CN111957331A - TiO for water treatment2-MXene composite catalyst and preparation method thereof - Google Patents
TiO for water treatment2-MXene composite catalyst and preparation method thereof Download PDFInfo
- Publication number
- CN111957331A CN111957331A CN202010678001.7A CN202010678001A CN111957331A CN 111957331 A CN111957331 A CN 111957331A CN 202010678001 A CN202010678001 A CN 202010678001A CN 111957331 A CN111957331 A CN 111957331A
- Authority
- CN
- China
- Prior art keywords
- tio
- mxene
- composite catalyst
- preparation
- water treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 9
- 238000004729 solvothermal method Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 13
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 10
- 239000002904 solvent Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 4
- 230000002588 toxic effect Effects 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 description 14
- 239000012065 filter cake Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 230000006798 recombination Effects 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 229910009819 Ti3C2 Inorganic materials 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000001471 micro-filtration Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000001507 sample dispersion Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/32—Freeze drying, i.e. lyophilisation
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The embodiment of the invention provides TiO for water treatment2-MXene composite catalyst and preparation method thereof, comprising the following steps: mixing MXene and TiO2Mixing according to a preset proportion; adding water and/or absolute ethyl alcohol, carrying out ultrasonic treatment and stirring to obtain a mixed solution; subjecting the mixed solution to solvothermal treatment at a predetermined temperatureReacting, and cooling after the reaction to obtain a sample; drying the sample in a vacuum environment to obtain TiO2-MXene complex catalyst. The preparation method is simple in preparation process, the preparation of the composite catalyst is carried out in water or an absolute ethyl alcohol solvent, no toxic solvent is used, the environment is protected, the amount of the catalyst for degrading the high-concentration methylene blue solution is small, the degradation effect is good, and the production cost and the treatment cost are reduced.
Description
Technical Field
The invention relates to the technical field of water treatment catalysts, in particular to TiO for water treatment2-MXene composite catalyst and preparation method thereof.
Background
In recent years, researchers have made extensive research in this field because photocatalytic technology has unique advantages in the degradation of organic pollutants. According to the present research results, TiO2As a photocatalyst with high efficiency, no toxicity, stable photochemistry and low cost, the photocatalyst is effectively applied to the aspect of difficult degradation of organic pollutants. However, some problems still remain, such as TiO2Low quantum yield, easy agglomeration, low catalytic efficiency under visible light and the like, and prevents TiO from being used2The application of the catalytic degradation technology is developed. Therefore, researchers have adopted doping, co-deposition of noble metals, mixing of two semiconductors, and the like to improve TiO2The photocatalytic efficiency of (c). Although the above method can improve TiO to some extent2The photocatalytic activity of (a) is still problematic, but some key problems have not been solved. For example, there is thermal instability of the doped material, increased carrier recombination probability, etc.
Disclosure of Invention
The invention provides TiO for water treatment, which aims to solve the technical problem that the existing water treatment catalyst is not beneficial to use2-MXene composite catalyst and preparation method thereof.
The embodiment of the invention provides TiO for water treatment2The preparation method of the-MXene composite catalyst comprises the following steps:
s1, mixing MXene and TiO2Mixing according to a preset proportion;
s2, adding water and/or absolute ethyl alcohol, and carrying out ultrasonic treatment and stirring to obtain a mixed solution;
s3, carrying out solvothermal reaction on the mixed solution at a preset temperature, and cooling after the reaction to obtain a sample;
s4, drying the sample in a vacuum environment to obtain TiO2-MXene complex catalyst.
Further, the MXene has a single layer or multiple layers and is nano-sized or micro-sized in size.
Further, the TiO is2The particle size of the (B) is 10-50 nm.
Further, in step S1, TiO2And MXene ratio range 10: 1-4: 1.
further, in step S2, TiO2And the ratio of the mass of MXene to the volume of the mixed solution was 100 mg: (10-100 ml).
Further, in step S2, the volume ratio of the water to the absolute ethyl alcohol is 3: 1-0: 1.
Further, in step S2, the ultrasonic treatment time is 5-30 min, and the stirring time is 5-30 min.
Further, in step S3, the solvothermal reaction time is 1 to 5 hours.
