CN112979869A - Hexagonal boron nitride nanosheet hydrogel composite material, and preparation method and application thereof - Google Patents
Hexagonal boron nitride nanosheet hydrogel composite material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a hexagonal boron nitride nanosheet hydrogel composite material, a preparation method and application thereof, wherein the preparation method comprises the following steps: adding hexagonal boron nitride powder into a eutectic solvent formed by mixing a hydrogen bond donor and a hydrogen bond acceptor, and then carrying out ultrasonic treatment, centrifugation and drying to obtain a hexagonal boron nitride nanosheet; and mixing acrylamide and halogenated quaternary ammonium salt or halogenated ammonium salt, stirring under a heating condition until transparent liquid is formed, cooling to room temperature, adding a cross-linking agent, an initiator and the prepared hexagonal boron nitride nanosheet to form a mixed solution, pouring the mixed solution into a glass test tube, heating, soaking the polymer in water after the reaction is finished, removing the polymer, and freeze-drying to obtain the hexagonal boron nitride nanosheet hydrogel composite material. The preparation method is simple in preparation process and quick in reaction, and the prepared hexagonal boron nitride nanosheet hydrogel has good adsorption property on methylene blue and can be well recycled.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a hexagonal boron nitride nanosheet hydrogel composite material, and a preparation method and application thereof.
Background
Along with the development of human industry, the problem of water pollution treatment is widely concerned all over the world, especially dyes are widely used in human life and production, economic development is promoted, and simultaneously water environment pollution is caused.
The hexagonal boron nitride is a white inorganic non-metallic material, has the same lattice structure with graphene, and is sp2The hybrid material is also called as "white graphene", and the hexagonal boron nitride has properties similar to those of graphene, such as strong mechanical strength, good adsorption performance, excellent thermal stability and the like, but also has properties which are not possessed by graphene, such as oxidation resistance, electrical insulation performance, excellent lubricity, a wide energy gap band and the like.According to researches, when hexagonal boron nitride is stripped into nanoscale hexagonal boron nitride nanosheets, the thermal conductivity, the optical property, the mechanical property and the adsorption property of the hexagonal boron nitride nanosheets are obviously enhanced, but the powdery hexagonal boron nitride nanosheets are not easy to recycle when used for sewage treatment, so that the development of the hexagonal boron nitride nanosheets is limited, and how to solve the problem of recycling of the hexagonal boron nitride nanosheets is a target to be solved.
Disclosure of Invention
The invention aims to provide a hexagonal boron nitride nanosheet hydrogel composite material, a preparation method and application thereof, and the hexagonal boron nitride nanosheet hydrogel composite material prepared by the preparation method has the characteristics of high speed, low energy consumption, high reaction speed and the like; the obtained hexagonal boron nitride nanosheet hydrogel has good adsorption performance on dyes in dye wastewater, especially methylene blue dye wastewater, and can be recycled.
The invention provides the following technical scheme: a preparation method of a hexagonal boron nitride nanosheet hydrogel composite material comprises the following steps:
1) preparation of the first eutectic solvent: heating a hydrogen bond donor and a hydrogen bond acceptor with a molar ratio of 1: 1-5 to 80 ℃, and melting for 10-15min to obtain a first eutectic agent combined in a hydrogen bond form;
2) adding 0.2g of hexagonal boron nitride powder with the purity of 99.9% into the first eutectic agent prepared in the step 1), performing ultrasonic treatment and centrifugation, standing overnight, taking two thirds of supernatant, performing suction filtration, and drying in a forced air drying oven at 70 ℃ for 12 hours to obtain a hexagonal boron nitride nanosheet with the particle size of 1-1.5 microns and the thickness of 1.2 nm;
3) preparation of a second eutectic solvent: heating acrylamide and halogenated quaternary ammonium salt or halogenated ammonium salt in a molar ratio of 1: 1-5 to 80 ℃, and melting for 10-15min to obtain a second eutectic agent combined in a hydrogen bond form;
4) adding the hexagonal boron nitride nanosheet obtained in the step 2), a cross-linking agent and an initiator into the second low co-solvent prepared in the step 3) to form a mixed solution, pouring the mixed solution into a test tube, heating by using an electric iron, and withdrawing the electric iron after the reaction is started until the reaction is finished to obtain a polymer; the mass of the hexagonal boron nitride nanosheet accounts for 1-9% of the mass of the second low eutectic agent, the mass of the cross-linking agent accounts for 1-3% of the mass of the second low eutectic agent, and the mass of the initiator accounts for 0.1-2% of the total mass of the second low eutectic agent;
5) cooling the polymer obtained in the step 4) to room temperature, then soaking and washing the polymer with deionized water, and after the soaking and washing are finished, carrying out freeze drying at the temperature of-50 ℃ to obtain the hexagonal boron nitride nanosheet hydrogel composite material.
