CN113307276A - Preparation method of SBA-15 microspheres - Google Patents
Preparation method of SBA-15 microspheres Download PDFInfo
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- CN113307276A CN113307276A CN202110520504.6A CN202110520504A CN113307276A CN 113307276 A CN113307276 A CN 113307276A CN 202110520504 A CN202110520504 A CN 202110520504A CN 113307276 A CN113307276 A CN 113307276A
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- sba
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- 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 discloses a preparation method of SBA-15 microspheres, which comprises the following steps: dissolving inorganic salt with preset quality in a polyvinyl alcohol solution, adding a sodium hydroxide catalyst, stirring and reacting at a certain temperature, cooling and filtering to obtain polyvinyl alcohol microspheres; step 2: dissolving a surfactant P123 in hydrochloric acid with a preset concentration, heating and stirring until the solution is clear, adding mesitylene (TMS) after the solution is cooled to a required temperature, adding Tetraethoxysilane (TEOS) as a precursor after the dropwise addition is finished, then adding polyvinyl alcohol microspheres as a dispersing agent, continuing heating and stirring for a period of time, cooling and standing after the reaction is finished, filtering, washing soluble salt components with distilled water, carrying out hydrothermal treatment on the obtained solution in a high-pressure kettle, filtering and drying the obtained solid, and calcining at a preset temperature to remove volatile components to obtain the SBA-15 microspheres. The SBA-15 microspheres prepared by the method have the advantages of good dispersibility and uniformity.
Description
Technical Field
The invention belongs to a high molecular polymerization technology, and particularly relates to a preparation method of SBA-15 microspheres.
Technical Field
SBA-15 is a well-known mesoporous silica (SiO2) prepared by taking P123 or similar block copolymer surfactant as a soft template and utilizing the self-assembly process between the soft template and silicon species, and has the advantages of large specific surface area, narrow pore size distribution, controllable pore size and the like. Therefore, the method has wide application prospects in the aspects of nano material reactors, catalysis, separation, adsorption, biosensors, drug slow release and the like.
The method for synthesizing the microspheres includes microemulsion polymerization, emulsion polymerization, dispersion polymerization, suspension polymerization and seed polymerization. At present, the surface active agent P123 is mainly used as a template or CATB is used as a template aid to prepare the micron-sized spherical SBA-15 in an alkaline or acidic condition for preparing the SBA-15 microsphere, but the dispersibility and the uniformity of the SBA-15 microsphere are poor in a common preparation method, so that the dispersibility and the uniformity of the SBA-15 microsphere need to be improved.
Disclosure of Invention
The invention provides a preparation method of SBA-15 microspheres with good dispersibility and uniformity by adding polyvinyl alcohol microspheres as a dispersing agent into a traditional P123/organic silicon/hydrochloric acid system.
The invention relates to a preparation method of SBA-15 microspheres, which comprises the following steps: a preparation method of SBA-15 microspheres is characterized by comprising the following steps: dissolving inorganic salt with preset quality in a polyvinyl alcohol solution, adding a sodium hydroxide catalyst, stirring and reacting at a certain temperature, cooling and filtering to obtain polyvinyl alcohol microspheres;
step 2: dissolving a surfactant P123 in hydrochloric acid with a preset concentration, heating and stirring until the solution is clear, adding mesitylene (TMS) after the solution is cooled to a required temperature, adding Tetraethoxysilane (TEOS) as a precursor after the dropwise addition is finished, then adding polyvinyl alcohol microspheres as a dispersing agent, continuing heating and stirring for a period of time, cooling and standing after the reaction is finished, filtering, washing soluble salt components with distilled water, carrying out hydrothermal treatment on the obtained solution in a high-pressure kettle, filtering and drying the obtained solid, and calcining at a preset temperature to remove volatile components to obtain the SBA-15 microspheres.
According to a further technical scheme, in the step 2, the concentration mass ratio of the hydrochloric acid is 30-37%.
In the step 2, the surfactant P123 is dissolved in hydrochloric acid with a preset concentration, and ultrasonic pretreatment is performed before heating and stirring, so that dispersion is facilitated.
According to a further technical scheme, in the step 2, the heating temperature is controlled to be 30-55 ℃, and the stirring speed is controlled to be 70-120 r/min.
According to a further technical scheme, in the step 2, the cooling and standing time is 20-24 hours.
According to a further technical scheme, in the step 2, the calcining temperature is 500-600 ℃, and the calcining time is 3-10 hours.