Further, in step S3, the preset temperature is 100-200 ℃; in step S4, the vacuum drying temperature is 40-80 ℃.
In another aspect, the present invention also provides a TiO for water treatment2-MXene composite catalyst, said TiO for water treatment2the-MXene composite catalyst is prepared by the preparation method.
The invention has the beneficial effects that: the MXene adopted by the invention is a two-dimensional material, the specific surface area is large, and the MXene surface contains a large number of functional groupsElectronegativity, capable of efficiently neutralizing TiO2The TiO is bonded together by electrostatic adsorption and Van der Waals force2Can be stably attached to MXene surface, and inhibit TiO2The contact area between the particles and pollutants is increased, the active sites of the particles are increased, and the photocatalytic efficiency is effectively improved. The specific surface area of the composite catalyst is larger than that of TiO2Greatly improves the reaction efficiency and can further promote the light degradation reaction. In addition, MXene has excellent conductivity and can obviously inhibit nano TiO2The above electron-hole recombination promotes accumulation of electrons, and, TiO2The multilayer structure of the/MXene composite material can provide abundant surface active sites for photocatalysis, can also improve the adsorption effect on methylene blue solution, and the black MXene nanosheet can also improve the utilization efficiency of light, so that the photocatalysis effect of the methylene blue is improved. The preparation method is simple in preparation process, the preparation of the composite catalyst is carried out in water or an absolute ethyl alcohol solvent, no toxic solvent is used, the environment is protected, the amount of the catalyst for degrading the high-concentration methylene blue solution is small, the degradation effect is good, and the production cost and the treatment cost are reduced.
Drawings
FIG. 1 shows TiO obtained in example 1 of the present invention2SEM picture of MXene composite catalyst.
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.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
The embodiment of the invention provides TiO for water treatment2The preparation method of the-MXene composite catalyst comprises the following steps:
s1, mixing MXene and TiO2Mixing according to a preset proportion;
s2, adding water and/or absolute ethyl alcohol, and carrying out ultrasonic treatment and stirring to obtain a mixed solution;
s3, carrying out solvothermal reaction on the mixed solution at a preset temperature, and cooling after the reaction to obtain a sample;
s4, drying the sample in a vacuum environment to obtain TiO2-MXene complex catalyst.
The MXene adopted by the invention is a two-dimensional material, the specific surface area is large, and the MXene surface contains a large number of functional groups, is electronegative and can effectively react with TiO2The TiO is bonded together by electrostatic adsorption and Van der Waals force2Can be stably attached to MXene surface, and inhibit TiO2The contact area between the particles and pollutants is increased, the active sites of the particles are increased, and the photocatalytic efficiency is effectively improved. The specific surface area of the composite catalyst is larger than that of TiO2Greatly improves the reaction efficiency and can further promote the light degradation reaction. In addition, MXene has excellent conductivity and can obviously inhibit nano TiO2The above electron-hole recombination promotes accumulation of electrons, and, TiO2The multilayer structure of the/MXene composite material can provide abundant surface active sites for photocatalysis, can also improve the adsorption effect on methylene blue solution, and the black MXene nanosheet can also improve the utilization efficiency of light, so that the photocatalysis effect of the methylene blue is improved. The preparation method is simple in preparation process, the preparation of the composite catalyst is carried out in water or an absolute ethyl alcohol solvent, no toxic solvent is used, the environment is protected, the amount of the catalyst for degrading the high-concentration methylene blue solution is small, the degradation effect is good, and the production cost and the treatment cost are reduced.
Two-dimensional (2D) layered materials have been extensively studied for their particular physicochemical properties, in particular graphene analogues such as g-C3N4And MoS2The study of (a) has developed vigorously in the last decade. Recently, twoVascular lamellar materials MXenes (e.g. Ti)3C2、Ti2C、Nb2C、V2C and Mo2C) Have received attention from researchers to find Ti3C2Was investigated with Ti3C2The high conductivity of the catalyst is used as an auxiliary catalyst to improve the photocatalytic hydrogen production performance of the CdS. In-situ growth of TiO on MXene by calcination2Nanoparticles using CO2Catalytic reduction of CH4The performance of the composite material is increased by 3.4 times, the catalytic mechanism is that the composite material has a large number of surface active sites, and Ti3C2The ultra-high conductivity of the material promotes the transfer of photogenerated electrons and inhibits the recombination of the photogenerated electrons and photogenerated holes. TiO for water treatment prepared in the embodiment of the invention2the-MXene composite catalyst has the advantages of simple preparation process, low cost and good photocatalytic effect.