Further, the ultrasonic time in the step 2) is 6-15 h.
Further, the rotating speed of a centrifugal machine adopted in the centrifugation in the step 2) is 6000 +/-100 rpm; the centrifugation time is 30-60 min.
Further, the membrane adopted in the suction filtration in the step 2) is a nylon membrane, and after the suction filtration is finished, the suction filtration is carried out again by using distilled water, and the process is repeated for three times.
Further, the cross-linking agent in the step 4) is N, N' -methylene bisacrylamide, and the initiator is any one of ammonium persulfate and potassium persulfate.
Further, the halogenated quaternary ammonium salt is choline chloride.
Further, the haloammonium salt is methyltributylammonium bromide.
Further, the freeze drying time in the step 5) is 12-24 hours.
The invention also provides the hexagonal boron nitride nanosheet hydrogel composite material prepared by the preparation method.
The invention also provides application of the hexagonal boron nitride nanosheet hydrogel composite material in dye wastewater, wherein the dye is methylene blue.
The invention has the beneficial effects that:
1. the preparation method of the hexagonal boron nitride nanosheet hydrogel composite material provided by the invention takes the first eutectic solvent as a solvent, and obtains the hexagonal boron nitride nanosheet through ultrasonic dispersion, wherein the eutectic solvent is cheap and easy to obtain, is non-toxic and biodegradable, and reduces the pollution to the environment.
2. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material provided by the invention adopts the second eutectic agent as a solvent to prepare the hexagonal boron nitride nanosheet hydrogel through a front-end polymerization method, the reaction time is short, the energy consumption is low, and the recovery utilization rate of the hexagonal boron nitride nanosheets is improved.
3. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material provided by the invention has the advantages that the hexagonal boron nitride nanosheet prepared by adopting the first eutectic agent is compounded with the second eutectic agent prepared by adopting a front-end polymerization method, so that the adsorption performance of the hydrogel can be improved, and the recovery utilization rate of the hexagonal boron nitride nanosheet can be improved;
front-end polymerization is a free radical reaction mode that converts polymer monomers into polymers by self-exothermicity by initiating local monomer polymerization at room temperature. Compared with the traditional polymerization method, the polymerization reaction has the advantages of simple operation, fast reaction and the like. The hydrogel prepared by the front-end polymerization method has a large hollow structure, and the defect of poor adsorption performance of the hydrogel is overcome by the hexagonal boron nitride nanosheets.
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The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is a scanning electron microscope SEM image of a hexagonal boron nitride nanosheet prepared in example 1 of the present invention;
FIG. 2 is an infrared spectrum of a hexagonal boron nitride nanosheet prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope SEM image of a hexagonal boron nitride nanosheet hydrogel composite prepared in example 1 of the present invention;
fig. 4 is a graph of the adsorption removal efficiency of different adding amounts of the hexagonal boron nitride nanosheet hydrogel composite material prepared in example 1 of the present invention on methylene blue dye in methylene blue dye sewage.
Detailed description of the preferred embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
8g of choline chloride is taken as a hydrogen bond acceptor, triethanolamine is taken as a hydrogen bond donor, and the ratio of 1: 2 mol ratio, and continuously stirring in a constant temperature heating oil bath kettle at 80 ℃ until a transparent liquid is formed, namely the first eutectic solvent. Adding 0.2g of hexagonal boron nitride into the prepared first eutectic solvent, stirring in a magnetic stirrer for 1h to uniformly disperse the hexagonal boron nitride in the first eutectic solvent to obtain a white dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 20h, standing overnight, centrifuging two thirds of supernatant liquid, centrifuging at 4000rpm/min for 30min to remove un-peeled hexagonal boron nitride, and centrifuging to obtain the supernatant liquid. And carrying out suction filtration on the obtained supernatant through a nylon membrane, carrying out suction filtration again by using deionized water after the suction filtration is finished, putting the product after the suction filtration into a vacuum drying oven at 70 ℃, and drying for 12 hours to obtain the product after drying, namely the hexagonal boron nitride nanosheet (the particle size is about 1-1.5 mu m, and the thickness is about 1.2 nm).
