CN109574031B - Method for synthesizing ordered mesoporous silica molecular sieve SBA-15 by high-temperature ultrasonic calcination method - Google Patents
Method for synthesizing ordered mesoporous silica molecular sieve SBA-15 by high-temperature ultrasonic calcination method Download PDFInfo
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- CN109574031B CN109574031B CN201811407718.7A CN201811407718A CN109574031B CN 109574031 B CN109574031 B CN 109574031B CN 201811407718 A CN201811407718 A CN 201811407718A CN 109574031 B CN109574031 B CN 109574031B
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Abstract
The invention discloses a method for synthesizing an ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method, which is based on the fact that a surfactant is used as a template agent, a silicon source and other auxiliary agents are used for regulating and controlling the micro morphology of the SBA-15, and the effect of rapid preparation is achieved by the high-temperature ultrasonic calcination method, so that the ordered porous material SBA-15 with the particle size of 1-2 um can be prepared. The prepared SBA-15 has highly ordered pore size and easy dispersibility, and can be widely applied to the aspects of drug loading, adsorption, separation, macromolecule catalysis, functional material preparation and the like.
Description
Technical Field
The invention relates to a method for synthesizing an ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method.
Background
In recent years, porous materials are receiving more and more attention from material science research, and are suitable for the directions of drug loading, adsorption, separation, macromolecular catalysis, functional material preparation and the like as a novel material system with wide application prospect. The advantages are regular pore diameter arrangement, adjustable size, high specific surface area, high porosity, high thermal stability and high water stability.
According to the IUPAC specification, the porous materials are classified into three types according to their size. The first, called micropores (micro pores) with a size less than 2nm, such as zeolites, organic tissues, etc., the second, called macropores (macropores) with a size greater than 50nm, such as vitamins, polyester materials, etc., the third, called mesopores or mesopores (mesopores) with a size between 2nm and 50nm, such as si (oet)4, Al (i-OPr)3, etc. The upper limit of three pore classes is typically 100 nm.
Researchers at Mobil corporation in 1992 have gradually attracted attention from the sol-gel method using hexadecyltrimethylammonium salt as a template to obtain mesoporous M41S silica materials. The group of the Zhao Dongyuan project in 1998 uses a block copolymer (nonionic surfactant) as a template in an acid synthesis system to prepare a mesoporous molecular sieve SBA-15 with ordered large pore diameter, which brings breakthrough progress of mesoporous material synthesis.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing an ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method, and the method is used as a load.
The purpose of the invention is realized by the following scheme: a method for synthesizing a length-adjustable ordered mesoporous molecular sieve SBA-15 by a high-temperature ultrasonic calcination method is characterized in that a surfactant is used as a template agent, a silicon source is used, other auxiliary agents are used for regulating and controlling the micro morphology of the SBA-15, and the effect of rapid preparation is achieved by the high-temperature ultrasonic calcination method, and the method specifically comprises the following steps:
a. weighing 20g of template agent, dissolving the template agent in 400ml of 4 mol/L acid solution, stirring the solution at a temperature of 15 +/-0.5 ℃ by using a uniform stirrer until the solution is clear and transparent;
b. then slowly dripping 5g of silicon source into the solution a by using a burette, stirring at a high speed for 15 min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 12 h;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min at the temperature of 95-100 ℃;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and finally, heating the reaction product in the step d to 300 ℃ at a speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15 with the particle size of 1-2 um.
The selected silicon source is any one of tetrapropyl orthosilicate, tetrabutyl orthosilicate, tetramethyl orthosilicate or tetraethyl orthosilicate.
Adding auxiliary active agents: the addition of the cationic active agent, the anionic active agent and the nonionic active agent is 1 time of that of the template agent.
The acid added is oxalic acid.
A method for synthesizing a length-adjustable ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method is characterized in that a surfactant (P123) is used as a template agent, Tetraethoxysilane (TEOS) is used as a silicon source, other auxiliary agents are used for regulating and controlling the micro morphology of the SBA-15, and the effect of rapid preparation is achieved by the high-temperature ultrasonic calcination method, and the method specifically comprises the following steps:
a. weighing 20g of P123, dissolving in 400ml of 4 mol/L oxalic acid solution, stirring at 15 +/-0.5 ℃ by using a uniform speed stirrer until the solution is clear and transparent;
b. slowly dripping 5g TEOS into the solution a by using a burette, stirring at a high speed for 15 min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 12 h;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min at the temperature of 95-100 ℃;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and finally, heating the reaction product in the step d to 300 ℃ at a speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15 with the particle size of 1-2 um.