In an alternative embodiment, the MXene has a single layer or multiple layers with dimensions of nanometer or micrometer scale. The TiO is2The particle size of the (B) is 10-50 nm.
In an alternative embodiment, in step S1, the TiO is2And MXene ratio range 10: 1-4: 1.
in an alternative embodiment, in step S2, the TiO is2And the ratio of the mass of MXene to the volume of the mixed solution was 100 mg: (10-100 ml). The volume ratio of the water to the absolute ethyl alcohol is 3: 1-0: 1. the ultrasonic treatment time is 5-30 min, and the stirring time is 5-30 min.
In an alternative embodiment, in step S3, the solvothermal reaction time is 1h to 5 h. The preset temperature is 100-200 ℃.
In an alternative embodiment, in step S4, the vacuum drying temperature is 40-80 ℃.
In another aspect, the present invention also provides a TiO for water treatment2-MXene composite catalyst, said TiO for water treatment2the-MXene composite catalyst is prepared by the preparation method.
MXene is a two-dimensional material, and the ratio of MXene to MXene isThe surface area is large, and MXene surface contains a large number of functional groups and is electronegative, thus being capable of effectively reacting with TiO2The TiO is bonded together by electrostatic adsorption and Van der Waals force2Can be stably attached to MXene surface, and inhibit TiO2The contact area between the particles and pollutants is increased, the active sites of the particles are increased, and the photocatalytic efficiency is effectively improved. The specific surface area of the composite catalyst is larger than that of TiO2Greatly improves the reaction efficiency and can further promote the light degradation reaction. In addition, MXene has excellent conductivity and can obviously inhibit nano TiO2The above electron-hole recombination promotes accumulation of electrons, and, TiO2The multilayer structure of the/MXene composite material can provide abundant surface active sites for photocatalysis, can also improve the adsorption effect on methylene blue solution, and the black MXene nanosheet can also improve the utilization efficiency of light, so that the photocatalysis effect of the methylene blue is improved. The preparation method is simple in preparation process, the preparation of the composite catalyst is carried out in water or an absolute ethyl alcohol solvent, no toxic solvent is used, the environment is protected, the amount of the catalyst for degrading the high-concentration methylene blue solution is small, the degradation effect is good, and the production cost and the treatment cost are reduced.
The specific embodiment is as follows: TiO 22-MXene composite catalyst
Example 1:
300mg of TiO2Adding the nanometer powder into 10ml water, stirring for 5min, ultrasonically dispersing at room temperature for 30min, adding MXene into the TiO after ultrasonic dispersion2In the dispersion, MXene and TiO2The mass ratio of (1): and 9, adding absolute ethyl alcohol, wherein the volume ratio of the absolute ethyl alcohol to the ultrapure water is 1: stirring for 10min at low temperature, ultrasonically dispersing for 30min, and mixing MXene and TiO2Transferring the mixed dispersion liquid into a reaction kettle, performing solvothermal reaction in an oven, heating at a constant temperature for 180min, cooling to room temperature after the reaction is finished, repeatedly washing and filtering the reacted sample dispersion liquid by using a polytetrafluoroethylene hydrophilic microfiltration membrane to form a filter cake, drying the filter cake in a freeze dryer to constant weight, grinding the dried filter cake to powder to obtain TiO2And (3) adding 10mg of the MXene composite catalyst into 60mg of L-1 methylene blue solution, wherein the degradation rate under the ultraviolet condition can reach 87.72%.
FIG. 1 is TiO2SEM topography of-MXene composite catalyst, spherical particles are uniformly loaded on the plate-shaped object, wherein the diameter of the spherical particles is about 25nm and conforms to the P25 TiO2The flake is MXene, so that nano TiO can be obtained2The MXene is uniformly loaded on the surface of MXene to form the composite catalyst. .
