CN1388213A - Prepn of petroleum hydrocarbon cracking catalyst - Google Patents
Prepn of petroleum hydrocarbon cracking catalyst Download PDFInfo
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- CN1388213A CN1388213A CN 01118437 CN01118437A CN1388213A CN 1388213 A CN1388213 A CN 1388213A CN 01118437 CN01118437 CN 01118437 CN 01118437 A CN01118437 A CN 01118437A CN 1388213 A CN1388213 A CN 1388213A
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Abstract
The preparation of petroleum hydrocarbon cracking catalyst incldues acid treatment of clay slurry, addition of pseudo-thin diasphore and water glass solution, addition (no) aluminium sol, addition of molecular sieve slurry, spray drying and water washing. The preparation process is suitable for molecualr sieve catalyst containing Si-Al matrix and has short technological process and low production cost.
Description
The invention relates to a kind of catalytic cracking of petroleum hydrocarbon Preparation of catalysts method, further say so about a kind of preparation method of cracking catalyst for petroleum hydrocarbon of sial matrix.
Since the eighties, catalytic cracking is developed to slag oil cracking by the wax oil cracking, and slag-mixing amount increases year by year.Contain in the residual oil such as colloid, bituminous matter at interior macromolecular substance, they can not enter in the molecular sieve inner duct of catalyzer because molecular diameter is excessive carries out cracking reaction, the cracking of this part material, as only leaning on the outside surface of molecular sieve, its transformation efficiency is very limited, because the outer surface area of molecular sieve only accounts for below 2% of its total surface area, this has had a strong impact on the reactivity worth of residue cracking catalyst.In order to improve macromolecular cracking, the active centre that needs other, macromole is cut into middle molecule, make it enter cracking again in the molecular sieve pore passage then rapidly, adopt the active matrix of macropore can be used for improving the macromolecular cracking ability of heavy oil, and the introducing of sial matrix components is one of means of using always.
Sial matrix is made of aluminum oxide and silicon oxide, belongs to the amorphous silicon aluminium type.In the prescription of cracking catalyst, introduce the method for sial matrix, a lot of bibliographical informations has been arranged, contain the acid sial catalyzer of gel matrix altogether as all having reported among USP4810369, USP4588702 and the USP4480047; The catalyzer that USP5147836 discloses is with silicon modification bayerite and/or δ-Al
2O
3, kaolin, binding agent and molecular sieve be the component preparation, wherein silicon modification bayerite and/or δ-Al
2O
3Heavily %, kaolin account for the heavy % of 10-60, binding agent accounts for the heavy % of 10-30 to account for 2-40, and molecular sieve accounts for the heavy % of 5-50, and this catalyzer has lower coke and hydrogen yield, and the gasoline of production and diesel oil fuel have water vapor heat-resistant quality preferably; CA2061663 has introduced bayerite and/or the δ-Al with the silicon modification
2O
3The catalytic cracking additive of preparation, this agent can be increased production gasoline and production of diesel oil, reduces coke and hydrogen.
In the prior art, the sial matrix of catalyzer is to be prepared by independent synthesis technique.For example, the method that discloses among the USP5001097 is to be raw material with silicon sol and aluminium salt, regulates pH value less than 4, and its co-precipitation is obtained; The said amorphous silicon aluminium of USP5135641 is that the pH value of the silicate solutions and the aluminate aqueous solution is transferred to 1-4, adds alkali more gradually, and forming pH value is the cogelled body of 5-9, through the intensification slaking, filters the back and obtains; The method that USP4508840 discloses is with siliceous basic solution and contain aluminic acid solution to be mixed to pH value be to obtain behind the 3.0-4.5; The method that USP5074990 and USP5070053 disclose is to do the shell of silicon oxide on the surface of aluminum compound, after the drying roasting as the matrix components of catalyzer; The method of EP238760 and EP228270 is to do the aluminum oxide shell on the surface of silicon compound, after the drying roasting as the catalyst substrates component; Having introduced a kind of substrate material among USP5304526 and the EP537871, is the agent matrix components through the silicon modification; Having introduced a kind of substrate material among USP5304526 and the EP537871, is bayerite and/or δ-Al through the silicon modification
2O
3, its preparation method is under the situation that the magnesium hydroxide crystal seed exists, and reacts after filtration washing acquisition, wherein SiO in pH value during for 10.5-11.5 by sodium aluminate solution, sodium silicate solution and alum liquor
2Content be the heavy % of 0.5-10.
