CN113666421B - Preparation method of manganese dioxide coated mesoporous silicon dioxide nano flower material - Google Patents
Preparation method of manganese dioxide coated mesoporous silicon dioxide nano flower material Download PDFInfo
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- CN113666421B CN113666421B CN202110835459.3A CN202110835459A CN113666421B CN 113666421 B CN113666421 B CN 113666421B CN 202110835459 A CN202110835459 A CN 202110835459A CN 113666421 B CN113666421 B CN 113666421B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/45—Aggregated particles or particles with an intergrown morphology
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Abstract
A preparation method of a nano flower material with manganese dioxide coating mesoporous silicon dioxide relates to the technical field of nano materials. The method obtains the nano flower composite material with the pore structure by constructing an alkaline reaction environment by using mesoporous silicon dioxide as a growth template and utilizing the principle that potassium permanganate and manganese ions are subjected to redox reaction to generate manganese dioxide nano sheets under the condition of normal temperature. The invention provides a preparation method of a manganese dioxide coated mesoporous silica nanoflower material which is low in preparation cost, simple in preparation method, mild in reaction condition and high in specific surface area, and can be used in the field of biomedical diagnosis and treatment.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a manganese dioxide coated mesoporous silica nano flower material.
Background
The mesoporous silica nano material has a unique nano structure, such as a regular pore channel structure, higher specific surface area, stable chemical and mechanical strength, good biocompatibility and easy surface functional modification. Due to the characteristic that the mesoporous silica nano material is easy to functionalize, the organic-hybrid mesoporous material formed by functionalizing the organic group can be more applied to various fields of biomedicine, environmental protection, industrial catalysis, new energy and the like.
Manganese dioxide is a bright-future photo-thermal electro-responsive semiconductor material, and is an important inorganic functional material with great application potential in the fields of energy, catalysis, electronics, electrochemistry, medicine and the like due to the characteristics of strong oxidizability, good adsorption capacity, high abundance, good acid resistance, small toxicity, narrow forbidden band, low price, no toxicity, environmental protection, high specific capacity and the like. So far, various methods for synthesizing manganese dioxide include hydrothermal synthesis, chemical precipitation, sol-gel method, template method, electrochemical method, etc., and manganese dioxide crystals (such as nanorods, nanowires, nanofibers, nanotubes, nanobelts, nanosheets, nanoflowers, etc.) with various morphologies have been obtained, but most of these methods have various processes, strict equipment requirements, and different morphologies and properties of products. Therefore, the preparation method provided by the invention is to obtain the nanoflower composite material with the pore structure by constructing an alkaline reaction environment by using mesoporous silicon dioxide as a growth template and utilizing the principle that potassium permanganate and manganese ions are subjected to redox reaction to generate manganese dioxide nanosheets under the normal temperature condition, and solves the problems of complex preparation process, harsh conditions and the like of the traditional manganese dioxide.
Disclosure of Invention
The invention aims to provide a preparation method of a manganese dioxide coated mesoporous silica nanoflower material which is low in preparation cost, simple in preparation method, mild in reaction condition and high in specific surface area, and can be used in the field of biomedical diagnosis and treatment.
In a first aspect of the present invention, the present invention provides a method for preparing a nanoflower material of manganese dioxide-coated mesoporous silica.
According to an embodiment of the invention, the method comprises: (1) preparing a mesoporous silica template; (2) And (3) preparing mesoporous silica/manganese dioxide nanoflowers.
The inventor finds that by adopting the preparation method of the embodiment of the invention, the nano flower composite material with the pore structure is obtained by using mesoporous silicon dioxide as a growth template and utilizing the principle that potassium permanganate and manganese ions are subjected to redox reaction to generate manganese dioxide nano sheets under the condition of normal temperature and by creating an alkaline reaction environment. The composite material has higher specific surface area, easy surface functional modification and good biocompatibility, is an ideal carrier material and can be used in the field of biomedical diagnosis and treatment.
