CN104307544A - Method for preparing catalytic cracking catalyst - Google Patents
Method for preparing catalytic cracking catalyst Download PDFInfo
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- CN104307544A CN104307544A CN201410615772.6A CN201410615772A CN104307544A CN 104307544 A CN104307544 A CN 104307544A CN 201410615772 A CN201410615772 A CN 201410615772A CN 104307544 A CN104307544 A CN 104307544A
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Abstract
The invention discloses a method for preparing a catalytic cracking catalyst, and belongs to the technical field of catalyst preparation. According to the method, kaolin ore is modified to obtain high-quality refined kaolin, and the refined kaolin is used in the catalytic cracking catalyst, so that the catalytic efficiency of the catalytic cracking catalyst is effectively improved, and meanwhile as the kaolin ore is modified, the method is applicable to catalytic cracking reaction of raw oil with high nickel-vanadium content.
Description
Technical field
The present invention relates to catalyst preparation technical field, particularly relate to a kind of preparation method of catalytic cracking catalyst.
Background technology
In the heavy oil deep process technology of petroleum refining process, catalytic cracking is a kind of most important secondary operations means of oil plant, and it makes more heavy oil obtain lighting.The know-why of catalytic cracking is that macromolecular cleavage becomes micromolecular chemical catalysis process, and be with acid centre be active sites acidic catalyst reaction.The core technology of research catalytic process and catalytic cracking catalyst to be one be now chemical industry and important science and technology basis.Wherein, in current catalytic cracking catalyst, take kaolin as the catalytic cracking catalyst of key component.The catalytic efficiency of this catalytic cracking catalyst is higher than other catalytic cracking catalysts, but due to the poor performance of most feed kaolin, causes the catalytic efficiency of its obtained catalytic cracking catalyst to can not get effective raising always.
Summary of the invention
The invention provides a kind of preparation method of catalytic cracking catalyst, this preparation method effectively can solve the poor performance because of feed kaolin, causes the catalytic efficiency of its obtained catalytic cracking catalyst to can not get the problem effectively improved always.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
It comprises following preparation process:
A. by kaolin raw ore, water and the dispersant kaolin raw ore in mass ratio after pulverizing: water: the ratio of dispersant=1:0.5 ~ 0.8:0.002 ~ 0.003 stirs, mixes, and obtained kaolin ore slurry is just expected;
B. the sulfuric acid solution of described stock quality 20% ~ 25% and the hydrogensulfite solution of described stock quality 75% ~ 80% is added in the slurry obtained to step A, mix, the pH value of its mixed liquor is regulated to be 2.0 ~ 3.0, then stir 0.5 hour ~ 1 hour with the speed of 250 revs/min ~ 450 revs/min, obtain kaolin ore slurry fine fodder;
C. by the spray-dried one-tenth microballoon of kaolin ore slurry fine fodder that step B is obtained, then at the temperature of 750 DEG C ~ 850 DEG C, roasting 2 hours ~ 4 hours;
D. by microballoon obtained for step C and additional aluminium source, acid solution microballoon in mass ratio: additional aluminium source: the ratio of acid solution=1:0.1 ~ 0.5:0.5 ~ 0.8 stirs, mixes, then under air-proof condition, 90 DEG C ~ 100 DEG C are heated to, isothermal reaction 1 hour ~ 2 hours, filter, drying, obtains modified kaolin;
E. the modified kaolin of D step roasting and alkali crystallization solution to be mixed under the hydrothermal condition being incorporated in 95 DEG C ~ 100 DEG C crystallization 10 hours ~ 15 hours, then filter, wash.
In technique scheme, technical scheme is more specifically: described dispersant is waterglass, one in both sodium phosphate trimers.
Further, the particle diameter of described microballoon is 0.05 millimeter ~ 0.06 millimeter.
Further, described additional aluminium source is the one in metallic aluminium powder, aluminium chloride.
Further, described acid solution is the one in hydrochloric acid solution, salpeter solution.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
1. the present invention is by carrying out modification by kaolin raw ore, obtains the refining kaolin of high-quality, and is used in catalytic cracking catalyst by this refining kaolin, thus the catalytic efficiency of the catalytic cracking catalyst obtained is effectively improved.