Example 2:
300mg of TiO2Adding the nanometer powder into 10ml water, stirring for 5min, ultrasonically dispersing at room temperature for 30min, adding MXene into the TiO after ultrasonic dispersion2In the dispersion, MXene and TiO2The mass ratio of (1): and 4, adding absolute ethyl alcohol, wherein the volume ratio of the absolute ethyl alcohol to the ultrapure water is 1: stirring for 10min at low temperature, ultrasonically dispersing for 30min, and mixing MXene and TiO2Transferring the mixed dispersion liquid into a reaction kettle, performing solvothermal reaction in an oven, heating at a constant temperature for 180min, cooling to room temperature after the reaction is finished, repeatedly washing and filtering the reacted sample dispersion liquid by using a polytetrafluoroethylene hydrophilic microfiltration membrane to form a filter cake, drying the filter cake in a freeze dryer to constant weight, grinding the dried filter cake to powder to obtain TiO2And (3) taking 10mg of a sample of the-MXene composite catalyst, adding the sample into 60mg of L-1 methylene blue solution, wherein the degradation rate under the ultraviolet condition can reach 96.44%.
Example 3:
300mg of TiO2Adding the nanometer powder into 10ml water, stirring for 5min, ultrasonically dispersing at room temperature for 30min, adding MXene into the TiO after ultrasonic dispersion2In the dispersion, MXene and TiO2The mass ratio of (1): and 4, adding absolute ethyl alcohol, wherein the volume ratio of the absolute ethyl alcohol to the ultrapure water is 1: 3, stirring for 10min at low temperature, ultrasonically dispersing for 30min, and then mixing MXene and TiO2Transferring the mixed dispersion liquid into a reaction kettle, putting the reaction kettle into an oven for solvothermal reaction, and heating at constant temperature for 180min, the reaction temperature is 130 ℃, after the reaction is finished, the reaction solution is cooled to room temperature, the sample dispersion liquid after the reaction is repeatedly washed and filtered by a polytetrafluoroethylene hydrophilic microfiltration membrane to form a filter cake, the filter cake is dried to constant weight in a freeze dryer, the dried filter cake is ground to powder, and TiO can be obtained2And (3) taking 10mg of a sample of the MXene composite catalyst, adding the sample into a 60 mg.L-1 methylene blue solution, wherein the degradation rate under the ultraviolet condition can reach 92.14%.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.
Claims (10)
1. TiO for water treatment2The preparation method of the-MXene composite catalyst is characterized by comprising the following steps:
s1, mixing MXene and TiO2Mixing according to a preset proportion;
s2, adding water and/or absolute ethyl alcohol, and carrying out ultrasonic treatment and stirring to obtain a mixed solution;
s3, carrying out solvothermal reaction on the mixed solution at a preset temperature, and cooling after the reaction to obtain a sample;
s4, drying the sample in a vacuum environment to obtain TiO2-MXene complex catalysisAnd (3) preparing.
2. TiO for water treatment according to claim 12The preparation method of the MXene composite catalyst is characterized in that the MXene has a single layer or multiple layers and is nano-sized or micro-sized in size.
3. TiO for water treatment according to claim 12The preparation method of the (E) -MXene composite catalyst is characterized in that the TiO is2The particle size of the (B) is 10-50 nm.
4. TiO for water treatment according to claim 12The method for preparing the (E) -MXene composite catalyst is characterized in that, in the step S1, TiO is added2And MXene ratio range 10: 1-4: 1.
5. TiO for water treatment according to claim 12The method for preparing the (E) -MXene composite catalyst is characterized in that, in the step S2, TiO is added2And the ratio of the mass of MXene to the volume of the mixed solution was 100 mg: (10-100 ml).
6. TiO for water treatment according to claim 12The preparation method of the-MXene composite catalyst is characterized in that, in the step S2, the volume ratio of the water to the absolute ethyl alcohol is 3: 1-0: 1.
7. TiO for water treatment according to claim 12The preparation method of the-M Xene composite catalyst is characterized in that in the step S2, the ultrasonic treatment time is 5-30 min, and the stirring time is 5-30 min.