According to the further technical scheme, in the step 2, the mass ratio of the raw materials is P123 to hydrochloric acid to TMB to TEOS to polyvinyl alcohol microspheres =1.0: 30-40: 0.3-1.0: 2.0-2.5: 0.3-0.7.
In a further technical scheme, in the step 1, the inorganic salt is hydrochloride or sulfate.
In a further technical scheme, the hydrochloride or the sulfate comprises one or a mixture of more of potassium chloride, sodium chloride, barium chloride, magnesium chloride, calcium chloride, potassium sulfate, sodium sulfate, barium sulfate, magnesium sulfate and calcium sulfate.
In the step 1, ultrasonic pretreatment is carried out on the solution before stirring reaction, which is beneficial to dispersion.
According to the further technical scheme, the reaction temperature of the polymerization is controlled to be 40-100 ℃, and the stirring speed is controlled to be 70-120 r/min.
The invention has the advantages of
The SBA-15 microspheres prepared by the method have the advantages of good dispersibility and uniformity.
Detailed Description
The essential features and advantages of the invention will be further explained below with reference to examples, but the invention is not limited to the examples listed.
The specific implementation mode is as follows:
embodiment 1:
dissolving 20g of polyvinyl alcohol in 250ml of deionized water, adding 5g of KCl and 4g of sodium hydroxide, dropwise adding 10ml of formaldehyde, treating for 2min by ultrasonic waves, heating to 50 ℃ in a water bath, stirring at a rotating speed of 100 r/min, and continuously stirring for reacting for 5 h. After the reaction, the mixture was cooled to room temperature, filtered, and the obtained solid was washed with anhydrous ethyl ether, filtered, and vacuum-dried to obtain 18.9g of polyvinyl alcohol microspheres.
Taking 250g of hydrochloric acid with the concentration of 37%, adding 7g of P123, carrying out ultrasonic pretreatment for 2min, heating to 40 ℃, stirring until the system is clear, cooling, dropwise adding 5g of TMB, 10g of TEOS and 3.5g of the prepared polyvinyl alcohol microspheres, heating to 50 ℃, stirring until all raw materials are completely dissolved, cooling to room temperature, and standing for 20 h. The deionized water washes the soluble salt components. And carrying out hydrothermal treatment on the obtained solution in a high-pressure kettle to obtain a solid, and filtering, drying and calcining at the high temperature of 550 ℃ for 7 hours to obtain 24.3g of SBA-15 microspheres.
Embodiment 2:
dissolving 30g of polyvinyl alcohol in 500ml of deionized water, adding 7g of barium sulfate and 6g of sodium hydroxide, dropwise adding 15ml of formaldehyde, treating for 2min by using ultrasonic waves, heating to 50 ℃ in a water bath, stirring at a rotating speed of 100 r/min, and continuously stirring for reacting for 6 h. After the reaction, the mixture is cooled to room temperature, filtered, and the obtained solid is washed by anhydrous ether, filtered and dried in vacuum to obtain 27.5g of polyvinyl alcohol microspheres.
Taking 300g of 35% hydrochloric acid, adding 10g of P123, carrying out ultrasonic pretreatment for 2min, heating to 40 ℃, stirring until the system is clear, cooling, dropwise adding 10g of TMB, 20g of TEOS and 7g of the prepared polyvinyl alcohol microspheres, heating to 50 ℃, stirring until all raw materials are completely dissolved, cooling to room temperature, and standing for 24 h. The deionized water washes the soluble salt components. And carrying out hydrothermal treatment on the obtained solution in a high-pressure kettle to obtain a solid, and filtering, drying and calcining the solid at the high temperature of 600 ℃ for 5 hours to obtain 45.7g of SBA-15 microspheres.
It should be noted that the above-mentioned preferred embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (11)
1. A preparation method of SBA-15 microspheres is characterized by comprising the following steps: dissolving inorganic salt with preset quality in a polyvinyl alcohol solution, adding a sodium hydroxide catalyst, stirring and reacting at a certain temperature, cooling and filtering to obtain polyvinyl alcohol microspheres;
step 2: dissolving a surfactant P123 in hydrochloric acid with a preset concentration, heating and stirring until the solution is clear, adding mesitylene (TMS) after the solution is cooled to a required temperature, adding Tetraethoxysilane (TEOS) as a precursor after the dropwise addition is finished, then adding polyvinyl alcohol microspheres as a dispersing agent, continuing heating and stirring for a period of time, cooling and standing after the reaction is finished, filtering, washing soluble salt components with distilled water, carrying out hydrothermal treatment on the obtained solution in a high-pressure kettle, filtering and drying the obtained solid, and calcining at a preset temperature to remove volatile components to obtain the SBA-15 microspheres.