The invention has the advantages that: the SBA-15 prepared by the method has highly ordered pore size and easy dispersibility, and can be widely applied to the aspects of drug loading, adsorption, separation, macromolecular catalysis, functional material preparation and the like.
Drawings
FIG. 1 SEM photograph of a synthesized product of example 1;
FIG. 2 TEM image of the synthesized product of example 1;
FIG. 3 SEM photograph of the synthesized product of example 2;
FIG. 4 TEM image of the synthesized product of example 2;
FIG. 5 SEM photograph of the synthesized product of example 3;
figure 6 TEM image of the product of example 3 synthesis.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
A method for synthesizing a length-adjustable ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method is based on that a surfactant is used as a template agent, a silicon source and other auxiliary agents are used for regulating and controlling the micro morphology of the SBA-15, and the high-temperature ultrasonic calcination method is used for achieving rapid preparation, and comprises the following steps:
a. weighing 20g of template agent P123, dissolving in 400ml of 4 mol/L oxalic acid solution, stirring to obtain clear and transparent solution a at 15 +/-0.5 ℃ by using a uniform speed stirrer;
b. then slowly dripping 5g TEOS (tetraethyl orthosilicate) into the solution a, stirring for 15 min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 12 h to obtain a white product;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min by using the heating plate at the temperature of 95-100 ℃ to obtain a product;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and finally, heating to 300 ℃ at the speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15 with the particle size of 1-2 um.
The scanning electron microscope is shown in FIG. 1, and the transmission electron microscope is shown in FIG. 2, which shows SBA-15 with an average length of 1um, 1-2 um and a pore diameter of 1-4 nm.
Example 2
The method for synthesizing the ordered mesoporous silica molecular sieve SBA-15 with adjustable length by a high-temperature ultrasonic calcination method has the similar steps to the example 1, and comprises the following steps:
a. weighing 18g of P123, dissolving in 400ml of 3 mol/L oxalic acid solution, stirring at 15 +/-0.5 ℃ by using a uniform stirrer until a clear and transparent solution a is obtained;
b. then slowly dripping 4g TEOS (tetraethyl orthosilicate) into the solution a, stirring for 13min, putting into an ultrasonic device, carrying out ultrasonic treatment for 8min, and standing in a water bath at 15 ℃ for aging for 8 h to obtain a white product;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min by using the heating plate at the temperature of 95-100 ℃;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and finally, heating to 400 ℃ at the speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15.
The SBA-15 displayed by a scanning electron microscope (as shown in FIG. 3) and a transmission electron microscope (as shown in FIG. 4) has an average length of 1.6um, 1.5-2.5 um and a pore diameter of 6-8 nm.
EXAMPLE 3
The method for synthesizing the ordered mesoporous silica molecular sieve SBA-15 with adjustable length by a high-temperature ultrasonic calcination method has the similar steps to the example 1, and comprises the following steps:
a. weighing 22g of P123, dissolving in 400ml of 5 mol/L oxalic acid solution, stirring at 15 +/-0.5 ℃ by using a uniform stirrer until a clear and transparent solution a is obtained;
b. then slowly dripping 6g TEOS (tetraethyl orthosilicate) into the solution a, stirring for 18 min, performing ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 16 h to obtain a white product;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min by using the heating plate at the temperature of 95-100 ℃;
d. then, carrying out suction filtration, washing with water, and drying in an oven to obtain white powder;
e. and finally, heating to 500 ℃ at the speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15.
The SBA-15 shown by a scanning electron microscope (FIG. 5) and a transmission electron microscope (FIG. 6) has an average length of 856nm, 0.5-0.9 um, and a pore diameter of 3-6 nm.