8. TiO for water treatment according to claim 12The preparation method of the-MXene composite catalyst is characterized in that in the step S3, the solvothermal reaction time is 1-5 h.
9. As claimed in claim1 the TiO for water treatment2The preparation method of the-MXene composite catalyst is characterized in that in the step S3, the preset temperature is 100-200 ℃; in step S4, the vacuum drying temperature is 40-80 ℃.
10. TiO for water treatment2-MXene composite catalyst, characterized in that said TiO for water treatment2the-MXene composite catalyst is prepared by the preparation method of any one of claims 1 to 9.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010678001.7A CN111957331A (en) | 2020-07-14 | 2020-07-14 | TiO for water treatment2-MXene composite catalyst and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010678001.7A CN111957331A (en) | 2020-07-14 | 2020-07-14 | TiO for water treatment2-MXene composite catalyst and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111957331A true CN111957331A (en) | 2020-11-20 |
Family
ID=73361475
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010678001.7A Pending CN111957331A (en) | 2020-07-14 | 2020-07-14 | TiO for water treatment2-MXene composite catalyst and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111957331A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112808253A (en) * | 2020-12-30 | 2021-05-18 | 合肥学院 | Electric field sensitive polyacrylamide/MXene hydrogel and preparation method and application thereof |
CN112933958A (en) * | 2021-02-10 | 2021-06-11 | 广西大学 | Method for photocatalytic carbon dioxide reduction |
CN113401937A (en) * | 2021-06-30 | 2021-09-17 | 河海大学 | MXene-TiO2Preparation method of (1) |
CN114452826A (en) * | 2021-12-14 | 2022-05-10 | 长安大学 | Light-driven self-cleaning Ti3C2@TiO2-C3N4Preparation method of heterojunction separation membrane |
CN114700095A (en) * | 2022-03-11 | 2022-07-05 | 华侨大学 | One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Preparation method of composite photocatalyst |
CN115845827A (en) * | 2022-11-22 | 2023-03-28 | 南京工业职业技术大学 | Has a photocatalytic functionOf TiO 2 2 Preparation method of substrate nano-sheet layer composite material, product and application |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105363483A (en) * | 2015-12-09 | 2016-03-02 | 陕西科技大学 | Preparation method of titanium dioxide nanowire/two-dimensional layered titanium carbide composite material |
AU2017101171A4 (en) * | 2017-08-25 | 2017-11-02 | Chen, Liang MR | The synthesis of GO/hemin/TiO2 nanocomposite catalyst and the photocatalytic degradation rate of organic pollutants |
CN109261181A (en) * | 2018-09-10 | 2019-01-25 | 浙江大学 | Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product |
CN109557159A (en) * | 2018-12-24 | 2019-04-02 | 青岛大学 | A kind of titanium carbide three-dimensional composite material and preparation method thereof and the application in building thrombin aptamers sensor |
CN110416507A (en) * | 2019-07-12 | 2019-11-05 | 广东工业大学 | A kind of three-dimensional flower-shaped cobalt disulfide of primary reconstruction/MXene composite material and preparation method and application |
RU2709599C1 (en) * | 2018-12-28 | 2019-12-18 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) | GAS SENSOR, A CHEMORESISTIVE TYPE MULTI-SENSOR RULER BASED ON OXIDIZED TWO-DIMENSIONAL TITANIUM CARBIDE (MXene) AND A METHOD FOR PRODUCTION THEREOF |
CN110841675A (en) * | 2019-11-21 | 2020-02-28 | 浙江大学 | Method for in-situ synthesis of BiOI composite catalyst and product |
-
2020
- 2020-07-14 CN CN202010678001.7A patent/CN111957331A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105363483A (en) * | 2015-12-09 | 2016-03-02 | 陕西科技大学 | Preparation method of titanium dioxide nanowire/two-dimensional layered titanium carbide composite material |