In order to achieve the purpose, the method for coating the nano flower material of the mesoporous silica by the manganese dioxide adopts the following technical scheme:
1) Preparing a mesoporous silica template:
adding 0.36 g triethanolamine into 72 ml deionized water and 48 ml hexadecyl trimethyl ammonium chloride solution with solute mass of 25%, rotating speed of 250 r/min, preheating for 1 hour under 60 ℃ oil bath condition; 36 ml of cyclohexane and 4 ml of tetraethyl silicate are mixed evenly, after the solution is preheated, a disposable plastic dropper is used for entering the flask by swirling along the mouth of the round bottom flask, and then the stirring is continued for 17 hours under the conditions of 250 r/min and 60 ℃ oil bath at constant temperature. And (3) after the reaction is finished, an obvious solution layering phenomenon can be seen, the upper oil phase solution is taken out and discarded, and the volume ratio of the lower water phase solution to ethanol is 1:3, and centrifuging at 9000 rpm for 3 minutes. And then washing the centrifuged precipitate for 3 times by using ethanol, wherein the centrifugation conditions of 3 times of washing are 10000 r/min, the time is 5 min, then placing the precipitate in a drying oven for drying at 60 ℃, grinding the dried sample, and calcining the ground sample at 540 ℃ for 2 h to obtain white powder solid, namely the mesoporous silicon dioxide.
Preparing mesoporous silica/manganese dioxide nanoflowers:
weighing 50 mg of the prepared mesoporous silica, ultrasonically dispersing the mesoporous silica in 20 ml of ultrapure water, and ultrasonically treating for 5 minutes; adding 70 mg of tetrahydrate manganese acetate and 150 mg of ammonium chloride into 10 ml of ultrapure water, ultrasonically dissolving, adding into the mesoporous silica solution, and stirring on a magnetic stirrer rotating at 300 revolutions; adding 30 mg of potassium permanganate into 3 ml of ultrapure water, ultrasonically dissolving, then sucking the potassium permanganate solution by using a 200 microliter liquid-transferring gun, dropwise adding the potassium permanganate solution into the mixed solution, stirring for 2 minutes, then adding 150 microliter of 28wt% ammonia water into the mixed solution, placing the mixed solution in a magnetic stirrer, and stirring overnight under the condition of 300 revolutions. Centrifuging the sample solution for 10 minutes under the condition of 10000 revolutions after the reaction is finished, separating out precipitate, washing the precipitate by ultrapure water for 3 times, centrifuging the precipitate for 10 minutes at the centrifugal rotating speed of 10000 revolutions after each washing, then drying the washed sample in a drying box at the temperature of 60 ℃, and grinding the dried sample to obtain the brown powdery mesoporous silica/manganese dioxide nanoflower material.
The mesoporous silica/manganese dioxide nanoflower prepared by the invention has the advantages of higher specific surface area, easy surface functional modification and good biocompatibility, is an ideal carrier material, and can be used in the field of biomedical diagnosis and treatment. In addition, the invention provides the preparation method of the mesoporous silica/manganese dioxide nanoflower material, which is simple to operate, mild in reaction conditions and low in raw material cost, and simultaneously solves the problems of complex preparation process, harsh conditions and the like of the traditional manganese dioxide.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a transmission electron microscope image of mesoporous silica prepared according to the present invention;
FIG. 2 is a transmission electron microscope image of the mesoporous silica/manganese dioxide nanoflower material prepared according to the present invention;
FIG. 3 is a diagram of the nitrogen adsorption pore diameter of the mesoporous silica/manganese dioxide nanoflower material prepared by the present invention;
FIG. 4 is an X-ray diffraction pattern of a mesoporous silica/manganese dioxide nanoflower material prepared in accordance with the present invention;
Detailed Description
Example 1:
1) Preparing a mesoporous silica template: adding 0.36 g triethanolamine into 72 ml deionized water and 48 ml hexadecyl trimethyl ammonium chloride solution with solute mass of 25%, rotating speed of 250 r/min, preheating for 1 hour under 60 ℃ oil bath condition; and (3) uniformly mixing 36 ml of cyclohexane and 4 ml of tetraethyl silicate, after the solution is preheated, enabling the solution to swirl along the mouth of the round-bottom flask by using a disposable plastic dropper to enter the flask, and then continuously stirring the solution at the constant temperature for 17 hours under the conditions of 250 revolutions per minute and 60 ℃ oil bath. After the reaction is finished, the solution has obvious layering phenomenon, the upper oil phase solution which is well reacted is taken out and discarded, and the lower water phase solution and ethanol are mixed according to the volume ratio of 1:3, and centrifuging at 9000 rpm for 3 minutes. And then washing the centrifuged precipitate for 3 times by using ethanol, wherein the centrifugation conditions of 3 times of washing are 10000 r/min and 5 minutes later, then placing the precipitate in a drying oven for drying at 60 ℃, grinding the dried sample, and calcining the dried sample for 2 hours at 540 ℃ to obtain the mesoporous silicon dioxide.
