CN104399445B - The preparation method of catalytic cracking catalyst - Google Patents
The preparation method of catalytic cracking catalyst Download PDFInfo
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- CN104399445B CN104399445B CN201410615717.7A CN201410615717A CN104399445B CN 104399445 B CN104399445 B CN 104399445B CN 201410615717 A CN201410615717 A CN 201410615717A CN 104399445 B CN104399445 B CN 104399445B
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Abstract
The present invention discloses the preparation method of a kind of catalytic cracking catalyst, belongs to catalyst preparation technical field.The present invention, by kaolin raw ore being modified, obtains the refining kaolin of high-quality, and is used in catalytic cracking catalyst by this refining kaolin, so that the catalytic efficiency of the catalytic cracking catalyst prepared effectively improves.
Description
Technical field
The present invention relates to catalyst preparation technical field, particularly relate to the preparation method of a kind 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 the chemical catalysis process that macromolecular cleavage becomes little molecule, and is the acidic catalyst reaction with acid centre as active sites.It is the core technology of chemical industry and important science and technology basis now that research catalytic process and catalytic cracking catalyst are one.Wherein, the catalytic cracking catalyst in current catalytic cracking catalyst, with Kaolin as 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 catalytic cracking catalyst prepared to can not get being effectively improved always.
Summary of the invention
The present invention provides the preparation method of a kind of catalytic cracking catalyst, and this preparation method can effectively solve the poor performance because of feed kaolin, causes the problem that the catalytic efficiency of its catalytic cracking catalyst prepared can not get being effectively improved always.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
It includes following preparation process:
A, by weight, 80 parts of Kaolin and 40 parts～130 parts of carbamide are sufficiently mixed in open container and stir, then proceed in hermetic container, be heated to 90 DEG C～100 DEG C and carry out insulation reaction, until obtaining intercalation rate to reach the Kaolin-carbamide intercalated compound of 99%；
B, Kaolin-carbamide intercalated compound step A prepared and 20 parts～40 parts of triethanolamine mix homogeneously, be heated to 120 DEG C～130 DEG C and carry out insulation reaction 1 hour～2 hours；
C, after step B, in the mixture that step B prepares, add 450 parts～1000 parts of 0.5mol/L iodomethane ethanol solution and 1000 parts～2000 parts of 0.3mol/L sodium cetanesulfonate aqueous solution are uniform, first it is cooled to 50 DEG C～80 DEG C, insulation reaction 1 hour～2 hours；It is warming up to 130 DEG C～150 DEG C the most again, insulation reaction 1 hour～2 hours, prepare Modification of kaolin slurry；
D. Modification of kaolin slurry spray-dried one-tenth microsphere step C prepared, then at a temperature of 750 DEG C～850 DEG C, roasting 2 hours～4 hours；
E. microsphere D step prepared and additional aluminum source, acid solution microsphere in mass ratio: the ratio of additional aluminum source: acid solution=1:0.1～0.5:0.5～0.8 stirs, mixs homogeneously, then under air-proof condition, it is heated to 90 DEG C～100 DEG C, isothermal reaction 1 hour～2 hours, filter, it is dried, obtains refining kaolin；
F. the modified kaolin of E step roasting and alkali crystallization solution are mixed and be incorporated in crystallization 10 hours～15 hours under the hydrothermal condition of 95 DEG C～100 DEG C, then filter, wash.
In technique scheme, more specifically technical scheme is: the particle diameter of described microsphere is 0.05 millimeter～0.06 millimeter.
Further, described additional aluminum source is the one in metallic aluminium powder, aluminum chloride.
Further, the one during described acid solution is hydrochloric acid solution, salpeter solution.
Owing to using technique scheme, the present invention obtains providing the benefit that:
The present invention, by kaolin raw ore being modified, obtains the refining kaolin of high-quality, and is used in catalytic cracking catalyst by this refining kaolin, so that the catalytic efficiency of the catalytic cracking catalyst prepared effectively improves.
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 intended to be limited to following example.
