CN111359595A - Preparation method of polypyrrole core-shell mesoporous silica microsphere adsorption material - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses a preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material, which takes a monodisperse silica microsphere as a template and a surfactant as a pore-making agent to prepare a core-shell mesoporous silica microsphere as an inorganic carrier of the adsorbent; pyrrole monomers are polymerized inside and outside and on the surface of a mesoporous pore passage through in-situ polymerization to prepare the polypyrrole core-shell mesoporous silica microsphere adsorbing material with large specific surface area, high adsorption capacity and high adsorption rate, and the material is mainly applied to the efficient removal of Cr (VI) in wastewater. In the test process, the removal rate of Cr (VI) adsorption is as high as 99.19%, and the method has good application prospect in industrial wastewater treatment.
Description
Technical Field
The invention relates to the field of heavy metal adsorption, in particular to a preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material.
Background
Chromium (Cr) is one of the most abundant elements in nature, and it exists in an aqueous environment mainly in two states: chromium (III) and chromium (VI). In general, chromium (VI) is more toxic than chromium (III), and cr (VI) accumulates in the food chain and causes serious health problems, causing skin irritation and even induction of genotoxicity and carcinogenesis.
In recent years, various methods for removing cr (vi) in wastewater have been extensively studied. The current major methods include chemical precipitation, ion exchange, adsorption, membrane separation, coagulation, and electrochemical methods. Among these methods, the adsorption method has advantages of simplicity, wide use, low cost, and the like, and thus is widely used.
The traditional adsorbent comprises active carbon, clay, zeolite, agricultural and forestry wastes (bagasse, orange peel, shaddock peel and the like), and when the concentration of Cr (VI) is relatively low, the traditional adsorbent has an unsatisfactory adsorption effect and cannot meet the requirements of people.
Disclosure of Invention
The invention aims to provide a preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material, and aims to solve the problem that the existing adsorbent is poor in adsorption effect when the concentration of Cr (VI) is low.
In order to achieve the purpose, the invention provides a preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material, which comprises the following steps: weighing absolute ethyl alcohol, deionized water, concentrated ammonia water and a silicon source according to the volume ratio of 5-10: 1-5: 0.1-0.5: 1, mixing the absolute ethyl alcohol, the deionized water and the concentrated ammonia water, stirring for 0.1-1.0 h at 20-50 ℃ to obtain a first mixed solution, adding the silicon source into the first mixed solution, and continuously stirring for 1.0-10.0 h to obtain monodisperse silicon dioxide microspheres;
weighing the silicon source and the surfactant according to a mass ratio of 5-10: 1, stirring the weighed surfactant and the monodisperse silica microspheres for 0.5-1.0 h to obtain a second mixed solution, adding the silicon source into the second mixed solution, continuously stirring for 20.0-24.0 h, washing and filtering the second mixed solution by using the deionized water and the absolute ethyl alcohol to obtain a white powder sample, placing the white powder sample at 70-100 ℃ for vacuum drying for 5.0-8.0 h, placing the white powder sample in a muffle furnace for roasting at 550 ℃ for 300min to obtain core-shell mesoporous silica microspheres;
weighing the core-shell mesoporous silica microspheres, a pyrrole monomer, deionized water and an initiator according to a mass ratio of 0.1-0.5: 0.1-1.0: 20-40: 1, dispersing the core-shell mesoporous silica microspheres and the pyrrole monomer in the deionized water, carrying out ultrasonic treatment for 0.5-1.0 h, stirring for 0.5-2.0 h at 20-50 ℃ to obtain a third mixed solution, adding the initiator into the third mixed solution, continuously stirring for 6-12 h, washing and filtering by using the deionized water and the absolute ethyl alcohol to obtain a black powder sample, and carrying out vacuum drying on the black powder sample at 50-100 ℃ for 8-12 h to obtain the polypyrrole core-shell mesoporous silica microsphere adsorbing material.
Wherein the silicon source is one or two of tetraethyl orthosilicate and sodium silicate.
Wherein the surfactant is one or more of cetyltrimethyl ammonium chloride, cetyltrimethyl ammonium bromide and octadecyl trimethoxy silane.
Wherein the initiator is one or more of ammonium persulfate, potassium persulfate, azodiisobutyronitrile and ferric sulfide hexahydrate.
