CN111498862B - Preparation method and application of spherical SBA-15 mesoporous molecular sieve - Google Patents
Preparation method and application of spherical SBA-15 mesoporous molecular sieve Download PDFInfo
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 7
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 229920000428 triblock copolymer Polymers 0.000 claims description 6
- KRZCOLNOCZKSDF-UHFFFAOYSA-N 4-fluoroaniline Chemical compound NC1=CC=C(F)C=C1 KRZCOLNOCZKSDF-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006482 condensation reaction Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 abstract description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000001103 potassium chloride Substances 0.000 abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 150000003935 benzaldehydes Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 125000001255 4-fluorophenyl group Chemical group [H]C1=C([H])C(*)=C([H])C([H])=C1F 0.000 description 1
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 238000005882 aldol condensation reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/02—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of compounds containing imino groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/24—After treatment, characterised by the effect to be obtained to stabilize the molecular sieve structure
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The invention relates to a preparation method and application of spherical SBA-15 mesoporous molecular sieve, which takes P123 triblock polymer surfactant as template agent, takes tetraethyl silicate as silicon source, takes HCl as solvent, achieves the formation of spherical outer body of the SBA-15 mesoporous molecular sieve by regulating and controlling the revolution and the stirring time of a magnetic stirrer, compared with the traditional method, the invention does not need to add extra additives such as cetyl trimethyl ammonium bromide or trimethyl benzene, potassium chloride and the like to reduce the hydrophobic effect of the template agent P123 in the experimental process, sets the temperature at 40-45 ℃, regulates and controls the revolution and the stirring time of the magnetic stirrer, can synthesize the spherical SBA-15 mesoporous molecular sieve with higher crystallinity and better appearance, the cost of the invention is low, the cost of raw materials is reduced, the production process is simple, and the experimental controllability is better, and practical technological application prospect.
Description
Technical Field
The invention relates to a preparation method and application of a spherical SBA-15 mesoporous molecular sieve.
Background
In recent years, SBA-15 mesoporous molecular sieves have high specific surface area, large pore volume and thick pore walls, and have high hydrothermal stability compared with MCM supported catalysts, so that SBA-15 mesoporous molecular sieves are favored by researchers in the fields of new catalysts and supports.
In scientific research experiments and practical application processes, the SBA-15 mesoporous molecular sieve plays a key role in scientific research experiments and practical application processes in addition to the main roles of the pore structure, the pore volume and the pore diameter. In recent years, researchers find that the particle morphology and the pore structure of the SBA-15 mainly influence the dispersion degree of the loaded active component, the number of modified acid sites and the diffusion performance of reaction molecules, so that the particle morphology and the pore structure of the SBA-15 have great influence on the catalytic performance of the catalyst. In addition to the traditional rod-like, columnar, fibrous and flaky shapes, the SBA-15 mesoporous molecular sieve has a spherical shape, wherein the spherical SBA-15 mesoporous molecular sieve shows excellent performance in scientific research experiments and actual application processes, so that the synthesis of the spherical SBA-15 mesoporous molecular sieve has attracted extensive attention of many researchers in recent years.
Compared with the spherical SBA-15 mesoporous molecular sieve catalyst, the rod-shaped, columnar, fibrous and sheet-shaped SBA-15 catalyst has the advantages that the mesoporous orifices of the rod-shaped, columnar, fibrous and sheet-shaped SBA-15 catalyst are only basically arranged at two ends of carrier particles, so that the catalyst has fewer carrier mesoporous orifices and the number of unmodified acid sites, and the dispersion degree of the loaded active components is increased and the diffusion performance of reaction molecules is enhanced due to other pore passages with longer shapes, and compared with the spherical SBA-15 mesoporous molecular sieve, the catalyst can not provide more active sites and has more mesoporous orifices, so that the catalyst has excellent performance which is not possessed by SBA-15 with other shapes.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method and application of a spherical SBA-15 mesoporous molecular sieve. The hydrophobic effect of the template agent P123 can be reduced by adding additional additives such as Cetyl Trimethyl Ammonium Bromide (CTAB) or trimethylbenzene and potassium chloride in the traditional process. The invention has the technical scheme that the temperature is set to be 40-45 ℃, and the spherical SBA-15 mesoporous molecular sieve with higher crystallinity and better appearance can be synthesized by regulating the revolution and the stirring time of the magnetic stirrer.