Embodiment 1
The preparation method of this catalytic cracking catalyst is as follows:
80 parts of Kaolin and 40 parts of carbamide are sufficiently mixed in open container and stir, then proceed in hermetic container, be heated to 90 DEG C and carry out insulation reaction, until obtaining intercalation rate to reach the Kaolin-carbamide intercalated compound of 99% by A, by weight；
B, Kaolin-carbamide intercalated compound step A prepared and 40 parts of triethanolamine mix homogeneously, be heated to 120 DEG C and carry out insulation reaction 2 hours；
C, after step B, in the mixture that step B prepares, add 450 parts of 0.5mol/L iodomethane ethanol solution and 2000 parts of 0.3mol/L sodium cetanesulfonate aqueous solution be uniform, be first cooled to 50 DEG C, insulation reaction 2 hours；It is warming up to 130 DEG C the most again, insulation reaction 2 hours, prepare Modification of kaolin slurry；
D. the microsphere that Modification of kaolin slurry spray-dried one-tenth particle diameter is 0.05 millimeter step C prepared, then at a temperature of 750 DEG C, roasting 4 hours；
E. microsphere D step prepared and metallic aluminium powder, hydrochloric acid solution microsphere in mass ratio: metallic aluminium powder: the ratio of hydrochloric acid solution=1:0.1:0.8 stirs, mixs homogeneously, then under air-proof condition, 90 DEG C it are heated to, isothermal reaction 2 hours, filter, it is dried, obtains refining kaolin；
F. the modified kaolin of E step roasting and alkali crystallization solution are mixed and be incorporated in crystallization 14 hours under the hydrothermal condition of 98 DEG C, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst prepared by the present embodiment improves 12%.
Embodiment 2
The preparation method of this catalytic cracking catalyst is as follows:
80 parts of Kaolin and 130 parts of carbamide are sufficiently mixed in open container and stir, then proceed in hermetic container, be heated to 100 DEG C and carry out insulation reaction, until obtaining intercalation rate to reach the Kaolin-carbamide intercalated compound of 99% by A, by weight；
B, Kaolin-carbamide intercalated compound step A prepared and 20 parts of triethanolamine mix homogeneously, be heated to 130 DEG C and carry out insulation reaction 1 hour；
C, after step B, in the mixture that step B prepares, add 1000 parts of 0.5mol/L iodomethane ethanol solution and 1000 parts of 0.3mol/L sodium cetanesulfonate aqueous solution be uniform, be first cooled to 80 DEG C, insulation reaction 1 hour；It is warming up to 150 DEG C the most again, insulation reaction 1 hour, prepare Modification of kaolin slurry；
D. the microsphere that Modification of kaolin slurry spray-dried one-tenth particle diameter is 0.06 millimeter step C prepared, then at a temperature of 850 DEG C, roasting 2 hours；
E. microsphere D step prepared and aluminum chloride, salpeter solution microsphere in mass ratio: aluminum chloride: the ratio of salpeter solution=1:0.5:0.5 stirs, mixs homogeneously, then under air-proof condition, 100 DEG C it are heated to, isothermal reaction 1 hour, filter, it is dried, obtains refining kaolin；
F. the modified kaolin of E step roasting and alkali crystallization solution are mixed and be incorporated in crystallization 15 hours under the hydrothermal condition of 95 DEG C, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst prepared by the present embodiment improves 14%.