2. the present invention is owing to having carried out modification by kaolin raw ore in advance, makes the catalytic cracking catalyst obtained can be applicable to the catalytic cracking reaction of nickelic content of vanadium crude oil.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
The preparation method of this catalytic cracking catalyst is as follows:
A. by kaolin raw ore, water and the waterglass kaolin raw ore in mass ratio after pulverizing: water: the ratio of waterglass=1:0.5:0.003 stirs, mixes, and obtained kaolin ore slurry is just expected;
B. the sulfuric acid solution of described stock quality 20% and the hydrogensulfite solution of described stock quality 75% is added in the slurry obtained to step A, mix, regulate the pH value of its mixed liquor to be 2.0, then stir 0.5 hour with the speed of 450 revs/min, obtain kaolin ore slurry fine fodder;
C. the spray-dried one-tenth particle diameter of kaolin ore slurry fine fodder step B obtained is the microballoon of 0.05 millimeter, then at the temperature of 750 DEG C, and roasting 4 hours;
D. by microballoon obtained for step C and metallic aluminium powder, salpeter solution microballoon in mass ratio: metallic aluminium powder: the ratio of salpeter solution=1:0.1:0.8 stirs, mixes, then under air-proof condition, be heated to 90 DEG C, isothermal reaction 2 hours, filter, drying, obtains modified kaolin;
E. the modified kaolin of D step roasting and alkali crystallization solution to be mixed under the hydrothermal condition being incorporated in 95 DEG C crystallization 15 hours, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst obtained by the present embodiment improves 12%.
Embodiment 2
The preparation method of this catalytic cracking catalyst is as follows:
A. by kaolin raw ore, water and the sodium phosphate trimer kaolin raw ore in mass ratio after pulverizing: water: the ratio of sodium phosphate trimer=1:0.8:0.002 stirs, mixes, and obtained kaolin ore slurry is just expected;
B. the sulfuric acid solution of described stock quality 25% and the hydrogensulfite solution of described stock quality 80% is added in the slurry obtained to step A, mix, regulate the pH value of its mixed liquor to be 3.0, then stir 1 hour with the speed of 250 revs/min, obtain kaolin ore slurry fine fodder;
C. the spray-dried one-tenth particle diameter of kaolin ore slurry fine fodder step B obtained is the microballoon of 0.06 millimeter, then at the temperature of 850 DEG C, and roasting 2 hours;
D. by microballoon obtained for step C and aluminium chloride, hydrochloric acid solution microballoon in mass ratio: aluminium chloride: the ratio of hydrochloric acid solution=1:0.5:0.5 stirs, mixes, then under air-proof condition, be heated to 100 DEG C, isothermal reaction 1 hour, filter, drying, obtains modified kaolin;
E. the modified kaolin of D step roasting and alkali crystallization solution to be mixed under the hydrothermal condition being incorporated in 100 DEG C crystallization 10 hours, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst obtained by the present embodiment improves 14%.
Embodiment 3
The preparation method of this catalytic cracking catalyst is as follows:
A. by kaolin raw ore, water and the waterglass kaolin raw ore in mass ratio after pulverizing: water: the ratio of waterglass=1:0.6:0.0025 stirs, mixes, and obtained kaolin ore slurry is just expected;
B. the sulfuric acid solution of described stock quality 23% and the hydrogensulfite solution of described stock quality 78% is added in the slurry obtained to step A, mix, regulate the pH value of its mixed liquor to be 2.5, then stir 0.5 hour with the speed of 350 revs/min, obtain kaolin ore slurry fine fodder;
C. the spray-dried one-tenth particle diameter of kaolin ore slurry fine fodder step B obtained is the microballoon of 0.05 millimeter, then at the temperature of 800 DEG C, and roasting 3 hours;
D. by microballoon obtained for step C and metallic aluminium powder, hydrochloric acid solution microballoon in mass ratio: metallic aluminium powder: the ratio of hydrochloric acid solution=1:0.3:0.6 stirs, mixes, then under air-proof condition, be heated to 95 DEG C, isothermal reaction 1.5 hours, filter, drying, obtains modified kaolin;
E. the modified kaolin of D step roasting and alkali crystallization solution to be mixed under the hydrothermal condition being incorporated in 98 DEG C crystallization 12 hours, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst obtained by the present embodiment improves 15%.