The invention is realized by the following technical scheme:
(1) weighing a poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) P123(EO20PO70EO20, Ma ═ 5800) triblock copolymer on an analytical balance, adding the triblock copolymer into an HCl solution, and stirring the mixture at normal temperature for 3 to 4 hours until the P123 is completely dissolved to obtain a clear and transparent solution; the mass ratio of the P123 triblock copolymer to the tetraethyl silicate is 1-2: 2-5; the HCl has a molar concentration of 1.6-2M
(2) Weighing tetraethyl silicate, dropwise adding the tetraethyl silicate into the solution obtained in the step (1), violently stirring at the constant temperature of 40-55 ℃, keeping the rotation number of a stirrer at 1200-1800r/min, keeping the stirring time at 20-30min, and aging for 24-30 h under a static state;
(3) transferring the sample into a crystallization kettle with a polytetrafluoroethylene lining, and continuously crystallizing for 20-24 hours at the temperature of 100-110 ℃;
(4) and (3) carrying out suction filtration on the crystallized solid by using absolute ethyl alcohol and deionized water, washing, drying for 10-12 hours at 80 ℃ in a constant-temperature drying box, heating to 500-600 ℃ at the heating rate of 2-5 ℃/min, calcining for 5-7 hours, and removing the organic template agent to obtain the white powdery spherical SBA-15 mesoporous molecular sieve.
The preparation method has the following main advantages:
1. the raw material cost of the process is reduced; by adopting the traditional method, extra additives such as Cetyl Trimethyl Ammonium Bromide (CTAB) or trimethylbenzene and potassium chloride are usually added and dissolved together with the template P123 to achieve the effect of reducing the hydrophobicity of the template P123, and the extra additives also greatly increase the error of the experiment and even cause the failure of the experiment. According to the invention, under the condition of not adding any additional additive, the raw material cost is saved, only by regulating and controlling the revolution and the stirring time of the magnetic stirrer, the template agent P123 micelle can be converted into the spherical micelle by adopting the unique stirring speed, the initial stable spherical morphology of the target product is formed by adopting the stirring time, and the target product can be obtained by standing and aging.
2. The operability of the process is improved; in the conventional process, the additional additives increase experimental errors and even cause failure of a laboratory, and the problem of poor experimental stability due to different temperature regulation in the same step cannot be solved. According to the invention, only the template agent P123, tetraethyl silicate and the solvent HCl are used for self-assembly of the mesoporous structure in the experimental reaction process, a proper amount of P123 promotes the full dissolution and assembly of silicon species, and a proper hydrochloric acid concentration promotes the condensation polymerization of the silicon species, so that the experimental error is reduced, the experimental operation difficulty is reduced, and the process is simpler and easier without affecting the experimental result.
3. The production efficiency of the process is improved; in the conventional process, the structure of the molecular sieve is easily destroyed when calcination is performed, and in order to prevent the structure of the molecular sieve from being destroyed, the temperature rise rate is usually 1 ℃/min. In the process operation, the calcination is carried out at the heating rate of 2-5 ℃/min, hexadecyl trimethyl ammonium bromide is not added in the experimental process, the SBA-15 structure is not damaged due to high-rate heating, and the incompletely formed aggregates can be calcined while the template agent is rapidly removed, so that the time of the whole production process can be reduced, and the production speed is accelerated.
Drawings
FIG. 1: the picture of the appearance of the sample of the spherical SBA-15 mesoporous molecular sieve prepared in example 1.
FIG. 2: scanning electron microscope pictures of the spherical SBA-15 mesoporous molecular sieve prepared in example 1.
FIG. 3: the X-ray diffraction pattern of the spherical SBA-15 mesoporous molecular sieve prepared in example 3.
FIG. 4: example 3 gas chromatogram and data after condensation reaction with addition of spherical SBA-15 catalyst.
