CN111790417A - Mxene-derived TiO2Nanosheet-graphene gel composite material and preparation method and application thereof - Google Patents
Mxene-derived TiO2Nanosheet-graphene gel composite material and preparation method and application thereof Download PDFInfo
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- CN111790417A CN111790417A CN202010445742.0A CN202010445742A CN111790417A CN 111790417 A CN111790417 A CN 111790417A CN 202010445742 A CN202010445742 A CN 202010445742A CN 111790417 A CN111790417 A CN 111790417A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 83
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 108
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000499 gel Substances 0.000 claims abstract description 33
- 239000011259 mixed solution Substances 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- 239000000017 hydrogel Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000004964 aerogel Substances 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 7
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 231100000512 nanotoxicity Toxicity 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B01J35/23—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- B01J35/39—
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- B01J35/40—
Abstract
The invention provides an Mxene derived TiO2 nanosheet-graphene gel composite material as well as a preparation method and application thereof, wherein the preparation method comprises the following steps: forming a graphene oxide aqueous solution in the aqueous solution by using graphite oxide; adding Mxene into a graphene oxide aqueous solution to obtain a first mixed solution; adding a reducing agent into the first mixed solution, and carrying out water bath to form Mxene-graphene hydrogel; adding the crystal face control agent into water to obtain a second mixed solution; placing the Mxene-graphene hydrogel in a second mixed solution and carrying out hydrothermal reaction to obtain TiO2 nanosheet-graphene hydrogel; freeze-drying to obtain a TiO2 nanosheet-graphene aerogel composite material; the TiO2 nanosheets in the material obtained by the method are regular in shape, uniform in size and uniform in crystalline phase; the addition of the graphene enhances the utilization rate of visible light and the electron transmission efficiency, and the macroscopic body of the composite material is easy to separate.
Description
Technical Field
The invention belongs to the technical field of synthesis of environmental materials, and particularly relates to an Mxene-derived TiO2 nanosheet-graphene gel composite material, and a preparation method and application thereof.
Background
In recent years, the two-dimensional nano material shows wide development potential in the field of photocatalysis application, compared with the similar materials, the large surface area/volume ratio of the two-dimensional nano material increases the active sites on the surface, and the ultra-thin structure reduces the migration distance from the block body to the surface, thereby reducing the photocatalysis performance of the composite reinforced material of the photon-generated carrier. The TiO2 nanosheet has excellent light absorption efficiency and electron transmission rate, but when the TiO2 nanosheet is synthesized by adopting a traditional hydrothermal method, the TiO2 nanosheet is easy to agglomerate during growth due to the strong surface activity, the length and the thickness of the prepared nanosheet are not easy to control, and the exertion of the excellent performance of the TiO2 nanosheet is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention mainly aims to provide an Mxene-derived TiO2 nanosheet-graphene gel composite material.
The second purpose of the invention is to provide a preparation method of the Mxene-derived TiO2 nanosheet-graphene gel composite material.
A third object of the present invention is to provide the use of the Mxene-derivatized TiO2 nanosheet-graphene gel composite described above.
In order to achieve the above purpose, the solution of the invention is as follows:
a preparation method of an Mxene derived TiO2 nanosheet-graphene gel composite material comprises the following steps: forming a graphene oxide aqueous solution in the aqueous solution by using graphite oxide; adding Mxene into a graphene oxide aqueous solution to obtain a first mixed solution; adding a reducing agent into the first mixed solution, and carrying out water bath to form Mxene-graphene hydrogel; adding the crystal face control agent into water to obtain a second mixed solution; placing the Mxene-graphene hydrogel in a second mixed solution and carrying out hydrothermal reaction to obtain TiO2 nanosheet-graphene hydrogel; and freeze-drying to obtain the TiO2 nanosheet-graphene aerogel composite material. The TiO2 nanosheets in the material obtained by the method are regular in shape, uniform in size and uniform in crystalline phase; the addition of the graphene enhances the utilization rate of visible light and the electron transmission efficiency, and the macroscopic body of the composite material is easy to separate.
