CN112194139B - Preparation method of mesoporous rod-like silicon dioxide - Google Patents
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- CN112194139B CN112194139B CN202011262123.4A CN202011262123A CN112194139B CN 112194139 B CN112194139 B CN 112194139B CN 202011262123 A CN202011262123 A CN 202011262123A CN 112194139 B CN112194139 B CN 112194139B
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Abstract
The invention provides a preparation method of mesoporous rod-shaped silicon dioxide, which is characterized in that silicate is used as a raw material and added into a template agent, alkali solution is added after the silicate is uniformly stirred to form a mixed solution, then pure water is used for suction filtration and washing, and the template is removed through high-temperature calcination after drying to obtain the mesoporous rod-shaped silicon dioxide. The mesoporous rod-like silicon dioxide prepared by the method has the advantages of uniform appearance, good dispersibility, few preparation process steps, simple and convenient operation and convenience for large-scale production.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a preparation method of mesoporous rod-like silicon dioxide.
Background
As is well known, silica materials have wide range and good biocompatibility, wherein the silica fibers with mesoporous structures have wide application prospects in the fields of adsorption, separation and catalysts due to excellent optical, electrical and special morphological structures, but the shape, size and dispersibility of the mesoporous silica in practical application influence the use effect. At present, the main methods for preparing the silica fiber are an electrostatic spinning method, a sol-gel method and a hard template method, and although the nano or micron silica fiber can be prepared, the methods have certain disadvantages and have certain obstruction in large-scale industrialization.
In patent publication No. CN107354516A entitled "porous silica fiber electrospinning solution" and "method for preparing porous silica fibers by electrospinning method", it is disclosed that a porous silica fiber having good flexibility is prepared by electrospinning a solution prepared by mixing silica sol, polyvinyl alcohol and a pore-forming agent, but the method uses an organic silicon source as a raw material and requires a fixed electrospinning machine, which is complicated in process.
In a patent with the publication number of CN101602507B and the patent name of a one-dimensional rod-shaped mesoporous material and a preparation method and application thereof, the rod-shaped material with the length-diameter ratio of 50 is prepared by using a hard template, namely a composite mesoporous film, the size of the rod-shaped material prepared by the method is easily influenced by a template agent, and an organic solvent methylene dichloride is required to be used for dissolving the template in the subsequent process, so that the method is not green and environment-friendly.
In a patent with publication No. CN1240615C, entitled mesoporous silica fiber preparation method, a method for preparing a hundred micron silica fiber using an organic silicon source under a strong acid condition containing a surfactant is disclosed. However, the method has the disadvantages of non-uniform fiber product morphology, low yield and long reaction period, and generally requires 1 to 3 days.
In a patent with publication number CN108793174A and the patent name of mesoporous silica fiber and a preparation method thereof, a nano rod-shaped material is prepared under hydrothermal conditions by using a special Gemini surfactant with a head group containing four hydroxyl groups as a template agent.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of mesoporous rod-shaped silicon dioxide, and the mesoporous rod-shaped silicon dioxide prepared by the method has uniform appearance and controllable size.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of mesoporous rod-shaped silicon dioxide comprises the following steps:
the method comprises the following steps: dissolving a template agent in an acid solution, and stirring until the solution is clear to form a solution A;
step two: dissolving silicate in water, and stirring until the solution is clear to form a solution B;
step three: pouring the solution B into the solution A, mixing, and stirring uniformly to form a solution C;
step four: adding diluted alkaline solution into the solution C, uniformly stirring, and standing until the reaction is finished to form a mixed solution D;
step five: and (3) carrying out suction filtration and washing on the mixed solution D after the reaction is finished by using pure water, drying, calcining for 4-6 hours at the temperature of 500-700 ℃ to remove the template, and obtaining the micron-sized mesoporous rod-shaped silicon dioxide.
Preferably, the template in the first step is any one or a mixture of two or more selected from triton X100, cetyltrimethylammonium bromide (CTAB) and Sodium Dodecylbenzenesulfonate (SDBS).
Preferably, the mass ratio of the silicate to the water in the solution B is 4-5: 30-40.
Preferably, the acidic solution in the first step is any one or a mixture of two or more selected from nitric acid, sulfuric acid, hydrochloric acid and acetic acid.
Preferably, the mass ratio of the template agent to the acidic solution to the water in the solution A is 1-4: 1-10: 50-300.
Preferably, in the third step, the stirring time is 2-4 hours.
Preferably, in the fourth step, the stirring time is 15-30 seconds.
Preferably, in the fourth step, the alkali solution is any one or a mixture of several of sodium hydroxide, ammonia water and potassium hydroxide.
Preferably, in the fourth step, the mass ratio of the alkali solution to the water is 0.2-4: 50-100.
Preferably, in the fourth step, the stirring time is 15-30 seconds; the standing time is 1-3 hours.