Claims (4)
1. A method for synthesizing a length-adjustable ordered mesoporous silica molecular sieve SBA-15 by a high-temperature ultrasonic calcination method is characterized in that the method is based on that a surfactant is used as a template agent, a silicon source and other auxiliary agents are used for regulating and controlling the micro morphology of the SBA-15, and the rapid preparation is realized by the high-temperature ultrasonic calcination method, and comprises the following steps:
a. weighing 20g of template agent, dissolving the template agent in 400ml of 4 mol/L acid solution, and stirring the solution at the temperature of 15 +/-0.5 ℃ until the solution is clear and transparent, wherein the acid is oxalic acid;
b. slowly dripping 5g of silicon source into the solution a by using a burette, stirring at a high speed for 15 min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 12 h to obtain a white product;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting at 95-100 ℃ for 10min to obtain a product;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and d, finally, heating the white powder in the step d to 300 ℃ at a speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15 with the particle size of 1-2 um.
2. The method for synthesizing the ordered mesoporous silica molecular sieve SBA-15 with adjustable length by the high-temperature ultrasonic calcination method according to claim 1, wherein the selected silicon source is any one of tetrapropyl orthosilicate, tetrabutyl orthosilicate, tetramethyl orthosilicate or tetraethyl orthosilicate.
3. The method for synthesizing the ordered mesoporous silica molecular sieve SBA-15 with adjustable length by the high-temperature ultrasonic calcination method according to claim 1, wherein the auxiliary other auxiliary agent is an additive auxiliary active agent, comprising: the addition amount of the cationic active agent, the anionic active agent and/or the nonionic active agent is 1 time of that of the template agent.
4. The method for synthesizing the ordered mesoporous silica molecular sieve SBA-15 with the adjustable length by the high-temperature ultrasonic calcination method according to claim 1, wherein the surfactant P123 is used as a template agent, Tetraethoxysilane (TEOS) is used as a silicon source, other auxiliary agents are used for regulating and controlling the micro-morphology of the SBA-15, and the high-temperature ultrasonic calcination method is used for achieving the effect of rapid preparation, and the method comprises the following specific steps:
a. weighing 20g of P123, dissolving in 400ml of 4 mol/L oxalic acid solution, stirring at 15 +/-0.5 ℃ by using a uniform stirrer until a clear and transparent solution a is obtained;
b. slowly dripping 5g TEOS into the solution a by using a burette, stirring at a high speed for 15 min, putting into an ultrasonic device, carrying out ultrasonic treatment for 10min, and standing in a water bath at 15 ℃ for aging for 12 h;
c. b, transferring the white product obtained in the step b to a sealed heating plate, and reacting for 10min at the temperature of 95-100 ℃;
d. c, carrying out suction filtration and washing on the product obtained in the step c, and drying in an oven to obtain white powder;
e. and d, finally, heating the white powder obtained in the step d to 300 ℃ at a speed of 2 ℃/min in the air, and roasting for 4 h to obtain the ordered porous material SBA-15 with the particle size of 1-2 um.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342605A (en) * | 2001-08-20 | 2002-04-03 | 复旦大学 | Process for synthesizing mesoporous silicon oxide molecular sieve material by ultrasonic system |
| CN1356265A (en) * | 2001-08-20 | 2002-07-03 | 复旦大学 | Process for preparing shape-controllable big-pore mesoporous molecular sieve |
| CN1730389A (en) * | 2005-06-17 | 2006-02-08 | 朱广山 | Ultrasonic method for synthesizing mesoporous monox nanometer ball carrier material |
| CN106517227A (en) * | 2016-11-08 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Microwave method for rapidly preparing short-rod-like SBA-15 |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342605A (en) * | 2001-08-20 | 2002-04-03 | 复旦大学 | Process for synthesizing mesoporous silicon oxide molecular sieve material by ultrasonic system |
| CN1356265A (en) * | 2001-08-20 | 2002-07-03 | 复旦大学 | Process for preparing shape-controllable big-pore mesoporous molecular sieve |
| CN1730389A (en) * | 2005-06-17 | 2006-02-08 | 朱广山 | Ultrasonic method for synthesizing mesoporous monox nanometer ball carrier material |
| CN106517227A (en) * | 2016-11-08 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Microwave method for rapidly preparing short-rod-like SBA-15 |
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