Claims (5)
1. a preparation method for catalytic cracking catalyst, is characterized in that comprising following preparation process:
A. by kaolin raw ore, water and the dispersant kaolin raw ore in mass ratio after pulverizing: water: the ratio of dispersant=1:0.5 ~ 0.8:0.002 ~ 0.003 stirs, mixes, and obtained kaolin ore slurry is just expected;
B. the sulfuric acid solution of described stock quality 20% ~ 25% and the hydrogensulfite solution of described stock quality 75% ~ 80% is added in the slurry obtained to step A, mix, the pH value of its mixed liquor is regulated to be 2.0 ~ 3.0, then stir 0.5 hour ~ 1 hour with the speed of 250 revs/min ~ 450 revs/min, obtain kaolin ore slurry fine fodder;
C. by the spray-dried one-tenth microballoon of kaolin ore slurry fine fodder that step B is obtained, then at the temperature of 750 DEG C ~ 850 DEG C, roasting 2 hours ~ 4 hours;
D. by microballoon obtained for step C and additional aluminium source, acid solution microballoon in mass ratio: additional aluminium source: the ratio of acid solution=1:0.1 ~ 0.5:0.5 ~ 0.8 stirs, mixes, then under air-proof condition, 90 DEG C ~ 100 DEG C are heated to, isothermal reaction 1 hour ~ 2 hours, filter, drying, obtains modified kaolin;
E. the modified kaolin of D step roasting and alkali crystallization solution to be mixed under the hydrothermal condition being incorporated in 95 DEG C ~ 100 DEG C crystallization 10 hours ~ 15 hours, then filter, wash.
2. catalytic cracking catalyst according to claim 1, is characterized in that: described dispersant is waterglass, one in both sodium phosphate trimers.
3. the catalytic cracking catalyst according to claim 1 or 2 or 3 or 4, is characterized in that: the particle diameter of described microballoon is 0.05 millimeter ~ 0.06 millimeter.
4. catalytic cracking catalyst according to claim 2, is characterized in that: described additional aluminium source is the one in metallic aluminium powder, aluminium chloride.
5. catalytic cracking catalyst according to claim 2, is characterized in that: described acid solution is the one in hydrochloric acid solution, salpeter solution.
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| CN201410615772.6A CN104307544B (en) | 2014-11-05 | 2014-11-05 | The preparation method of catalytic cracking catalyst |
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| CN201410615772.6A CN104307544B (en) | 2014-11-05 | 2014-11-05 | The preparation method of catalytic cracking catalyst |
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| CN104307544B CN104307544B (en) | 2016-10-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646481A (en) * | 2020-06-11 | 2020-09-11 | 漳州阳盛贸易有限公司 | Kaolin for preparing heavy oil catalytic cracking catalyst and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4843052A (en) * | 1982-05-21 | 1989-06-27 | W. R. Grace & Co.-Conn. | Acid-reacted metakaolin catalyst and catalyst support compositions |
| CN101619228A (en) * | 2008-07-04 | 2010-01-06 | 中国石油化工股份有限公司 | Method for quick in situ synthesis of catalytic cracking catalyst |
| CN102019197A (en) * | 2009-09-18 | 2011-04-20 | 中国石油天然气股份有限公司 | Method for synthesizing kaolin microsphere in-situ crystallized product containing small crystal grain NaY molecular sieves |
| CN104030307A (en) * | 2014-05-16 | 2014-09-10 | 茂名市茂群高岭土有限公司 | Kaolin for preparing heavy-oil catalytic cracking catalyst |
-
2014
- 2014-11-05 CN CN201410615772.6A patent/CN104307544B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4843052A (en) * | 1982-05-21 | 1989-06-27 | W. R. Grace & Co.-Conn. | Acid-reacted metakaolin catalyst and catalyst support compositions |
| CN101619228A (en) * | 2008-07-04 | 2010-01-06 | 中国石油化工股份有限公司 | Method for quick in situ synthesis of catalytic cracking catalyst |
| CN102019197A (en) * | 2009-09-18 | 2011-04-20 | 中国石油天然气股份有限公司 | Method for synthesizing kaolin microsphere in-situ crystallized product containing small crystal grain NaY molecular sieves |
| CN104030307A (en) * | 2014-05-16 | 2014-09-10 | 茂名市茂群高岭土有限公司 | Kaolin for preparing heavy-oil catalytic cracking catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111646481A (en) * | 2020-06-11 | 2020-09-11 | 漳州阳盛贸易有限公司 | Kaolin for preparing heavy oil catalytic cracking catalyst and preparation method thereof |
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Address after: Huanjiang Maonan Autonomous County, Hechi City, the Guangxi Zhuang Autonomous Region 547100 Enzhen North Development Zone Patentee after: Wu Junrong Address before: 545005 the Guangxi Zhuang Autonomous Region Liuzhou Liunan District City Station Road No. 94 District 18 Building 2 unit 401 Patentee before: Wu Junrong |
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Effective date of registration: 20201127 Address after: Room A107, public service center, No.1 Zhongma street, Qinzhou Industrial Park, Qinzhou port area, Qinzhou pilot Free Trade Zone, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Qinbao Network Technology Co., Ltd Address before: Huanjiang Maonan Autonomous County, Hechi City, the Guangxi Zhuang Autonomous Region 547100 Enzhen North Development Zone Patentee before: Wu Junrong |