In the preparation method of the mesoporous rod-shaped silicon dioxide, the size of the rod-shaped silicon dioxide is controlled by adjusting the pH value of the acidic solution; the morphology and the dispersity of the silicon dioxide can be controlled by controlling the adding amounts of the template agent and the silicate, the size of the rod-shaped silicon dioxide can be controlled, and the morphology and the dispersity of the silicon dioxide can be controlled by controlling the adding amounts of the template agent and the silicate. In the preparation method, silicate is always hydrolyzed under an acidic condition in the early stage, and self-assembly is carried out according to the micelle shape of the template agent under an alkaline condition in the later stage to form micron-sized silicon dioxide. The rod-like structure of the silicon dioxide is realized by controlling the proportion of the silicate and the template.
Compared with the prior art, the silicon dioxide prepared by the preparation method has the characteristics of uniform appearance, good dispersion performance and controllable size, and is micron-sized mesoporous rod-shaped silicon dioxide.
The invention uses weak acid condition to hydrolyze according to soft template, and polycondensation forming technique under alkaline condition, with low requirement for condition, less steps, and convenient and simple operation. The inorganic silicon source silicate used in the invention has low raw material cost and high yield, and is convenient for large-scale industrial production.
Drawings
FIG. 1 is an SEM image of the mesoporous rod-shaped silica obtained in example 1;
FIG. 2 is an EDS chart of the mesoporous rod silica composition obtained in example 1;
FIG. 3 is an SEM image of the mesoporous rod-shaped silica obtained in example 2;
FIG. 4 is an SEM image of the mesoporous rod-shaped silica obtained in example 3;
FIG. 5 is an SEM image of the mesoporous rod-shaped silica obtained in example 4.
FIG. 6 is an SEM image of the mesoporous rod-shaped silica obtained in example 5;
FIG. 7 is an SEM image of the mesoporous rod-shaped silica morphology obtained in example 6.
Detailed Description
The invention will be further described with reference to examples of embodiments shown in the drawings to which the invention is attached. However, the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not mentioned are conventional conditions in the industry. The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1:
the method comprises the following steps: adding 3g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 1.5g of triton X100 in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 4g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, stirring for 30s, stopping, and standing at room temperature for 2h to form a mixed solution D with white floccules;
step six; filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining for 5 hours at 550 ℃ to remove the template, and obtaining the mesoporous rod-like silicon dioxide.
Referring to fig. 1, fig. 1 is an SEM image of the obtained product, and it can be seen that the obtained mesoporous rod-shaped silica has a mesoporous rod-shaped morphology, no entanglement, good dispersion, and a size of 25-50 μm. FIG. 2 is the EDS diagram of the product, the composition of which is silica.
Example 2:
the method comprises the following steps: adding 3g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 0.3g of triton X100 in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 4g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, stirring for 30s, stopping, and standing at room temperature for 2h to form a mixed solution D with white floccules;
step six; filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining the mixture for 5 hours at 550 ℃ to remove the template, thus obtaining the spherical silicon dioxide.
As shown in figure 3, the addition amount of the template agent is reduced, and the obtained silica is 10-25 microns spherical silica, the morphology of which is changed and is not rod-shaped silica any longer. Experiments show that the control of the proportion of the silicate and the template is the key for realizing the rod-shaped structure of the silicon dioxide, and the obtained silicon dioxide is non-rod-shaped when the proportion exceeds the set proportion range.
Example 3:
the method comprises the following steps: adding 3g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 1.5g of triton X100 in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 1g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, stirring for 30s, stopping, and standing at room temperature for 2h to form a mixed solution D with white floccules;
step six; filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining the mixture for 5 hours at 550 ℃ to remove the template, and obtaining the irregular-shaped silicon dioxide agglomerates.
As shown in figure 4, the addition of silicate is reduced to obtain irregular-shaped silicon dioxide agglomerates, and the dispersibility of the irregular-shaped silicon dioxide agglomerates is poor while the morphology is changed.
Example 4:
all the steps of example 1 were repeated except that the alkali solution and the solution C in the fifth step were kept standing without mixing and stirring.
The method comprises the following steps: adding 3g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 1.5g of triton X100 in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 4g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, and standing for 2 hours at room temperature to form a mixed solution D with white floccules;
step six; filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining the mixture for 5 hours at 550 ℃ to remove the template, and obtaining the irregular-shaped silicon dioxide agglomerates.
As shown in FIG. 5, if the mixing and stirring are not carried out, the reaction does not proceed sufficiently, and irregular-shaped silica agglomerates are obtained, and the self-dispersibility is poor.
Example 5:
the method comprises the following steps: adding 5g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 1.5g of triton X100 in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 4g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, stirring for 30s, stopping, and standing at room temperature for 2h to form a mixed solution D with white floccules;
step six: filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining for 5 hours at 550 ℃ to remove the template, and obtaining the mesoporous rod-like silicon dioxide.