In sum, in the prior art of the catalytic cracking catalyst of preparation sial matrix, need with independent equipment through the good amorphous silicon aluminium of independent process prepared beforehand, and then with other constituent element of catalyzer, as mixing such as clay, molecular sieves, the investment of equipment is increased, and the flow process complexity.
The purpose of this invention is to provide a kind of preparation method who need not to prepare the amorphous silicon aluminium step separately, shortens the sial matrix cracking catalyst for petroleum hydrocarbon of preparation flow.
The preparation method of cracking catalyst for petroleum hydrocarbon provided by the invention adds pseudo-boehmite with clay slurry after with acid treatment, carries out burin-in process, adds water glass solution, after pulling an oar evenly, adds finely dispersed molecular sieve pulp again, spraying drying, washing.
In particular, preparation method provided by the invention includes the following step:
(1) with clay water making beating, control slurries solids content adds acid treatment after 2-30 minute at the heavy % of 12-25, adds pseudo-boehmite making beating 30-60 minute, and wherein the weight ratio of the aluminum oxide that provides of Suan add-on and pseudo-boehmite is 0.15-0.25;
(2) be warmed up to 30-70 ℃ of aging 10-120 minute;
(3) be cooled to room temperature after, in 5-60 minute, add water glass solution and fully stir homogeneous;
(4) add finely dispersed molecular sieve pulp, stir more than 30 minutes;
(5) catalyst slurry is spray-dried, washing.
In the Preparation of catalysts method provided by the invention, after said step (3) water glass solution adds making beating, before step (4) molecular sieve pulp adds, the step that adds aluminium colloidal sol can also be arranged.
Among the preparation method provided by the present invention, handle the used acid of clay in the step (1) and be selected from a kind of among hydrochloric acid, sulfuric acid, nitric acid and the acetate, wherein preferred hydrochloric acid.
Among the preparation method provided by the present invention, said water glass solution is acid and pore distribution improving agent as matrix, its SiO
2Content be the heavy % of 2 heavy %-15, modulus is 2.9-3.2.
Preparation method provided by the present invention is applicable to that the aluminum oxide of molecular sieve, the heavy % of 15-45 of clay, the heavy % of 10-50 of the heavy % of the cracking catalyst with following composition: 15-80 and the weight ratio of the aluminum oxide that provides with pseudo-boehmite are the silicon oxide of 0.03-0.25, in the wherein said aluminum oxide, account for the heavy % of 15-30, account for the heavy % of 0-15 from the aluminum oxide of aluminium colloidal sol from the aluminum oxide of pseudo-boehmite.
Said clay is selected from one or more in kaolin, metakaolin or the halloysite.Said molecular sieve is one or more in rare-earth type, rare earth Hydrogen or the super steady type Y zeolite, also can be selected from the mixture of they and MFI structure shape-selective molecular sieve, said MFI structure molecular screen comprises ZSM-5 or belongs to one or more zeolite of MFI structure with it together, ZRP series molecular sieve for example, this series molecular sieve is existing open in documents such as CN1052290A, CN1058382A, CN1147420A and CN1194181A.
The preparation method of catalytic cracking catalyst provided by the invention compared with prior art, need not to prepare separately amorphous silicon aluminium, and provide the silicon source with water glass solution, directly add cracking catalyst and prepare in the still and get final product, technical process is shortened greatly, has also reduced productive expense.
