful effect optionally.
CN1353086A is with ammonium ion and rare earth ion exchanged NaY molecular sieve, and hydrothermal calcine, then with the phosphide reaction, in conjunction with the P of last 0.2-10% (W)
2O
5, carry out hydrothermal calcine again.The Y zeolite of this method preparation can significantly reduce the olefin(e) centent of FCC gasoline, and keep good coke selectivity.
Summary of the invention
The purpose of this invention is to provide the rare earth-activated silicon oxide of a kind of employing, improve the heavy oil cracking activity of silica-based semi-synthetic carrier and cracking catalyst optionally.
Composition and the content (is 100 in composition weight sum) that contains the silica-based semi-synthetic Hydrocarban coversion catalysts of rare earth of the present invention:
Containing rare earth salts (in rare earth oxide REO) is the molecular sieve 1-60% of 0.1-20% acidic silicasol 10-50%, natural aluminium silicate clay 1-80% and synthetic.
The rare earth salts siloxane solvent that contains of the present invention, be to be 2.5-3.5 water glass and to contain rare earth salts and the mixture of acid with modulus, making PH is the acidic silicasol of the rear earth containing of 0.5-3.0 (best 1.0-3.0), and silicon sol middle-weight rare earths salt (in REO) optimum content is 1.0-10%.Described rare earth salts is meant a kind of, two or more the solubility salt in the group of the lanthanides non radioactive element, comprises the nitrate of rare earth, muriate or its mixture of rare earth.Acid in the mixing of described rare earth salts and acid comprises a kind of, two or more the mixture in nitric acid, sulfuric acid, the hydrochloric acid.
Aluminum silicate clay of the present invention comprises natural aluminium silicate clay that the cracking catalyst of kaolin, halloysite, wilkinite, illiteracy bentonite, sepiolite is commonly used or a kind of, two or more mixture in their artificial highly finished product, and its optimal addn is 10-70%.
Synthetic molecular sieve of the present invention comprises a kind of, two or more the mixture of the molecular sieve that molecular sieve, L with faujusite structure zeolite structured molecular sieve, the molecular sieve of mordenite structure, ZSM-5 are zeolite structured, and its optimal addn is 5-50%.
Preparation of catalysts method of the present invention comprises following process: be that 2.5-3.5 contains SiO with modulus earlier
2Water glass for 2-20%, to be mixed into PH be 0.5-3.0, contain the acidic silicasol that REO is 0.1-20% with containing rare earth salts and mineral acid, acidic silicasol again with natural aluminium silicate clay, synthetic molecular sieve mixing making beating, spray drying forming, wash, be drying to obtain catalyst prod.
Advantage of the present invention and effect:
Key problem in technology of the present invention is to utilize rare earth to come active oxidation silicon, improves the activity and the selectivity of the heavy oil cracking of silica-based semi-synthetic carrier.The present invention joins water glass in earth solution and the sour mixed solution to form the acidic silicasol that contains rare earth, and the rare earth constituent element of adding is disperseed at the carrier camber, allows rare earth oxide and silicon-dioxide form certain chemical framework on the catalyst base.The rare earth constituent element of silicon-dioxide high dispersing, to change the insufficient situation of the semi-synthetic carrier heavy oil cracking ability of silicon sol, improve the heavy oil cracking activity of the semi-synthetic carrier of silicon sol effectively, transformation efficiency improves 1.9-2.3%, and improve molecular sieve catalyst for cracking heavy oil preventing from heavy metal pollution ability, change product and distribute.Simultaneously, be accompanied by the raising of catalyzer cracking activity, this catalyzer reduces the effect of olefins in FCC gasoline and sulphur content in addition, reduces 2-8 percentage point of gasoline olefin, and content of sulfur in gasoline reduces 5-15%.