2. The preparation method of SBA-15 microspheres according to claim 1, wherein the hydrochloric acid concentration in step 2 is 30-37% by mass.
3. The method for preparing SBA-15 microspheres according to claim 1, wherein in step 2, the surfactant P123 is dissolved in hydrochloric acid with a predetermined concentration, and is subjected to ultrasonic pretreatment before heating and stirring for facilitating dispersion.
4. The preparation method of SBA-15 microspheres according to claim 1, wherein in step 2, the heating temperature is controlled to be 30-55 ℃, and the stirring speed is controlled to be 70-120 r/min.
5. The preparation method of SBA-15 microspheres according to claim 1, wherein in step 2, the cooling and standing time is 20-24 hours.
6. The preparation method of SBA-15 microspheres according to claim 1, wherein in step 2, the calcination temperature is 500-600 ℃ and the calcination time is 3-10 hours.
7. The preparation method of the SBA-15 microsphere according to claim 1, wherein in the step 2, the mass ratio of the raw materials is P123: hydrochloric acid: TMB: TEOS: polyvinyl alcohol microsphere =1.0: 30-40: 0.3-1.0: 2.0-2.5: 0.3-0.7.
8. The method for preparing SBA-15 microspheres according to claim 1, wherein in step 1, said inorganic salt is hydrochloride or sulfate.
9. The method for preparing SBA-15 microspheres according to claim 8, wherein the hydrochloride or sulfate comprises one or more of potassium chloride, sodium chloride, barium chloride, magnesium chloride, calcium chloride, potassium sulfate, sodium sulfate, barium sulfate, magnesium sulfate, and calcium sulfate.
10. The method for preparing SBA-15 microspheres according to claim 1, wherein in step 1, the solution is pretreated by ultrasonic wave before stirring reaction for dispersion.
11. The preparation method of the SBA-15 microsphere according to claim 1, wherein the reaction temperature of the polymerization is controlled to be 40-100 ℃, and the stirring rate is controlled to be 70-120 r/min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872684A (en) * | 2006-06-16 | 2006-12-06 | 清华大学 | Method for synthesizing microspheres of high ordered mesoporous silicon dioxide |
| US20110226990A1 (en) * | 2008-11-26 | 2011-09-22 | Glennon Jeremy D | process for preparing silica microparticles |
| CN102515173A (en) * | 2011-12-05 | 2012-06-27 | 聊城大学 | Method for preparing mesoporous SBA-15 unstuck micro spheres |
| CN103536973A (en) * | 2013-10-25 | 2014-01-29 | 北京大学 | Polyvinyl alcohol magnetic particles as well as preparation method and application thereof |
| CN104353424A (en) * | 2014-11-24 | 2015-02-18 | 辽宁大学 | Amine-containing functional mesoporous material and application thereof to separation of rhenium and molybdenum |
| CN108483453A (en) * | 2018-04-23 | 2018-09-04 | 东北大学 | A kind of preparation method of SBA-15 types mesoporous silicon dioxide micro-sphere |
-
2021
- 2021-05-13 CN CN202110520504.6A patent/CN113307276A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872684A (en) * | 2006-06-16 | 2006-12-06 | 清华大学 | Method for synthesizing microspheres of high ordered mesoporous silicon dioxide |
| US20110226990A1 (en) * | 2008-11-26 | 2011-09-22 | Glennon Jeremy D | process for preparing silica microparticles |
| CN102515173A (en) * | 2011-12-05 | 2012-06-27 | 聊城大学 | Method for preparing mesoporous SBA-15 unstuck micro spheres |
| CN103536973A (en) * | 2013-10-25 | 2014-01-29 | 北京大学 | Polyvinyl alcohol magnetic particles as well as preparation method and application thereof |
| CN104353424A (en) * | 2014-11-24 | 2015-02-18 | 辽宁大学 | Amine-containing functional mesoporous material and application thereof to separation of rhenium and molybdenum |
| CN108483453A (en) * | 2018-04-23 | 2018-09-04 | 东北大学 | A kind of preparation method of SBA-15 types mesoporous silicon dioxide micro-sphere |
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