Preparing the hexagonal boron nitride nanosheet hydrogel: 4g of choline chloride as a hydrogen bond acceptor and acrylamide as a hydrogen bond donor, and the ratio of 1: 2 mol ratio, and continuously stirring in a constant temperature heating oil bath kettle at 80 ℃ until a transparent liquid is formed, namely the second eutectic solvent. Mixing 8g of second eutectic solvent, 0.234g of cross-linking agent N, N-methylene bisacrylamide, 0.167g of initiator potassium persulfate and 0.4g of hexagonal boron nitride nanosheet (the particle size is about 1-1.5 mu m, the thickness is about 1.2nm) according to a certain proportion, pouring into a test tube of 100 x 13mm, fixing by using a test tube clamp, placing a heated electric soldering iron at a position of 20mm of the liquid level, and withdrawing the soldering iron after the front end of the polymer is formed. After the reaction is finished, cooling the test tube to room temperature, soaking the generated hydrogel in deionized water for 6 days (changing water every other day) for washing out unreacted monomers and choline chloride, and then freeze-drying the hydrogel for 12 hours to obtain the hexagonal boron nitride nanosheet hydrogel composite material.
Adsorption experiment: putting 100mL of methylene blue solution with the concentration of 10mg/L into a 250mL conical flask, adjusting the pH to 8 by using 0.1mol/L hydrochloric acid and sodium hydroxide solution, putting the conical flask into a shaking table, shaking at the temperature of 30 ℃ at the speed of 160r/min, and respectively adding 0.01, 0.02, 0.05, 0.08, 0.1 and 0.15g of composite material, wherein the shaking time is 3 h. And taking the supernatant, and measuring the concentration of the residual solution by using an ultraviolet spectrophotometer at the maximum absorption wavelength of methylene blue of 664 nm.
Example 2
6g of choline chloride as a hydrogen bond acceptor and ethylene glycol as a hydrogen bond donor, the ratio of 1: 2 mol ratio, and continuously stirring in a constant temperature heating oil bath kettle at 80 ℃ until a transparent liquid is formed, namely the first eutectic solvent. Adding 0.3g of hexagonal boron nitride into the prepared first eutectic solvent, stirring in a magnetic stirrer for 2 hours to uniformly disperse the hexagonal boron nitride in the first eutectic solvent to obtain a white dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 10 hours, standing overnight, centrifuging two thirds of supernatant, centrifuging at 6000rpm/min for 30min to remove un-peeled hexagonal boron nitride, and centrifuging to obtain the supernatant liquid. And carrying out suction filtration on the obtained supernatant through a nylon membrane, carrying out suction filtration again by using deionized water after the suction filtration is finished, putting the product after the suction filtration into a vacuum drying oven at 70 ℃, and drying for 20 hours to obtain the product after the drying, namely the hexagonal boron nitride nanosheet (the particle size is about 1-1.5 mu m, and the thickness is about 1.2 nm).
Preparing the hexagonal boron nitride nanosheet hydrogel: 10g of decaalkylamine serving as a hydrogen bond acceptor and acrylamide serving as a hydrogen bond donor are mixed according to a molar ratio of 1:1, and the mixture is continuously stirred in a constant-temperature heating oil bath kettle at the temperature of 80 ℃ until transparent liquid is formed, namely the second eutectic solvent. Mixing 8g of second eutectic solvent, 0.357g of cross-linking agent N, N-methylene bisacrylamide, 0.213g of initiator ammonium persulfate and 0.6g of hexagonal boron nitride nanosheet (the particle size is about 1-1.5 mu m, the thickness is about 1.2nm) according to a certain proportion, pouring into a test tube of 100 x 13mm, fixing by using a test tube clamp, placing a heated electric soldering iron at a position of 20mm of the liquid level, and withdrawing the electric soldering iron after the front end of the polymer is formed. After the reaction is finished, cooling the test tube to room temperature, soaking the generated hydrogel in deionized water for 6 days (changing water every other day) for washing out unreacted monomers, and then freeze-drying the hydrogel for 24 hours to obtain the hexagonal boron nitride nanosheet hydrogel composite material.