Embodiment
Further specify characteristics of the present invention below by specific examples:
Example 1
To contain 5%SiO
2Modulus be 3.22 water glass 110.8L and contain 31.0gRECl
3/ L concentration is 10% H
2SO
415.9L thorough mixing becomes PH=2 to contain the silicon sol of rare earth, again with contain 54% kaolin slurry 21.3L, and contain 34%USY (super steady Y) molecular sieve pulp 21.6L, be mixed into glue, be spray dried to microspheroidal, Na is removed in washing then
+, SO
4 =, CL
-, drying, the highly active semisynthetic hydrocarbon cracking catalyzer A that contains 20% silicon sol (wherein containing 5% rare earth), 30% super-stable Y molecular sieves.
Example 2
This example is a reference example 1, is that a kind of usefulness does not contain the catalyzer that the silicon sol of rare earth makes.Concrete preparation process:
To contain 5%SiO
2Modulus be 3.22 water glass 118.5L and contain 10%H
2SO
416.6L thorough mixing becomes not contain the silicon sol of rare earth, again with contain 54% kaolinic slurries 21.3L, contain 34%USY molecular sieve pulp 21.6L, be mixed into glue, be spray dried to microspheroidal, Na is removed in washing again
+, SO
4 =, drying, promptly do not contained rare earth 20% conventional silicon sol, contain semisynthetic hydrocarbon cracking catalyzer (reference agent) B of 30% super-stable Y molecular sieves.
Example 3
To contain 8%SiO
2Modulus be 3.22 water glass 70.8L and contain 59gRECl
3/ L concentration is 10% H
2SO
416.5L thorough mixing becomes the silicon sol that contains rare earth of PH=2.4, contains 54% kaolin slurry with 25.5L again, and contain 20%REHY (rare earth hydrogen Y) molecular sieve liquid and be mixed into glue, spray-dried one-tenth microspheroidal, Na is removed in washing then
+, SO
4 =, CL
-, drying, highly actively contain 20% silicon sol (wherein containing 1% rare earth), contain the semisynthetic hydrocarbon cracking catalyzer C of 20% rare earth hydrogen Y zeolite.
Example 4
To contain 10%SiO
2Modulus be 3.0 water glass 35.8L
With contain 36.9gRECl
3The solution 30.9L concentration of/L is 6% HNO
3Thorough mixing becomes PH=2.6 to contain the silicon sol of rare earth, contains 54% kaolin slurry with 23.4L again, and contain 32%REHY molecular sieve liquid and be mixed into glue, spray-dried one-tenth microspheroidal, Na is removed in washing then
+, SO
4 =, CL
-, dry again, highly actively contain 15% silicon sol (wherein containing 1% rare earth), contain the semisynthetic hydrocarbon cracking catalyzer D of 30% rare earth superstable Y-type molecular sieve.
Example 5
This example is a reference example 2, is the catalyzer that a kind of silicon sol that does not contain rare earth makes.Concrete preparation process:
To contain 10%SiO
2Modulus be 3.0 water glass 42.0L and 6% H
2SO
4Solution 36.3L thorough mixing becomes not contain the silicon sol of the PH=2.5 of rare earth, and contain 54% kaolin slurry 23.3L with 23.4L again, contain 32%REUSY (hyperastable Y-type RE) molecular sieve liquid and be mixed into glue, spray-dried one-tenth microspheroidal, Na is removed in washing then
+, NO
3 -, drying, do not contain rare earth 15% silicon sol, contain the semisynthetic hydrocarbon cracking catalyzer E of rare earth 30% rare earth superstable Y-type molecular sieve.
Example 6
To contain 20%SiO
2Modulus be 2.8 water glass 22.2L and contain 173gRECl
3/ L concentration is the silicon sol that 3% HCL52.0L thorough mixing becomes to contain rare earth, contains 54% kaolin slurry with 17.7L again, and 28.7L contains 32%REUSY and becomes glue with the mixed molecular sieve slurries of ZSM-5, and spray-dried one-tenth microspheroidal is washed then, removes Na
+, CL
-, drying, the highly active semisynthetic hydrocarbon cracking catalyzer F that contains 20% silicon sol (wherein containing 10% rare earth), contains 35%REUSY type molecular sieve and 2%ZSM-5 molecular sieve.