As shown in figure 6, the acid solution concentration is increased, and the pH value is reduced to obtain the micron-sized mesoporous rod-shaped silica with rough surface and 10-25 microns of size.
Example 6:
the method comprises the following steps: adding 3g of acetic acid into 110g of water, uniformly stirring to form an acid solution, dissolving 0.5g of triton X100 and 1.0g of CTAB in the acid solution, and stirring the solution by using a magnetic stirrer until the solution is clarified to form a solution A;
step two: dissolving 4g of zero-water sodium metasilicate in 30g of water, and stirring until the solution is clear to form solution B;
step three: pouring the solution B into the stirred solution A, and stirring at a low speed for 2 hours to form a solution C;
step four: diluting 3g of ammonia water by 100 times to form an alkali solution;
step five: adding the diluted alkaline solution into the solution C, stirring for 30s, stopping, and standing at room temperature for 2h to form a mixed solution D with white floccules;
step six: filtering and washing the mixed solution D with pure water, and drying in an oven; then calcining for 5 hours at 550 ℃ to remove the template, and obtaining the mesoporous rod-like silicon dioxide.
As shown in figure 7, the kind of micelle substance is changed from micelle to mixed micelle, and the micron-sized mesoporous rod-shaped silica is obtained, but the surface is rough, and the size is 5-15 microns.
In the preparation method of the mesoporous rod-shaped silicon dioxide, a template is dissolved in an acid solution and stirred to be clear, and in a formed solution A, the mass ratio of the template to the acid solution to water is 1-4: 1-10: 50-300, and in some embodiments, the mass ratio of the template agent to the acidic solution to the water is 1: 2-8: 60-200 or 1: 2-4: 70-200.
The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.
Claims (8)
1. A preparation method of mesoporous rod-like silicon dioxide is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dissolving a template agent in an acid solution, and stirring until the solution is clear to form a solution A, wherein the mass ratio of the template agent to the acid solution to water in the solution A is 1-4: 1-10: 50-300 parts of;
step two: dissolving silicate in water, and stirring until the solution is clear to form a solution B, wherein the mass ratio of the silicate to the water in the solution B is 4-5: 30-40;
step three: pouring the solution B into the solution A, mixing to perform hydrolysis reaction, and stirring uniformly to form a solution C;
step four: adding diluted alkaline solution into the solution C to perform self-assembly reaction of polycondensation forming, uniformly stirring, and standing until the reaction is finished to form a mixed solution D;
step five: and (3) carrying out suction filtration and washing on the mixed solution D after the reaction is finished by using pure water, drying, calcining for 4-6 hours at the temperature of 500-700 ℃ to remove the template, and obtaining the micron-sized mesoporous rod-shaped silicon dioxide.
2. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: the template agent in the first step is any one or a mixture of two or more of triton X100, Cetyl Trimethyl Ammonium Bromide (CTAB) and Sodium Dodecyl Benzene Sulfonate (SDBS).
3. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: the acidic solution in the first step is any one or a mixture of two or more of nitric acid, sulfuric acid, hydrochloric acid and acetic acid.
4. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: in the third step, the stirring time is 2-4 hours.
5. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: in the fourth step, the stirring time is 15-30 seconds.
6. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: in the fourth step, the alkali solution is any one or a mixture of sodium hydroxide, ammonia water and potassium hydroxide.
7. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: in the fourth step, the mass ratio of the alkali solution to the water is 0.2-4: 50-100.
8. The method for preparing mesoporous rod-shaped silica according to claim 1, wherein: in the fourth step, the stirring time is 15-30 seconds; the standing time is 1-3 hours.
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| CN113698188B (en) * | 2021-08-20 | 2023-03-31 | 南京理工大学 | Method for preparing silicon dioxide fiber with rectangular cross section by taking silica sol as raw material |
| CN116375035A (en) * | 2023-03-15 | 2023-07-04 | 湖北斯诺新材料科技有限公司 | Preparation method of three-dimensional porous silicon-carbon composite material and composite material thereof |
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| CN1264747C (en) * | 2003-08-12 | 2006-07-19 | 中国科学院理化技术研究所 | columnar mesoporous silicon dioxide and preparation method thereof |
| CN101704527B (en) * | 2009-12-15 | 2013-06-26 | 南开大学 | Monodisperse mesoporous silica nano-particle with controllable appearance and synthesis method thereof |
| CN103224239A (en) * | 2013-04-08 | 2013-07-31 | 天津大学 | Chiral mesoporous silica nano-rod and preparation method thereof |
| CN103803560B (en) * | 2014-01-23 | 2015-10-07 | 齐鲁工业大学 | A kind of bending bar-shaped mesoporous SiO 2and preparation method thereof |
| CN107827118A (en) * | 2017-11-24 | 2018-03-23 | 北京欧美中科学技术研究院 | A kind of preparation method of the adjustable mesoporous silica hollow ball of shell thickness |
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