A preparation method of an Mxene derived TiO2 nanosheet-graphene gel composite material specifically comprises the following steps:
(1) forming a graphene oxide aqueous solution in the aqueous solution by using graphite oxide;
(2) adding Mxene into the graphene oxide aqueous solution to obtain a first mixed solution;
(3) adding a reducing agent into the first mixed solution and carrying out water bath to form Mxene-graphene hydrogel;
(4) adding the crystal face control agent into water to obtain a second mixed solution;
(5) placing the Mxene-graphene hydrogel in a second mixed solution and carrying out hydrothermal reaction to obtain a TiO2 nanosheet-graphene hydrogel;
(6) and freeze-drying the composite material to obtain the TiO2 nanosheet-graphene aerogel composite material.
Preferably, in the step (1), the concentration of the graphene oxide in the graphene oxide aqueous solution is 2-8 mg/mL.
Preferably, in step (2), the Mxene added is Ti3C2Tx, and the ratio of the Mxene added to the graphite oxide is 0.5-2.
Preferably, in step (3), the reducing agent is selected from ascorbic acid, sodium ascorbate, oxalic acid, anhydrous sodium iodide, sodium hypophosphite, sodium sulfite, sodium sulfide, hydrogen iodide.
Preferably, in step (3), the reducing agent is added in a ratio of 1 to 3 to the graphite oxide.
Preferably, in step (3), the temperature of the water bath heating is 80-95 ℃.
Preferably, in the step (4), the crystal plane control agent is NaBF4 and HCL.
Preferably, in the step (4), the concentration of NaBF4 is 0.1 mol/L.
Preferably, in step (4), the concentration of HCL is 1.0 mol/L.
Preferably, in step (5), the hydrothermal temperature is 160 ℃.
Preferably, in the step (5), the hydrothermal time is greater than or equal to 9-12 h.
An Mxene-derived TiO2 nanosheet-graphene gel composite material is prepared by the preparation method.
The Mxene-derived TiO2 nanosheet-graphene gel composite material is applied to the field of photocatalysis.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the invention skillfully utilizes the instability of a two-dimensional Mxene material and adds a crystal face control agent to generate an ultrathin TiO2 nanosheet with uniform crystal phase.
Secondly, the formation of the graphene gel network enables the limited growth of the TiO2 nanosheets, avoids the agglomeration of the TiO2 nanosheets, and enables the obtained TiO2 nanosheets to be regular in shape and uniform in size.
Thirdly, the compounding of the graphene can reduce the band gap of the material, increase the absorption of visible light, enhance photoelectron transfer to reduce the compounding of photo-generated electron holes and improve the photocatalytic performance.
Fourthly, the Mxene derived TiO2 nanosheet-graphene gel macroscopic body obtained by the method is easy to separate, and the nano toxicity of the material is reduced.
In a word, the Mxene (two-dimensional transition metal carbon/nitride) and graphene excellent properties are utilized, the Mxene is oxidized to generate an ultrathin two-dimensional TiO2 nanosheet by utilizing the instability of the Mxene, the TiO2 nanosheet grows in a limited mode by utilizing the porous network structure of the graphene gel and adding a crystal face control agent, the agglomeration of the TiO2 nanosheet is effectively avoided, and the Mxene derived TiO2 nanosheet-graphene gel composite material which is regular in shape, uniform in size and uniform in crystal phase is obtained.