Example 7
To contain 6%SiO
2Modulus be that 3.1 water glass 74.4L and 18.7L contain 58.8gRE (NO
3)
3/ L concentration is 9% NHO
3Thorough mixing becomes to contain the silicon sol of rare earth, contains 54% kaolin with 22.7L again, and 7.8L contains 25%REHY and USY mixed molecular sieve liquid is mixed into glue, spray-dried one-tenth microspheroidal, and Na is removed in washing then
+, NO
3 -, drying, promptly make contain 18% silicon sol (wherein containing 15% rare earth), contain 10% rare earth hydrogen Y zeolite, the semisynthetic hydrocarbon cracking catalyzer G of 17% super-stable Y molecular sieves.
Example 8
To contain 15%SiO
2Modulus be 3.3 water glass 77.8L and contain 68.0gRECl
3/ L concentration is 15% HCL16.0L, and thorough mixing becomes to contain the silicon sol of rare earth, contains 54% kaolin slurry with 7.2L again, and 33.7L contains 26.9%REUSY molecular sieve liquid and is mixed into glue, spray-dried one-tenth microspheroidal, and Na is removed in washing then
+, CL
-, drying is promptly made and is contained 42% silicon sol (wherein containing 5% rare earth), contains the semisynthetic hydrocarbon cracking catalyzer H of 40% rare earth superstable Y-type molecular sieve.
Example 9
This example is the hydrocarbon cracking catalyzer A of the present invention of example 1 and example 4 and the application example of D, and compares with example 2 and example 5 reference agent B and E.
Experiment is to carry out the cracking reaction evaluation on small fixed flowing bed.Experimental technique: catalyzer is deposited on 3000ppmNi and 4000ppmV respectively, under 813 ℃ of temperature, normal pressure, 90% water vapor, 10% air conditions, hydro-thermal is urged and being worn out after 5 hours, carries out catalytic cracking reaction, contrasts the ability that its cracking performance and an anti-huge sum of money pollute.Stock oil character and reaction conditions see Table 1, and evaluation result sees Table 2.As shown in Table 2, the catalyzer of the present invention's preparation is compared stock oil with the reference agent transformation efficiency exceeds 1.9 and 2.3 units, and the activity of conversion height reduces 2-8 unit of gasoline olefin, and sulfur in gasoline content reduces 5-15%.
Table 1
| Stock oil character | |
| Density (20 °), g/cm 3 | 0.9221 |
| Viscosity (80 °), mm 2/S | 36.74 |
| Carbon residue, m% | 5.1 |
| S content, m% | 0.53 |
| Reaction conditions | |
| Temperature of reaction, ℃ | 510 |
| Agent: oil ratio (quality) | 3 |
| Weight hourly space velocity | 20 |
Table 2
| Catalyzer | A | B | D | E | ||
| Chemical constitution % | AL 2O 3 | 27.8 | 27.8 | 31.2 | 31.2 | |
| Na 2O | 0.17 | 0.17 | 0.13 | 0.14 | ||
| RE 2O 3 | 1.0 | 3.3 | 1.0 | |||
| Specific surface, m 2/g | 213 | 202 | 220 | 211 | ||
| Pore volume, ml/g | 0.31 | 0.31 | 0.33 | 0.33 | ||
| MAT | 73 | 71 | 76 | 73 | ||
| Pollution metal, ppm | Ni | 2930 | 2920 | 2900 | 2990 | |
| V | 4030 | 4030 | 3980 | 3980 | ||
| The preventing from heavy metal reaction evaluating | Transformation efficiency, % | 55.7 | 53.8 | 59.9 | 57.6 | |
| Gasoline, % | 38.6 | 37.8 | 41.1 | 39.5 | ||
| Diesel oil, % | 25.1 | 25.2 | 26.0 | 25.7 | ||
| Liquefied gas, % | 11.3 | 10.4 | 12.8 | 11.9 | ||
| Coke, % | 3.4 | 3.7 | 3.7 | 4.0 | ||
| ＜C2，％ | 1.8 | 1.9 | 2.0 | 2.2 | ||
| Heavy oil, % | 19.8 | 21.0 | 14.1 | 16.7 | ||
| Gasoline property | Alkene, % | 32.3 | 38.6 | 27.5 | 35.9 | |
| S，ppm | 450 | 510 | 420 | 490 | ||
Claims (6)
1. silica-based semi-synthetic Hydrocarban coversion catalysts that contains rare earth, it is characterized in that making by following method: be that 2.5-3.5 contains SiO with modulus earlier with containing rare earth salts with silicon sol 10-50%, natural silicate clay 1-80% and synthetic molecular sieve 1-60% that REO counts 0.1-20%
2Water glass for 2-20%, to be mixed into PH be 0.5-3.0, contain the acidic silicasol that REO is 0.1-20% with containing rare earth salts and mineral acid, acidic silicasol again with molecular sieve mixing making beating, the spray drying forming of natural aluminium silicate clay, synthetic, wash, be drying to obtain catalyst prod.