Wherein the polypyrrole core-shell mesoporous silica microsphere adsorbing material has a mesoporous aperture of 2-15 nm and a pore volume of 0.5-1.2 cm3A specific surface area of 300 to 900 m/g2/g。
According to the preparation method of the polypyrrole core-shell mesoporous silica microsphere adsorption material, the prepared polypyrrole core-shell mesoporous silica microsphere adsorption material has high specific surface area, high adsorption capacity and high adsorption rate, and is mainly applied to efficient removal of Cr (VI) in wastewater. Test results show that the removal rate of the polypyrrole core-shell mesoporous silica microspheres to Cr (VI) is as high as 99.19%, so that the problem that the existing adsorbent is poor in adsorption effect when the concentration of Cr (VI) is low is solved. The polypyrrole core-shell mesoporous silica microsphere adsorption material is simple to synthesize, easy to realize industrial production, excellent in adsorption performance and capable of being widely applied to the field of water purification.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flowchart of a preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material according to an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of monodisperse silica microspheres prepared in an example of the present invention;
FIG. 3 is a scanning electron micrograph of core-shell mesoporous silica microspheres prepared in an example of the present invention;
FIG. 4 is a scanning electron microscope photograph of the polypyrrole core-shell mesoporous silica microsphere adsorbing material prepared in the example of the present invention;
FIG. 5 is a graph showing the change of the Cr (VI) adsorption rate with adsorption time in the embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example the procedure is as shown in figure 1,
s101, mixing 162.8mL of absolute ethyl alcohol, 30.0mL of deionized water and 3.14mL of concentrated ammonia water, stirring at 30 ℃ for 30min to obtain a first mixed solution, adding 15.0mL of tetraethyl orthosilicate into the first mixed solution, and continuously stirring for 2.0h to obtain the monodisperse silica microspheres.
The deionized water is used for hydrolyzing the tetraethyl orthosilicate to form silicon dioxide, the anhydrous ethanol is used for controlling the size of the formed silicon dioxide microspheres, and the strong ammonia water mainly provides an alkaline environment to control the hydrolysis rate of the tetraethyl orthosilicate, so that the monodisperse silicon dioxide microspheres are obtained. The monodisperse silica microspheres shown in fig. 2 were prepared, and it can be seen that the prepared silica microspheres have good monodispersity and sphericity.
S102, adding 0.5g of hexadecyl trimethyl ammonium bromide into the monodisperse silicon dioxide microspheres prepared in the S101, stirring for 30min to obtain a second mixed solution, then adding 5.0g of tetraethyl orthosilicate into the second mixed solution, continuously stirring for 20.0h, washing for 3 times by using deionized water and absolute ethyl alcohol respectively after stirring is finished, filtering, separating, and drying in vacuum at 80 ℃ for 5.0 h. And finally, placing the powder sample in a muffle furnace at 550 ℃ for roasting for 300min to obtain the core-shell mesoporous silica microspheres shown in the figure 3. The preparation of the core-shell mesoporous silica microspheres shown in fig. 3 shows that the particle size of the core-shell mesoporous silica microspheres is increased.
The method comprises the steps of using the hexadecyl trimethyl ammonium bromide as a pore-forming agent, providing the tetraethyl orthosilicate as a pore-forming material, using the deionized water and the absolute ethyl alcohol to clean the concentrated ammonia water, the hexadecyl trimethyl ammonium bromide and the tetraethyl orthosilicate, and then preparing a core-shell mesoporous silica microsphere serving as an inorganic carrier of an adsorbent through filtering, separating, drying and roasting.
S103, preparing the core-shell mesoporous silica microspheres prepared from 1.0g S102, and performing ultrafiltrationThe mixture was dispersed by sonication in 100mL of deionized water, 0.5g of pyrrole monomer was added, and the mixture was stirred at 30 ℃ for 30min to obtain a third mixed solution. Then, 3.54g of ammonium persulfate was dissolved in 10mL of deionized water, added to the third mixed solution, and stirred for 12 hours. Finally, washing the powder sample for 3 times respectively by using deionized water and absolute ethyl alcohol, filtering the powder sample, and drying the powder sample for 12 hours in vacuum at the temperature of 60 ℃ to obtain the polypyrrole core-shell mesoporous silica microsphere adsorbing material, wherein the mesoporous aperture of the polypyrrole core-shell mesoporous silica microsphere adsorbing material is 2-15 nm, and the pore volume is 0.5-1.2 cm3A specific surface area of 300 to 900 m/g2(ii) in terms of/g. The core-shell mesoporous silica microsphere adsorption material shown in fig. 4 is obtained, and it can be seen that polypyrrole has been successfully loaded on the surface of the core-shell mesoporous silica microsphere.
By utilizing the advantages of the larger specific surface area and the mesoporous pore canal of the core-shell mesoporous silica microsphere, pyrrole monomers enter the inner surface and the outer surface of the core-shell mesoporous silica microsphere, the inner surface and the outer surface of the mesoporous pore canal are subjected to polymerization reaction through ammonium persulfate, and the polypyrrole core-shell mesoporous silica microsphere adsorption material is obtained after cleaning, filtering and drying.
The concentration of Cr (VI) is 25mg/L, the polypyrrole core-shell mesoporous silica microspheres prepared in this example are used as an adsorbent, and the adsorption kinetics of Cr (VI) are studied. The testing method is that 30mg of polypyrrole core-shell mesoporous silica microsphere adsorbing material is added into 200mL of Cr (VI) solution under the condition of pH 2 by adopting a typical kinetic experiment, and the rotating speed is adjusted to 400 rpm. The samples were taken at predetermined times and after filtration the samples were tested for the concentration of residual cr (vi) in the solution using a uv spectrophotometer according to GB 7467-87. The test results are shown in FIG. 5, and it can be seen that the adsorption capacity (q) for Cr (VI) increases with timee) And gradually increases. The result shows that the removal rate of the polypyrrole core-shell mesoporous silica microsphere adsorbing material to Cr (VI) is as high as 99.19%.