Embodiment 3
The preparation method of this catalytic cracking catalyst is as follows:
80 parts of Kaolin and 80 parts of carbamide are sufficiently mixed in open container and stir, then proceed in hermetic container, be heated to 95 DEG C and carry out insulation reaction, until obtaining intercalation rate to reach the Kaolin-carbamide intercalated compound of 99% by A, by weight；
B, Kaolin-carbamide intercalated compound step A prepared and 30 parts of triethanolamine mix homogeneously, be heated to 125 DEG C and carry out insulation reaction 1.5 hours；
C, after step B, in the mixture that step B prepares, add 750 parts of 0.5mol/L iodomethane ethanol solution and 1500 parts of 0.3mol/L sodium cetanesulfonate aqueous solution be uniform, be first cooled to 60 DEG C, insulation reaction 1.5 hours；It is warming up to 140 DEG C the most again, insulation reaction 1.5 hours, prepare Modification of kaolin slurry；
D. the microsphere that Modification of kaolin slurry spray-dried one-tenth particle diameter is 0.05 millimeter step C prepared, then at a temperature of 800 DEG C, roasting 3 hours；
E. microsphere D step prepared and metallic aluminium powder, salpeter solution microsphere in mass ratio: metallic aluminium powder: the ratio of salpeter solution=1:0.3:0.7 stirs, mixs homogeneously, then under air-proof condition, 95 DEG C it are heated to, isothermal reaction 1.5 hours, filter, it is dried, obtains refining kaolin；
F. the modified kaolin of E step roasting and alkali crystallization solution are mixed and be incorporated in crystallization 10 hours under the hydrothermal condition of 100 DEG C, then filter, wash.
Compared with similar products, the catalytic efficiency of the catalytic cracking catalyst prepared by the present embodiment improves 13%.
Claims (4)
1. the preparation method of a catalytic cracking catalyst, it is characterised in that include following preparation process:
A, by weight, 80 parts of Kaolin and 40 parts～130 parts of carbamide are sufficiently mixed in open container and stir, then proceed in hermetic container, be heated to 90 DEG C～100 DEG C and carry out insulation reaction, until obtaining intercalation rate to reach the Kaolin-carbamide intercalated compound of 99%；
B, Kaolin-carbamide intercalated compound step A prepared and 20 parts～40 parts of triethanolamine mix homogeneously, be heated to 120 DEG C～130 DEG C and carry out insulation reaction 1 hour～2 hours；
C, after step B, in the mixture that step B prepares, add 450 parts～1000 parts of 0.5mol/L iodomethane ethanol solution and 1000 parts～2000 parts of 0.3mol/L sodium cetanesulfonate aqueous solution are uniform, first it is cooled to 50 DEG C～80 DEG C, insulation reaction 1 hour～2 hours；It is warming up to 130 DEG C～150 DEG C the most again, insulation reaction 1 hour～2 hours, prepare Modification of kaolin slurry；
D. Modification of kaolin slurry spray-dried one-tenth microsphere step C prepared, then at a temperature of 750 DEG C～850 DEG C, roasting 2 hours～4 hours；
E. microsphere D step prepared and additional aluminum source, acid solution microsphere in mass ratio: the ratio of additional aluminum source: acid solution=1:0.1～0.5:0.5～0.8 stirs, mixs homogeneously, then under air-proof condition, it is heated to 90 DEG C～100 DEG C, isothermal reaction 1 hour～2 hours, filter, it is dried, obtains refining kaolin；
F. refining kaolin E step obtained and alkali crystallization solution mix crystallization 10 hours～15 hours under the hydrothermal condition being incorporated in 95 DEG C～100 DEG C, then filter, wash.
Catalytic cracking catalyst the most according to claim 1, it is characterised in that: the particle diameter of described microsphere is 0.05 millimeter～0.06 millimeter.
Catalytic cracking catalyst the most according to claim 2, it is characterised in that: described additional aluminum source is the one in metallic aluminium powder, aluminum chloride.
4. according to the catalytic cracking catalyst described in claim 1 or 2 or 3, it is characterised in that: described acid solution is the one in hydrochloric acid solution, salpeter solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410615717.7A CN104399445B (en) | 2014-11-05 | The preparation method of catalytic cracking catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410615717.7A CN104399445B (en) | 2014-11-05 | The preparation method of catalytic cracking catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104399445A CN104399445A (en) | 2015-03-11 |
| CN104399445B true CN104399445B (en) | 2017-01-04 |
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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: 20201123 Address after: 535035 5th floor, building 6, light equipment production building, science and Technology Park (business incubation base), No.5 Zhongma street, Qinzhou Industrial Park, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: GUANGXI ZHONGMA INDUSTRIAL PARK MANUFACTURED BY YOU 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 |