2. according to the described catalyzer of claim 1, it is characterized in that the described silicon sol that contains rare earth salts, be to be that the PH that the mixture of the water glass of 2.5-3.5 and rare earth salts and acid is made is the acidic silicasol of 0.5-3.0 with modulus, described rare earth salts is the nitrate that comprises rare earth of the solubility salt in the group of the lanthanides radioelement, muriate or its mixture of rare earth, and described acid comprises a kind of, two or more the mixture in nitric acid, sulfuric acid or the hydrochloric acid.
3. according to the described catalyzer of claim 1, the rare earth salts of its feature in silicon sol is 1.0-10% in the content of REO.
4. according to the described catalyzer of claim 2, the PH that it is characterized in that described silicon sol is 1.0-3.0.
5. according to the described catalyzer of claim 1, it is characterized in that described natural aluminium silicate clay comprises the natural aluminium silicate clay of kaolin, halloysite, wilkinite, illiteracy bentonite, sepiolite or a kind of, two or more mixture in their artificial highly finished product, its add-on is 10-70%.
6. according to the described catalyzer of claim 1, it is characterized in that described synthetic molecular sieve comprises a kind of, two or more the mixture of the molecular sieve that molecular sieve, L with faujusite structure zeolite structured molecular sieve, the molecular sieve of mordenite structure, ZSM-5 are zeolite structured, its add-on is 5-50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021534187A CN1194072C (en) | 2002-11-27 | 2002-11-27 | RE-containing Si-base partially-synthesized hydrocarbon converting catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021534187A CN1194072C (en) | 2002-11-27 | 2002-11-27 | RE-containing Si-base partially-synthesized hydrocarbon converting catalyst |
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|---|---|
| CN1417297A CN1417297A (en) | 2003-05-14 |
| CN1194072C true CN1194072C (en) | 2005-03-23 |
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|---|---|---|---|
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100338188C (en) * | 2003-08-20 | 2007-09-19 | 中国石油化工股份有限公司 | Desulfurizer for decreasing sulfur content of gasoline |
| CN101450321B (en) * | 2007-11-28 | 2011-02-09 | 中国石油化工股份有限公司石油化工科学研究院 | Catalytic cracking auxiliary agent capable of increasing propylene in yield |
| CN101455977B (en) * | 2007-12-13 | 2010-11-24 | 中国石油化工股份有限公司 | Preparation method of silicon-containing cracking catalyst |
| RU2548362C2 (en) | 2009-06-25 | 2015-04-20 | Чайна Петролеум & Кемикал Корпорейшн | Catalyst for catalytic cracking and method of increasing catalyst selectivity (versions) |
| CN105728022A (en) * | 2014-12-10 | 2016-07-06 | 中国石油天然气股份有限公司 | A preparing method of a catalytic cracking catalyst containing a silica sol binder |
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2002
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