The concentration of Cr (VI) is 50.0mg/L, the polypyrrole core-shell mesoporous silica microspheres prepared by the embodiment are used as an adsorbent, and the adsorption effect of Cr (VI) is studied. The test method comprises the steps of adding 10.0mg of polypyrrole core-shell mesoporous silica microsphere adsorbing material into 10.0mL of Cr (VI) solution under the condition that the pH value is 2, adjusting the rotating speed to 400rpm, stopping stirring after 20.0h of adsorption, and standing for 1.0h to obtain an adsorption effect graph of the polypyrrole core-shell mesoporous silica microsphere on Cr (VI). It can be seen that compared with the unadsorbed cr (vi) solution, after the polypyrrole core-shell mesoporous silica microsphere adsorbing material is used for adsorption, the color of the cr (vi) solution becomes colorless, which indicates that the polypyrrole core-shell mesoporous silica microsphere adsorbing material has excellent adsorption performance on cr (vi).
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of a polypyrrole core-shell mesoporous silica microsphere adsorption material is characterized in that,
the method comprises the following steps: weighing absolute ethyl alcohol, deionized water, concentrated ammonia water and a silicon source according to the volume ratio of 5-10: 1-5: 0.1-0.5: 1, mixing the absolute ethyl alcohol, the deionized water and the concentrated ammonia water, stirring for 0.1-1.0 h at 20-50 ℃ to obtain a first mixed solution, adding the silicon source into the first mixed solution, and continuously stirring for 1.0-10.0 h to obtain monodisperse silicon dioxide microspheres;
weighing the silicon source and the surfactant according to a mass ratio of 5-10: 1, stirring the weighed surfactant and the monodisperse silica microspheres for 0.5-1.0 h to obtain a second mixed solution, adding the silicon source into the second mixed solution, continuously stirring for 20.0-24.0 h, washing and filtering the second mixed solution by using the deionized water and the absolute ethyl alcohol to obtain a white powder sample, placing the white powder sample at 70-100 ℃ for vacuum drying for 5.0-8.0 h, placing the white powder sample in a muffle furnace for roasting at 550 ℃ for 300min to obtain core-shell mesoporous silica microspheres;
weighing the core-shell mesoporous silica microspheres, a pyrrole monomer, deionized water and an initiator according to a mass ratio of 0.1-0.5: 0.1-1.0: 20-40: 1, dispersing the core-shell mesoporous silica microspheres and the pyrrole monomer in the deionized water, carrying out ultrasonic treatment for 0.5-1.0 h, stirring for 0.5-2.0 h at 20-50 ℃ to obtain a third mixed solution, adding the initiator into the third mixed solution, continuously stirring for 6-12 h, washing and filtering by using the deionized water and the absolute ethyl alcohol to obtain a black powder sample, and carrying out vacuum drying on the black powder sample at 50-100 ℃ for 8-12 h to obtain the polypyrrole core-shell mesoporous silica microsphere adsorbing material.
2. The preparation method of the polypyrrole core-shell mesoporous silica microsphere adsorbing material according to claim 1, wherein,
the silicon source is one or two of tetraethyl orthosilicate and sodium silicate.
3. The preparation method of the polypyrrole core-shell mesoporous silica microsphere adsorbing material according to claim 1, wherein,
the surfactant is one or more of cetyltrimethyl ammonium chloride, cetyltrimethyl ammonium bromide and octadecyl trimethoxy silane.
4. The preparation method of the polypyrrole core-shell mesoporous silica microsphere adsorbing material according to claim 1, wherein,
the initiator is one or more of ammonium persulfate, potassium persulfate, azodiisobutyronitrile and ferric sulfide hexahydrate.
5. The preparation method of the polypyrrole core-shell mesoporous silica microsphere adsorbing material according to claim 1, wherein,
the polypyrrole core-shell mesoporous silica microsphere adsorbing material has a mesoporous aperture of 2-15 nm and a pore volume of 0.5-1.2 cm3Specific surface area/gThe product is 300-900 m2/g。
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Cited By (2)
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| CN114392771A (en) * | 2022-02-08 | 2022-04-26 | 西北大学 | Composite nano photocatalytic material and preparation method and application thereof |
| CN114920250A (en) * | 2022-04-12 | 2022-08-19 | 苏州星谱生物科技有限公司 | Preparation method of echinoid magnetic beads and application of echinoid magnetic beads in nucleic acid extraction |
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| CN114920250A (en) * | 2022-04-12 | 2022-08-19 | 苏州星谱生物科技有限公司 | Preparation method of echinoid magnetic beads and application of echinoid magnetic beads in nucleic acid extraction |
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