Drawings
Fig. 1 is a transmission electron micrograph of Mxene-derived TiO2 nanosheet-graphene gel composite in example 2.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1:
the preparation method of the Mxene-derived TiO2 nanosheet-graphene gel composite material of the embodiment comprises the following steps:
(1) weighing 0.5g of graphite oxide, dissolving in a neutral aqueous solution, transferring into a 250mL volumetric flask, and stirring and performing ultrasonic treatment for 300min to form a uniform graphene oxide aqueous solution, wherein the concentration of the graphene oxide is 2 mg/mL;
(2) adding 0.5g of Ti3C2Tx into the graphene oxide aqueous solution, performing ultrasonic treatment for 300min, and uniformly dispersing to obtain a first mixed solution;
(3) adding 0.5g of sodium ascorbate into the first mixed solution, performing ultrasonic treatment for 15min to uniformly disperse the sodium ascorbate, performing water bath at 95 ℃ for 6h to form Mxene-graphene hydrogel, and washing away impurities remained in the gel with distilled water;
(4) preparing a solution of 0.1mol/L NaBF4 and 1.0mol/L HCL as a second mixed solution;
(5) placing the Mxene-graphene hydrogel in the second mixed solution in the step (3) in a hydrothermal kettle, reacting for 12 hours at 160 ℃ to obtain TiO2 nanosheet-graphene hydrogel, and washing away impurities remained in gel spheres by using distilled water;
(6) and (3) freeze-drying the composite material for 48 hours to obtain the TiO2 nanosheet-graphene aerogel composite material.
Example 2:
the preparation method of the Mxene-derived TiO2 nanosheet-graphene gel composite material of the embodiment comprises the following steps:
(1) weighing 0.5g of graphite oxide, dissolving in a neutral aqueous solution, transferring into a 250mL volumetric flask, and stirring and performing ultrasonic treatment for 300min to form a uniform graphene oxide aqueous solution, wherein the concentration of the graphene oxide is 2 mg/mL;
(2) adding 0.25g of Ti3C2Tx into the graphene oxide aqueous solution, performing ultrasonic treatment for 300min, and uniformly dispersing to obtain a first mixed solution;
(3) adding 0.5g of sodium ascorbate into the first mixed solution, performing ultrasonic treatment for 15min to uniformly disperse the sodium ascorbate, performing water bath at 95 ℃ for 6h to form Mxene-graphene hydrogel, and washing away impurities remained in the gel with distilled water;
(4) preparing a solution of 0.1mol/L NaBF4 and 1.0mol/L HCL as a second mixed solution;
(5) placing the Mxene-graphene hydrogel in the second mixed solution in the step (3) in a hydrothermal kettle, reacting for 9 hours at 160 ℃ to obtain TiO2 nanosheet-graphene hydrogel, and washing away impurities remained in gel spheres by using distilled water;
(6) and (3) freeze-drying the composite material for 48 hours to obtain the TiO2 nanosheet-graphene aerogel composite material.
Fig. 1 is a transmission electron microscope image of an Mxene-derived TiO2 nanosheet-graphene gel composite material according to an embodiment of the present invention, and it can be seen from the image that TiO2 nanosheets with a length and a width of about 150nm and a regular shape are grown on the surface of few-layer graphene in graphene gel.
An Mxene-derived TiO2 nanosheet-graphene gel composite material can be used as a photocatalyst.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (9)
1. A preparation method of Mxene derived TiO2 nanosheet-graphene gel composite material is characterized by comprising the following steps: forming a graphene oxide aqueous solution in the aqueous solution by using graphite oxide; adding Mxene into a graphene oxide aqueous solution to obtain a first mixed solution; adding a reducing agent into the first mixed solution, and carrying out water bath to form Mxene-graphene hydrogel; adding the crystal face control agent into water to obtain a second mixed solution; placing the Mxene-graphene hydrogel in a second mixed solution and carrying out hydrothermal reaction to obtain TiO2 nanosheet-graphene hydrogel; and freeze-drying to obtain the TiO2 nanosheet-graphene aerogel composite material.