In addition, adopt the catalyzer of method preparation provided by the invention, its specific surface SA is 200-350m
2/ g, pore volume PV is 0.19-0.24ml/g, in pore distribution, the hole of 5-20 nanometer range accounts for the 25.8V%-43.4V% of total pore volume, the 18.6V% by the catalyzer of prior art for preparing has more mesopore ratio, this helps macromolecular pre-cracking, improves yield of light oil, reduces coke and hydrogen yield.
Following example will the present invention is further illustrated, but content of the present invention is not subjected to the restriction of these examples.
Comparative Examples
With 6.7kg (butt, China Suzhou kaolin company product, down with) kaolin adds making beating in the 20kg decationized Y sieve water evenly the back is with the hcl acidifying of 613ml36% after 10 minutes, (Shandong Aluminum Plant produces to add the pseudo-boehmite of 33% solid content, 10kg down together), it is aging fully to heat up after the stirring, and behind aging the finishing, the adding alumina content is 21% aluminium colloidal sol (Shandong catalyst plant production, 4.8kg down together), (butt, the Shandong catalyst plant is produced, Na to add the homodisperse DASY of containing then
2O 1.1%) 3.1kg and REHY (butt, the production of Shandong catalyst plant, Na
2O 4.0 heavy %, silica alumina ratio 5.6, down together) the 1.5kg molecular sieve pulp, and restir 30min removes spray drying forming, and the moulding sample is through washing.Sample number into spectrum is W.
Example 1
5.4kg butt kaolin is added the even back of pulling an oar in the 20kg decationized Y sieve water uses the hcl acidifying of 845ml36% after 10 minutes, the pseudo-boehmite 13.8kg that adds 33% solid content, be warmed up to 70 ℃ after fully stirring and wear out, the aging postcooling that finishes slowly adds 4%SiO then to room temperature
2Content, modulus are 3.1 water glass (production of Shandong catalyst plant) 5.8kg, and behind the stir about 30min, (butt, the Shandong catalyst plant is produced, Na to add homodisperse REDASY
2O 1.0%, down together) molecular sieve pulp 5.4kg, more than the restir 30min, remove spray drying forming, the moulding sample is through washing.Sample number into spectrum is A.
Example 2
5.4kg butt kaolin is added the even back of pulling an oar in the 20kg decationized Y sieve water uses the hcl acidifying of 931ml36% after 15 minutes, the pseudo-boehmite 13.8kg that adds 33% solid content, be warmed up to 50 ℃ after fully stirring and wear out, the aging postcooling that finishes slowly adds 12 heavy %SiO then to room temperature
2, to contain hydromodule be 3.1 water glass 7.7kg, behind the stir about 30min, adds homodisperse REDASY butt 4.45kg and the ZSM-5 (butt of containing, Shandong catalyst plant production) molecular sieve pulp of 0.15kg, more than the restir 30min, remove spray drying forming, the moulding sample is through washing.Sample number into spectrum is B.
Example 3
6.7kg butt kaolin is added the even back of pulling an oar in the 20kg decationized Y sieve water uses the hcl acidifying of 613ml36% after 15 minutes, the pseudo-boehmite 10kg that adds 33% solid content, be warmed up to 70 ℃ after fully stirring and wear out, the aging postcooling that finishes slowly adds 8%SiO then to room temperature
2Contain hydromodule and be 3.1 water glass 4.1kg, behind the stir about 30min, the adding alumina content is 21% aluminium colloidal sol 4.8kg, behind the stir about 30min, add the homodisperse molecular sieve pulp that contains DASY3.1kg and REHY1.5kg, more than the restir 30min, remove spray drying forming, the moulding sample is through washing.Sample number into spectrum is C.