FIG. 5: example 3 gas chromatogram and data of the condensation reaction without addition of spherical SBA-15 catalyst.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the applicability of the invention:
example 1
A preparation method of spherical SBA-15 mesoporous molecular sieve, wherein the revolution is 1500r/min, stirring is carried out for 20 minutes, and the following specific embodiments are provided:
weighing 4g P123 template agent on an analytical balance, adding the template agent into a round-bottom flask containing 140ml of 1.6M HCl solution, stirring for 4 hours at 40 ℃, and stirring to form a vortex until P123 is completely dissolved to obtain a clear and transparent solution; weighing 8.56g of tetraethyl silicate, dropwise adding the tetraethyl silicate into the solution, heating the oil bath to 45 ℃, adjusting the revolution of the magnetic stirrer to 1500r/min, stirring for 20 minutes, stopping stirring, and aging for 24 hours in a static state; transferring the obtained sample into a crystallization kettle with a polytetrafluoroethylene lining, and crystallizing for 24 hours at 100 ℃; and (3) carrying out suction filtration on the crystallized solid by using absolute ethyl alcohol and deionized water, washing, drying in a constant-temperature drying oven at 80 ℃ for 10 hours, and finally calcining at 550 ℃ for 6 hours at a heating rate of 2 ℃/min to remove the surfactant, thus obtaining the white powdery spherical SBA-15 mesoporous molecular sieve.
Example 2
A preparation method of spherical SBA-15 mesoporous molecular sieve, wherein the revolution is 1200r/min, stirring is carried out for 30 minutes, and the following specific embodiments are provided:
weighing 4g P123 template agent on an analytical balance, adding the template agent into a round-bottom flask containing 140ml of 1.6M HCl solution, stirring for 4 hours at 40 ℃, and stirring to form a vortex until P123 is completely dissolved to obtain a clear and transparent solution; weighing 8.56g of tetraethyl silicate, dropwise adding the tetraethyl silicate into the solution, heating the oil bath to 45 ℃, adjusting the rotation number of a magnetic stirrer to 1200r/min, stirring for 30 minutes, stopping stirring, and aging for 24 hours in a static state; transferring the obtained sample into a crystallization kettle with a polytetrafluoroethylene lining, and crystallizing for 24 hours at 100 ℃; and (3) carrying out suction filtration on the crystallized solid by using absolute ethyl alcohol and deionized water, washing, drying in a constant-temperature drying oven at 80 ℃ for 10 hours, and finally calcining at 550 ℃ for 6 hours at a heating rate of 2 ℃/min to remove the surfactant, thus obtaining the white powdery spherical SBA-15 mesoporous molecular sieve.
Both of the above-mentioned preparation methods can produce a spherical SBA-15 mesoporous molecular sieve having a high degree of synthesis crystallinity and a good appearance, and can be used for the reaction study of aldehyde and ammonia in the following example 3 by studying the stirring speed and the stirring time, and the participation data are shown in fig. 4 and 5.
Example 3
The spherical SBA-15 mesoporous molecular sieve prepared in example 1 or 2 was subjected to aluminum modification with Si/Al ═ 30, thereby increasing the acidic sites and hydrothermal stability of the spherical SBA-15, and then used as a catalyst for the aldol condensation reaction, and the following is a specific embodiment:
simultaneously carrying out two groups of ammonia-aldehyde condensation reactions, respectively adding benzaldehyde compounds, 4-fluoroaniline and solvent anhydrous methanol into a round-bottom flask, adopting the molar ratio of the 4-fluoroaniline compounds to the benzaldehyde compounds to be 1.5:1, adding an aluminum modified spherical SBA-15 catalyst into one group of reactions, and stirring the other group of reactions at room temperature without adding the catalyst.
The compound benzaldehyde and 4-fluoroaniline are respectively fed in an amount of 0.1mmol and 0.15mmol, the dosage of Al/SBA-15 catalyst is 6mg, and the dosage of solvent anhydrous methanol is 4 ml; after 1.5 hours of reaction, adding a spherical SBA-15 catalyst, finishing the reaction, and after 2 hours of reaction, finishing the reaction of the other group without adding the catalyst.
After the reaction is finished, the two groups of reactions are respectively processed to generate the target product (Z) -N- (4-fluorophenyl) -1-phenylmethylimine. The group without the aluminum-modified spherical SBA-15 catalyst was analyzed to produce an imine target product at a yield of 60.00%, and the other group with the catalyst added increased the yield of the imine target product to 82.28%.