2. The method for preparing an Mxene-derived TiO2 nanosheet-graphene gel composite material of claim 1, wherein: which comprises the following steps:
(1) forming a graphene oxide aqueous solution in the aqueous solution by using graphite oxide;
(2) adding Mxene into the graphene oxide aqueous solution to obtain a first mixed solution;
(3) adding a reducing agent into the first mixed solution and carrying out water bath to form Mxene-graphene hydrogel;
(4) adding the crystal face control agent into water to obtain a second mixed solution;
(5) placing the Mxene-graphene hydrogel in a second mixed solution and carrying out hydrothermal reaction to obtain a TiO2 nanosheet-graphene hydrogel;
(6) and freeze-drying the composite material to obtain the TiO2 nanosheet-graphene aerogel composite material.
3. A method of preparing a Mxene derivatized TiO2 nanoplatelet-graphene gel composite material according to claim 2, characterized in that: in the step (1), the concentration of graphene oxide in the graphene oxide aqueous solution is 2-8 mg/mL;
in the step (2), the added Mxene is Ti3C2Tx, and the ratio of the added Mxene to the graphite oxide is 0.5-2.
4. A method of preparing a Mxene derivatized TiO2 nanoplatelet-graphene gel composite material according to claim 2, characterized in that: in the step (3), the reducing agent is selected from ascorbic acid, sodium ascorbate, oxalic acid, anhydrous sodium iodide, sodium hypophosphite, sodium sulfite, sodium sulfide and hydrogen iodide.
5. A method of preparing a Mxene derivatized TiO2 nanoplatelet-graphene gel composite material according to claim 2, characterized in that: step (3), the ratio of the reducing agent to the graphite oxide is 1-3;
in the step (3), the temperature of the water bath heating is 80-95 ℃.
6. The method of preparing a Mxene-derivatized TiO2 nanosheet-graphene gel composite material of claim 1, wherein: in the step (4), the crystal face control agents are NaBF4 and HCL;
in the step (4), the concentration of NaBF4 is 0.1 mol/L;
in the step (4), the concentration of the HCL is 1.0 mol/L.
7. The method of preparing a Mxene-derivatized TiO2 nanosheet-graphene gel composite material of claim 1, wherein: in the step (5), the hydrothermal temperature is 160 ℃;
in the step (5), the hydrothermal time is more than or equal to 9-12 h.
8. An Mxene derived TiO2 nanosheet-graphene gel composite material is characterized in that: obtained by the process according to any one of claims 1 to 11.
9. An Mxene-derived TiO2 nanosheet-graphene gel composite material as defined in claim 8, being applied to the field of photocatalysis.
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| CN113501542A (en) * | 2021-07-12 | 2021-10-15 | 中国石油大学(华东) | Dielectric film based on plate-barrier structure nano filler composition |
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| CN114377706A (en) * | 2022-01-04 | 2022-04-22 | 上海第二工业大学 | MXene/TiO loaded by glass fiber ball bundle2Aerogel composite material and preparation method thereof |
| CN116889867A (en) * | 2023-06-20 | 2023-10-17 | 盐城工学院 | MXene derived porous TiO 2 Method for preparing RGO nano-sheet composite photocatalyst and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113501542A (en) * | 2021-07-12 | 2021-10-15 | 中国石油大学(华东) | Dielectric film based on plate-barrier structure nano filler composition |
| CN113718281A (en) * | 2021-09-26 | 2021-11-30 | 河海大学 | Graphene quantum dot/MXene nanosheet two-dimensional composite material and preparation method and application thereof |
| CN114377706A (en) * | 2022-01-04 | 2022-04-22 | 上海第二工业大学 | MXene/TiO loaded by glass fiber ball bundle2Aerogel composite material and preparation method thereof |
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| CN116889867A (en) * | 2023-06-20 | 2023-10-17 | 盐城工学院 | MXene derived porous TiO 2 Method for preparing RGO nano-sheet composite photocatalyst and application thereof |
| CN116889867B (en) * | 2023-06-20 | 2024-04-05 | 盐城工学院 | MXene derived porous TiO 2 Method for preparing RGO nano-sheet composite photocatalyst and application thereof |
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