Adsorption and desorption experiments of the hexagonal boron nitride nanosheet hydrogel: performing an adsorption and analysis experiment under the conditions that the initial concentration of MB is 10mg/L, the adsorption time is 3h, and the addition amount of the hexagonal boron nitride nanosheet hydrogel is 0.1g at 25 ℃, performing four-cycle adsorption and analysis experiments on the MB solution by the hexagonal boron nitride nanosheet hydrogel, gradually reducing the removal rate along with the increase of the cycle number, and obtaining that the removal rate of the hexagonal boron nitride nanosheet hydrogel still reaches 71.62% after the four-cycle adsorption and analysis experiments, so that the hexagonal boron nitride nanosheet hydrogel has a certain recycling capacity.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (10)
1. A preparation method of a hexagonal boron nitride nanosheet hydrogel composite material is characterized by comprising the following steps:
1) preparation of the first eutectic solvent: heating a hydrogen bond donor and a hydrogen bond acceptor with a molar ratio of 1: 1-5 to 80 ℃, and melting for 10-15min to obtain a first eutectic agent combined in a hydrogen bond form;
2) adding 0.2g of hexagonal boron nitride powder with the purity of 99.9% into the first eutectic agent prepared in the step 1), performing ultrasonic treatment and centrifugation, standing overnight, taking two thirds of supernatant, performing suction filtration, and drying in a forced air drying oven at 70 ℃ for 12 hours to obtain a hexagonal boron nitride nanosheet with the particle size of 1-1.5 microns and the thickness of 1.2 nm;
3) preparation of a second eutectic solvent: heating acrylamide and halogenated quaternary ammonium salt or halogenated ammonium salt in a molar ratio of 1: 1-5 to 80 ℃, and melting for 10-15min to obtain a second eutectic agent combined in a hydrogen bond form;
4) adding the hexagonal boron nitride nanosheet obtained in the step 2), a cross-linking agent and an initiator into the second low co-solvent prepared in the step 3) to form a mixed solution, pouring the mixed solution into a test tube, heating by using an electric iron, and withdrawing the electric iron after the reaction is started until the reaction is finished to obtain a polymer; the mass of the hexagonal boron nitride nanosheet accounts for 1-9% of the mass of the second low eutectic agent, the mass of the cross-linking agent accounts for 1-3% of the mass of the second low eutectic agent, and the mass of the initiator accounts for 0.1-2% of the total mass of the second low eutectic agent;
5) cooling the polymer obtained in the step 4) to room temperature, then soaking and washing the polymer with deionized water, and after the soaking and washing are finished, carrying out freeze drying at the temperature of-50 ℃ to obtain the hexagonal boron nitride nanosheet hydrogel composite material.
2. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material according to claim 1, wherein the ultrasound time in the step 2) is 6-15 hours.
3. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material according to claim 1, wherein the rotation speed of a centrifuge used in the centrifugation in the step 2) is 6000 ± 100 rpm; the centrifugation time is 30-60 min.
4. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material according to claim 1, wherein the membrane used for suction filtration in step 2) is a nylon membrane, and after the suction filtration is completed, the membrane is again subjected to suction filtration by using distilled water, and the process is repeated three times.
5. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material according to claim 1, wherein the cross-linking agent in step 4) is N, N' -methylenebisacrylamide, and the initiator is any one of ammonium persulfate and potassium persulfate.
6. The method for preparing a hexagonal boron nitride nanosheet hydrogel composite according to claim 1, wherein the quaternary ammonium halide salt is choline chloride.
7. The method for preparing a hexagonal boron nitride nanosheet hydrogel composite according to claim 1, wherein the haloammonium salt is methyltributylammonium bromide.
8. The preparation method of the hexagonal boron nitride nanosheet hydrogel composite material according to claim 1, wherein the freeze-drying time in the step 5) is 12-24 hours.
9. The hexagonal boron nitride nanosheet hydrogel composite prepared according to any one of claims 1-8.
10. The use of a hexagonal boron nitride nanosheet hydrogel composite of claim 9 in dye wastewater, wherein the dye is methylene blue.
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Cited By (3)
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| CN114805925A (en) * | 2022-04-25 | 2022-07-29 | 西安理工大学 | Preparation method of h-BN/HQ/GO heat-conducting composite material |
| CN115041149A (en) * | 2022-06-20 | 2022-09-13 | 扬州工业职业技术学院 | Composite material for efficiently adsorbing ammonia |
| CN115448291A (en) * | 2022-10-13 | 2022-12-09 | 宁夏中星显示材料有限公司 | Carbon oxide quantum dot, carbon oxide quantum dot/sepiolite composite material, and preparation method and application thereof |
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