Example 4
7.6kg butt kaolin is added the even back of pulling an oar in the 22kg decationized Y sieve water with behind the hcl acidifying certain hour of 446ml36%, the pseudo-boehmite 7.3kg that adds 33% solid content, it is aging fully to stir the back intensification, and the aging postcooling that finishes slowly adds 10%SiO then to room temperature
2Contain hydromodule and be 3.1 water glass 2.4kg, behind the stir about 30min, add alumina content and be 21% aluminium colloidal sol 7.3kg, behind the stir about 30min, adds homodisperse REDASY1.3kg and REY (butt, the production of Shandong catalyst plant, the Na of containing
2O1.2%) molecular sieve pulp of 2.6kg more than the restir 30min, removes spray drying forming, and the moulding sample is through washing.Sample number into spectrum is D.
Example 5
3.0kg butt kaolin is added the even back of pulling an oar in the 20kg decationized Y sieve water uses the hcl acidifying of 1052ml 36% after 15 minutes, the pseudo-boehmite 21.0kg that adds 33% solid content, being warmed up to 70 ℃ after fully stirring wears out, the aging postcooling that finishes slowly adds then and contains 4 heavy %SiO to room temperature
2, modulus is 3.1 water glass 17.6kg, behind the stir about 30min, adds homodisperse REDASY molecular sieve pulp 6.6kg (butt), more than the restir 30min, removes spray drying forming, the moulding sample is through washing.Sample number into spectrum is E.
Example 6
5.4kg butt kaolin is added the even back of pulling an oar in the 20kg decationized Y sieve water uses the hcl acidifying of 845ml 36% after 15 minutes, the pseudo-boehmite 13.8kg that adds 33% solid content, be warmed up to 60 ℃ after fully stirring and wear out, the aging postcooling that finishes slowly adds 8%SiO then to room temperature
2Content, modulus are 3.1 water glass 8.8kg, behind the stir about 30min, add homodisperse REDASY molecular sieve pulp 5.4kg (butt), more than the restir 30min, remove spray drying forming, and the moulding sample is through washing.Sample number into spectrum is F.
Catalyst sample W and A-F that Comparative Examples and example 1-6 are prepared, their BET pore distribution data are obtained by the low-temperature nitrogen adsorption method analysis, list in the table 1.SA is a surface-area in the table, and PV is a pore volume.
Table 1
| Catalyst sample | ????A | ???B | ??C | ??D | ??E | ??F | Contrast W |
| ?SA??m 2/g ?PV??ml/g | ??284 ??0.19 | ??277 ??0.24 | ??259 ??0.20 | ??216 ??0.19 | ??293 ??0.23 | ??284 ??0.23 | ????242 ????0.17 |
| Pore distribution V%＜5nm 5-20nm＞20nm | ? ??68.0 ??25.8 ??6.2 | ? ??50.9 ??43.4 ??5.7 | ? ??53.9 ??34.2 ??11.9 | ? ??48.1 ??29.4 ??22.5 | ? ??59.2 ??36.9 ??3.9 | ? ??61.3 ??35.0 ??4.7 | ? ????73.3 ????18.6 ????8.1 |
As seen from Table 1, the prepared catalyzer of the inventive method has bigger mesopore ratio, and the mesopore ratio of its 5～20nm scope is at 25.8-43.4V%, all greater than the 18.6V% of contrast medium W.
Example 7
This example explanation contrast medium sample W and through the cracking performance of the catalyst sample A-F of present method preparation.
Raw material is the triumph decompressed wax oil, and its character sees Table 2.
Catalyst sample is all through 800 ℃/4h/100% steam aging, and its heavy oil micro anti-evaluation is the result list in the table 3.
Reaction conditions is: 482 ℃ of C/O=3 of temperature of reaction.