2) Preparing a mesoporous silicon dioxide/manganese dioxide nanoflower material: weighing 50 mg of mesoporous silica, ultrasonically dispersing in 20 ml of ultrapure water, and ultrasonically treating for 5 minutes; adding 70 mg of tetrahydrate manganese acetate and 150 mg of ammonium chloride into 10 ml of ultrapure water, ultrasonically dissolving, adding into the mesoporous silica solution, and stirring on a magnetic stirrer rotating at 300 revolutions; adding 30 mg of potassium permanganate into 3 ml of ultrapure water, ultrasonically dissolving, then sucking the potassium permanganate solution by using a 200 microliter liquid-transferring gun, dropwise adding the potassium permanganate solution into the mixed solution, stirring for 2 minutes, then adding 150 microliter of 28wt% ammonia water into the mixed solution, placing the mixed solution in a magnetic stirrer, and stirring for 12 hours under the condition of 300 revolutions. And after the reaction is finished, centrifuging the sample solution for 10 minutes under the condition of 10000 revolutions, washing the sample solution for 3 times by using ultrapure water, centrifuging the sample solution for 10 minutes at the centrifugal rotating speed of 10000 revolutions per minute, and then drying the washed sample in a drying box at the temperature of 60 ℃ to obtain the mesoporous silica/manganese dioxide nanoflower material.
Example 2:
1) Preparing a mesoporous silica template: adding 0.36 g triethanolamine into 72 ml deionized water and 48 ml hexadecyl trimethyl ammonium chloride solution with solute mass of 25%, rotating speed of 250 r/min, preheating for 1 hour under 60 ℃ oil bath condition; and (3) uniformly mixing 36 ml of cyclohexane and 4 ml of tetraethyl silicate, after the solution is preheated, enabling the solution to swirl along the mouth of the round-bottom flask by using a disposable plastic dropper to enter the flask, and then continuously stirring the solution at the constant temperature for 17 hours under the conditions of 250 revolutions per minute and 60 ℃ oil bath. After the reaction is finished, the solution has obvious layering phenomenon, the upper oil phase solution which is well reacted is taken out and discarded, and the lower water phase solution and ethanol are mixed according to the volume ratio of 1:3, and centrifuging at 9000 rpm for 3 minutes. And then washing the centrifuged precipitate for 3 times by using ethanol, wherein the centrifugation conditions of 3 times of washing are 10000 r/min and 5 min, then drying in a drying oven at 60 ℃, grinding the dried sample, and calcining for 2 h at 540 ℃ to obtain the mesoporous silicon dioxide.
2) Preparing a mesoporous silica/manganese dioxide nanoflower material: weighing 100 mg of mesoporous silica, ultrasonically dispersing in 40 ml of ultrapure water, and ultrasonically treating for 5 minutes; adding 140 mg of tetrahydrate manganese acetate and 300 mg of ammonium chloride into 20 ml of ultrapure water, ultrasonically dissolving, adding into the mesoporous silica solution, and stirring on a 300-turn magnetic stirrer; adding 60 mg of potassium permanganate into 6 ml of ultrapure water, ultrasonically dissolving, then sucking the potassium permanganate solution by using a 200 microliter liquid-transferring gun, dropwise adding the potassium permanganate solution into the mixed solution, stirring for 2 minutes, then adding 300 microliter of 28wt% ammonia water into the mixed solution, placing the mixed solution in a magnetic stirrer, and stirring for 12 hours under the condition of 300 revolutions. And after the reaction is finished, centrifuging the sample solution for 10 minutes under the condition of 10000 revolutions, washing the sample solution for 3 times by using ultrapure water, centrifuging the sample solution for 10 minutes at the centrifugal rotating speed of 10000 revolutions per minute, and then drying the washed sample in a drying box at the temperature of 60 ℃ to obtain the mesoporous silica/manganese dioxide nanoflower material.