The invention relates to a preparation method and application for synthesizing a spherical SBA-15 mesoporous molecular sieve, wherein the result of the prepared SBA-15 mesoporous molecular sieve indicates that the spherical SBA-15 with better appearance and a normal molecular sieve structure can be obtained.
The above description is only for the specific embodiment of the present invention, but not limited to the application of the present invention, and those skilled in the art of research can modify the raw material ratio, change the stirring speed and change the stirring time without departing from the scope of the present invention, and these changes should be considered as the protection scope of the present invention.
Claims (5)
1. The application of spherical SBA-15 mesoporous molecular sieve as a catalyst in catalyzing the condensation reaction of 4-fluoroaniline and benzaldehyde is characterized in that the molar ratio of the 4-fluoroaniline to the benzaldehyde is 1.5: 1;
the preparation method of the spherical SBA-15 mesoporous molecular sieve comprises the following steps:
(1) adding HCl solution into the P123 triblock copolymer, and stirring until the P123 triblock copolymer is completely dissolved to obtain clear and transparent solution;
(2) adding tetraethyl silicate solution into the solution obtained in the step (1) drop by drop, stirring and aging in a static state;
(3) transferring the obtained aged sample into a crystallization kettle with a polytetrafluoroethylene lining, and continuously crystallizing for 20-24 hours at the temperature of 100-110 ℃;
(4) and (3) carrying out suction filtration, washing, drying and high-temperature calcination on the crystallized solid by using absolute ethyl alcohol and deionized water to prepare the spherical SBA-15 mesoporous molecular sieve, wherein the reaction formula is as follows:
2. use according to claim 1, characterized in that: in the step (1), the mass ratio of the P123 triblock copolymer to the tetraethyl silicate is 1-2: 2-5; the molar concentration of HCl is 1.6-2M.
3. Use according to claim 1, characterized in that: after the tetraethyl silicate solution is added in the step (2), the temperature in the stirring process is 40-55 ℃.
4. Use according to claim 1, characterized in that: in the stirring process in the step (2), the rotation speed of the stirrer is 1200-1800r/min, and the stirring time is 20-30 min.
5. Use according to claim 1, characterized in that: in the high-temperature calcination process in the step (4), the temperature is raised to 500-600 ℃ at the temperature rise rate of 2-5 ℃/min, and the calcination is carried out for 5-7 h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6544923B1 (en) * | 1999-08-25 | 2003-04-08 | Massachusetts Institute Of Technology | Surface-confined catalytic compositions |
| CN101768038A (en) * | 2009-12-25 | 2010-07-07 | 华东师范大学 | Method for preparing Schiff base |
| CN102728340A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院青岛生物能源与过程研究所 | Solid base catalyst and an application thereof |
| CN103803573A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Preparation method of mesoporous silica molecular sieve |
| CN109499609A (en) * | 2018-12-05 | 2019-03-22 | 浙江工业大学 | A kind of immobilized 2-aza-adamantane N-oxyl radical catalyst of SBA-15 and its preparation and application |
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| CN100383043C (en) * | 2005-06-15 | 2008-04-23 | 浙江大学 | Process for synthesizing mesic porous molecular sieve SBA-15 |
| CN101659617A (en) * | 2009-09-10 | 2010-03-03 | 华东理工大学 | Preparation method of alky-substituted aromatic diamine |
| CN104140090B (en) * | 2014-08-02 | 2016-08-31 | 孙超 | A kind of preparation method of hydrophilic ordered mesoporous carbon material |
| CN106629772A (en) * | 2016-11-29 | 2017-05-10 | 辽宁石油化工大学 | Method for preparing hierarchical porous SAPO-11 molecular sieve by using templating agent P123-containing SBA-15 as silicon source |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6544923B1 (en) * | 1999-08-25 | 2003-04-08 | Massachusetts Institute Of Technology | Surface-confined catalytic compositions |
| CN101768038A (en) * | 2009-12-25 | 2010-07-07 | 华东师范大学 | Method for preparing Schiff base |
| CN102728340A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院青岛生物能源与过程研究所 | Solid base catalyst and an application thereof |
| CN103803573A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Preparation method of mesoporous silica molecular sieve |
| CN109499609A (en) * | 2018-12-05 | 2019-03-22 | 浙江工业大学 | A kind of immobilized 2-aza-adamantane N-oxyl radical catalyst of SBA-15 and its preparation and application |
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