Table 2
| Project | Numerical value |
| Density (20 ℃) g/cm 3 | ????0.8652 |
| Viscosity mm 2/s | ????14.58 |
| Bituminous matter m% | ????0.686 |
| Conradson carbon residue m% | ????0.04 |
| Boiling range ℃ IBP 10% 50% 90% 95% FBP | ????227 ????289 ????389 ????446 ????458 ????475 |
Table 3
| The catalyzer numbering | ????A | ?????B | ?????C | ?????D | ????E | ????F | ?????W |
| Product distributes, m% gas coke gasoline, diesel＞330 ℃ of transformation efficiencys, the m% yield of light oil, m% | ? ???11.1 ???1.7 ???58.2 ???18.7 ???10.3 ???71.0 ???76.9 | ? ???12.2 ???1.6 ???56.2 ???19.2 ???10.8 ???70.0 ???75.4 | ? ???12.4 ???2.1 ???60.8 ???16.6 ???8.1 ???75.3 ???77.4 | ? ???12.3 ???2.2 ???62.1 ???15.6 ???7.8 ???76.6 ???77.7 | ? ??11.4 ??1.7 ??58.7 ??18.5 ??9.7 ??71.8 ??77.2 | ? ??11.3 ??1.8 ??59.4 ??17.9 ??9.6 ??72.5 ??77.3 | ? ??10.5 ??1.9 ??56.1 ??19.6 ??11.9 ??68.5 ??75.7 |
The catalyzer that shows the inventive method preparation from the data of table 3 has better heavy oil cracking performance and higher yield of light oil than the catalyzer of prior art for preparing.
Claims (9)
1, a kind of preparation method of cracking catalyst for petroleum hydrocarbon, it is characterized in that with clay slurry with acid treatment after, add pseudo-boehmite, carry out burin-in process, add water glass solution, after pulling an oar evenly, add finely dispersed molecular sieve pulp again, spraying drying and washing.
2, in accordance with the method for claim 1, it is characterized in that this method contains the following step:
(1) with clay water making beating, control slurries solids content adds acid treatment after 2-30 minute at the heavy % of 12-25, adds pseudo-boehmite making beating 30-60 minute, and wherein the weight ratio of the aluminum oxide that provides of Suan add-on and pseudo-boehmite is 0.15-0.25;
(2) be warmed up to 30-70 ℃ of aging 10-120 minute;
(3) be cooled to room temperature after, in 5-60 minute, add water glass solution and fully stir homogeneous;
(4) add finely dispersed molecular sieve pulp, stir more than 30 minutes;
(5) catalyst slurry is spray-dried, washing.
3, according to claim 1 or 2 described methods, it is characterized in that step (3) water glass solution adds after the making beating, step (4) molecular sieve pulp can also add aluminium colloidal sol before adding.
4, in accordance with the method for claim 1, it is characterized in that said cracking catalyst has the molecular sieve of the aluminum oxide of the clay of the heavy % of following composition: 15-80, the heavy % of 15-45, the heavy % of 10-50 and the weight ratio of the aluminum oxide that provides with pseudo-boehmite is the silicon oxide of 0.03-0.25, account for the heavy % of 15-30, account for the heavy % of 0-15 from the aluminum oxide of pseudo-boehmite in the said aluminum oxide from the aluminum oxide of aluminium colloidal sol.
5,, it is characterized in that said clay is selected from one or more in kaolin, metakaolin or the halloysite according to claim 1 or 2 described methods.
6,, it is characterized in that one or more or they of said molecular screening in rare-earth type, rare earth Hydrogen, super steady type Y zeolite and the mixture of MFI structure shape-selective molecular sieve according to claim 1 or 2 described methods.
7, in accordance with the method for claim 6, it is characterized in that said MFI structure shape-selective molecular sieve is ZSM-5 or one or more the zeolite that belongs to the MFI structure with it together.
8,, it is characterized in that said acid is selected from one of hydrochloric acid, sulfuric acid, nitric acid or acetate according to claim 1 or 2 described methods.