Example 3:
1) Preparing a mesoporous silica template: adding 0.36 g triethanolamine into 72 ml deionized water and 48 ml hexadecyl trimethyl ammonium chloride solution with solute mass of 25%, rotating speed of 250 r/min, preheating for 1 hour under 60 ℃ oil bath condition; and (3) uniformly mixing 36 ml of cyclohexane and 4 ml of tetraethyl silicate, after the solution is preheated, enabling the solution to swirl along the mouth of the round-bottom flask by using a disposable plastic dropper to enter the flask, and then continuously stirring the solution at the constant temperature for 17 hours under the conditions of 250 revolutions per minute and 60 ℃ oil bath. After the reaction is finished, the solution has obvious layering phenomenon, the upper oil phase solution is taken out and discarded, and the lower water phase solution and ethanol are mixed according to the volume ratio of 1:3, and centrifuging at 9000 rpm for 3 minutes. And then washing the centrifuged precipitate for 3 times by using ethanol, wherein the centrifugation conditions of 3 times of washing are 10000 r/min and 5 min, then drying in a drying oven at 60 ℃, grinding the dried sample, and calcining for 2 h at 540 ℃ to obtain the mesoporous silicon dioxide.
2) Preparing a mesoporous silica/manganese dioxide nanoflower material: weighing 50 mg of mesoporous silica, ultrasonically dispersing in 20 ml of ultrapure water, and ultrasonically treating for 5 minutes; adding 70 mg of tetrahydrate manganese acetate and 100 mg of ammonium chloride into 10 ml of ultrapure water, ultrasonically dissolving, adding into the mesoporous silica solution, and stirring on a 300-turn magnetic stirrer; adding 30 mg of potassium permanganate into 3 ml of ultrapure water, ultrasonically dissolving, then sucking the potassium permanganate solution by using a 200 microliter liquid-transferring gun, dropwise adding the potassium permanganate solution into the mixed solution, stirring for 2 minutes, adding 28wt% of 150 microliter ammonia water into the mixed solution, placing the mixed solution in a magnetic stirrer, and stirring for 12 hours under the condition of 300 revolutions. And after the reaction is finished, centrifuging the sample solution for 10 minutes under the condition of 10000 revolutions, washing the sample solution for 3 times by using ultrapure water, centrifuging the sample solution for 10 minutes at the centrifugal rotation speed of 10000 revolutions per minute, and then drying the washed sample in a drying oven at the temperature of 60 ℃ to obtain the mesoporous silica/manganese dioxide nanoflower material.
Example 4:
1) Preparing a mesoporous silica template: adding 0.36 g triethanolamine into 72 ml deionized water and 48 ml hexadecyl trimethyl ammonium chloride solution with solute mass of 25%, rotating speed of 250 r/min, preheating for 1 hour under 60 ℃ oil bath condition; and (3) uniformly mixing 36 ml of cyclohexane and 4 ml of tetraethyl silicate, slowly swirling the solution along the mouth of the round-bottom flask by using a disposable plastic dropper after the solution is preheated, feeding the solution into the flask, and continuously stirring the solution at the constant temperature for 17 hours under the conditions of 250 revolutions per minute and 60 ℃ oil bath. After the reaction is finished, the solution has obvious layering phenomenon, the upper oil phase solution is taken out and discarded, and the lower water phase solution and ethanol are mixed according to the volume ratio of 1:3, and centrifuging at 9000 rpm for 3 minutes. And then washing the centrifuged precipitate for 3 times by using ethanol, wherein the centrifugation conditions of 3 times of washing are 10000 r/min and 5 min, then drying in a drying oven at 60 ℃, grinding the dried sample, and calcining for 2 h at 540 ℃ to obtain the mesoporous silicon dioxide.
2) Preparing a mesoporous silica/manganese dioxide nanoflower material: weighing 50 mg of mesoporous silica, ultrasonically dispersing in 20 ml of ultrapure water, and ultrasonically treating for 5 minutes; adding 70 mg of tetrahydrate manganese acetate and 100 mg of ammonium chloride into 10 ml of ultrapure water, ultrasonically dissolving, adding into the mesoporous silica solution, and stirring on a 300-turn magnetic stirrer; adding 30 mg of potassium permanganate into 3 ml of ultrapure water, ultrasonically dissolving, then sucking the potassium permanganate solution by using a 200 microliter liquid-transferring gun, dropwise adding the potassium permanganate solution into the mixed solution, stirring for 2 minutes, then adding 100 microliter of 28wt% ammonia water into the mixed solution, placing the mixed solution in a magnetic stirrer, and stirring for 12 hours under the condition of 300 revolutions. And after the reaction is finished, centrifuging the sample solution for 10 minutes under the condition of 10000 revolutions, washing the sample solution for 3 times by using ultrapure water, centrifuging the sample solution for 10 minutes at the centrifugal rotating speed of 10000 revolutions per minute, and then drying the washed sample in a drying box at the temperature of 60 ℃ to obtain the mesoporous silica/manganese dioxide nanoflower material.
Claims (9)
1. A preparation method of a mesoporous silica/manganese dioxide nanoflower material is characterized by comprising the following steps:
(1) Preparing a mesoporous silica template: dissolving 0.36 g of triethanolamine in 72 ml of deionized water and 48 ml of hexadecyltrimethylammonium chloride solution, stirring and reacting for 1 hour at constant temperature in an oil bath pot, adding the uniformly mixed 36 ml of cyclohexane and 4 ml of tetraethyl silicate into the solution by using a disposable plastic dropper, reacting for 17 hours in an oil bath, centrifuging, washing, drying, and removing a template to obtain a mesoporous silica template;
(2) Preparing a mesoporous silica/manganese dioxide nanoflower material: dispersing the mesoporous silica in 20 ml of ultrapure water under the condition of normal temperature, performing ultrasonic treatment, and adding tetrahydrate manganese acetate and ammonium chloride, wherein the mass ratio of the mesoporous silica to the tetrahydrate manganese acetate is 5:7, the mass ratio of the mesoporous silica to the ammonium chloride is 1:3; and then, dropwise adding a potassium permanganate solution with the concentration of 10 mg/ml, adding ammonia water when the solution turns brown, wherein the ammonia water is added to react with ammonium salt to form an alkaline environment, so that the pH value of the solution is greater than 7, reacting and stirring for 12 hours, centrifuging, washing and drying to obtain the mesoporous silica/manganese dioxide nanoflower material.
2. The method according to claim 1, wherein in the step (1), the constant temperature stirring temperature is 60 ℃ and the rotation speed is 250 rpm.
3. The preparation method according to claim 1, wherein in the step (1), the solution is delaminated after the reaction is completed, the upper oil phase solution is discarded, the lower aqueous phase solution is taken out, and the ratio of the aqueous phase solution: ethanol is 1:3, the rotating speed of the centrifugation is 9000 r/min, and the time is 3 min; the washing method is to wash by using ethanol, the centrifugation times are 3 times, the centrifugation speed is 10000 r/min, and the time is 5 min.
4. The method according to claim 1, wherein in the step (1), the concentration of the solute in the cetyltrimethylammonium chloride solution is 25% by mass.
5. The production method according to claim 1, wherein in the step (1), the temperature drying condition for drying is 60 degrees centigrade.
6. The method according to claim 1, wherein in the step (1), the temperature of the depanning plate is 540 ℃.
7. The process according to claim 1, wherein in the step (2), the amount of aqueous ammonia used is 28% by weight.
8. The method according to claim 1, wherein in step (2), the centrifugation speed is 10000 rpm for 10 minutes.
9. The method according to claim 1, wherein in the step (2), the drying temperature is 60 ℃.
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