9,, it is characterized in that the SiO of said water glass solution according to claim 1 or 2 described methods
2Content is the heavy % of 2 heavy %-15, and modulus is 2.9-3.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01118437XA CN1191123C (en) | 2001-05-30 | 2001-05-30 | Prepn of petroleum hydrocarbon cracking catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB01118437XA CN1191123C (en) | 2001-05-30 | 2001-05-30 | Prepn of petroleum hydrocarbon cracking catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1388213A true CN1388213A (en) | 2003-01-01 |
| CN1191123C CN1191123C (en) | 2005-03-02 |
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ID=4663179
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB01118437XA Expired - Lifetime CN1191123C (en) | 2001-05-30 | 2001-05-30 | Prepn of petroleum hydrocarbon cracking catalyst |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1311907C (en) * | 2004-07-29 | 2007-04-25 | 中国石油化工股份有限公司 | Cracking catalyst for petroleum hydrocarbon, and preparation method |
| US7485595B2 (en) | 2003-05-30 | 2009-02-03 | China Petroleum & Chemical Corporation | Molecular sieve-containing catalyst for cracking hydrocarbons and a method for preparing the same |
| CN101451074B (en) * | 2007-11-28 | 2012-03-21 | 中国石油化工股份有限公司 | Catalyst for heavy oil catalytic cracking and preparation method thereof |
| CN104549541A (en) * | 2013-10-25 | 2015-04-29 | 湖南长岭石化科技开发有限公司 | Heavy oil catalytic cracking catalyst carrier and catalyst and preparation method thereof |
| CN105148985A (en) * | 2014-06-10 | 2015-12-16 | 中国石油化工股份有限公司 | Catalytic cracking catalyst, preparation method thereof and application |
| CN108404897A (en) * | 2017-02-10 | 2018-08-17 | 中国石油天然气股份有限公司 | A kind of catalyst carrier for hydrgenating heavy oil, preparation method, using its catalyst and catalyst preparation method |
| CN112169828A (en) * | 2020-10-14 | 2021-01-05 | 岳阳明科催化技术有限公司 | Clay-type catalytic cracking catalyst and preparation method thereof |
-
2001
- 2001-05-30 CN CNB01118437XA patent/CN1191123C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7485595B2 (en) | 2003-05-30 | 2009-02-03 | China Petroleum & Chemical Corporation | Molecular sieve-containing catalyst for cracking hydrocarbons and a method for preparing the same |
| CN1311907C (en) * | 2004-07-29 | 2007-04-25 | 中国石油化工股份有限公司 | Cracking catalyst for petroleum hydrocarbon, and preparation method |
| CN101451074B (en) * | 2007-11-28 | 2012-03-21 | 中国石油化工股份有限公司 | Catalyst for heavy oil catalytic cracking and preparation method thereof |
| CN104549541A (en) * | 2013-10-25 | 2015-04-29 | 湖南长岭石化科技开发有限公司 | Heavy oil catalytic cracking catalyst carrier and catalyst and preparation method thereof |
| CN104549541B (en) * | 2013-10-25 | 2017-03-15 | 湖南长岭石化科技开发有限公司 | A kind of catalyst for heavy oil catalytic cracking carrier and catalyst and preparation method thereof |
| CN105148985A (en) * | 2014-06-10 | 2015-12-16 | 中国石油化工股份有限公司 | Catalytic cracking catalyst, preparation method thereof and application |
| CN105148985B (en) * | 2014-06-10 | 2018-05-18 | 中国石油化工股份有限公司 | A kind of catalytic cracking catalyst and its preparation method and application |
| CN108404897A (en) * | 2017-02-10 | 2018-08-17 | 中国石油天然气股份有限公司 | A kind of catalyst carrier for hydrgenating heavy oil, preparation method, using its catalyst and catalyst preparation method |
| CN112169828A (en) * | 2020-10-14 | 2021-01-05 | 岳阳明科催化技术有限公司 | Clay-type catalytic cracking catalyst and preparation method thereof |
| CN112169828B (en) * | 2020-10-14 | 2022-11-15 | 岳阳明科催化技术有限公司 | Clay-type catalytic cracking catalyst and preparation method thereof |
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|---|---|
| CN1191123C (en) | 2005-03-02 |
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