AU2017101171A4 (en) * | 2017-08-25 | 2017-11-02 | Chen, Liang MR | The synthesis of GO/hemin/TiO2 nanocomposite catalyst and the photocatalytic degradation rate of organic pollutants |
CN109261181A (en) * | 2018-09-10 | 2019-01-25 | 浙江大学 | Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product |
CN109557159A (en) * | 2018-12-24 | 2019-04-02 | 青岛大学 | A kind of titanium carbide three-dimensional composite material and preparation method thereof and the application in building thrombin aptamers sensor |
RU2709599C1 (en) * | 2018-12-28 | 2019-12-18 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) | GAS SENSOR, A CHEMORESISTIVE TYPE MULTI-SENSOR RULER BASED ON OXIDIZED TWO-DIMENSIONAL TITANIUM CARBIDE (MXene) AND A METHOD FOR PRODUCTION THEREOF |
CN110416507A (en) * | 2019-07-12 | 2019-11-05 | 广东工业大学 | A kind of three-dimensional flower-shaped cobalt disulfide of primary reconstruction/MXene composite material and preparation method and application |
CN110841675A (en) * | 2019-11-21 | 2020-02-28 | 浙江大学 | Method for in-situ synthesis of BiOI composite catalyst and product |
Non-Patent Citations (2)
Title |
---|
YUAN LIAO ET AL.: "2D-layered Ti3C2 MXenes for promoted synthesis of NH3 on P25 photocatalysts", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
郑会奇: "二维 Ti3C2Tx复合半导体材料的能带调控及光催化性能研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112808253A (en) * | 2020-12-30 | 2021-05-18 | 合肥学院 | Electric field sensitive polyacrylamide/MXene hydrogel and preparation method and application thereof |
CN112933958A (en) * | 2021-02-10 | 2021-06-11 | 广西大学 | Method for photocatalytic carbon dioxide reduction |
CN113401937A (en) * | 2021-06-30 | 2021-09-17 | 河海大学 | MXene-TiO2Preparation method of (1) |
CN114452826A (en) * | 2021-12-14 | 2022-05-10 | 长安大学 | Light-driven self-cleaning Ti3C2@TiO2-C3N4Preparation method of heterojunction separation membrane |
CN114452826B (en) * | 2021-12-14 | 2022-11-08 | 长安大学 | Light-driven self-cleaning Ti 3 C 2 @TiO 2 -C 3 N 4 Preparation method of heterojunction separation membrane |
CN114700095A (en) * | 2022-03-11 | 2022-07-05 | 华侨大学 | One-dimensional CdS nanorod/three-dimensional multilayer Ti3C2Preparation method of composite photocatalyst |
CN115845827A (en) * | 2022-11-22 | 2023-03-28 | 南京工业职业技术大学 | Has a photocatalytic functionOf TiO 2 2 Preparation method of substrate nano-sheet layer composite material, product and application |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111957331A (en) | TiO for water treatment2-MXene composite catalyst and preparation method thereof | |
Yu et al. | Decorating g-C3N4 nanosheets with Ti3C2 MXene nanoparticles for efficient oxygen reduction reaction | |
Han et al. | Graphene/graphitic carbon nitride hybrids for catalysis | |
Qiao et al. | Enhanced catalytic reduction of p-nitrophenol on ultrathin MoS2 nanosheets decorated with noble metal nanoparticles | |
Zhao et al. | A highly efficient composite catalyst constructed from NH2-MIL-125 (Ti) and reduced graphene oxide for CO2 photoreduction | |
Tian et al. | Zr-MOFs based on Keggin-type polyoxometalates for photocatalytic hydrogen production | |
Gu et al. | Hybrid of g-C3N4 assisted metal–organic frameworks and their derived high-efficiency oxygen reduction electrocatalyst in the whole pH range | |
Zhu et al. | Cobalt oxide supported on phosphorus-doped g-C3N4 as an efficient electrocatalyst for oxygen evolution reaction | |
Liu et al. | Nitrogen-doped graphene nanoribbons as efficient metal-free electrocatalysts for oxygen reduction | |
Wang et al. | CuO@ CoFe layered double hydroxide core–shell heterostructure as an efficient water oxidation electrocatalyst under mild alkaline conditions | |
Zhang et al. | Confining iron carbide nanocrystals inside CN x@ CNT toward an efficient electrocatalyst for oxygen reduction reaction | |
Qin et al. | Ni/Ni3C core/shell hierarchical nanospheres with enhanced electrocatalytic activity for water oxidation | |
Zhao et al. | Graphite-wrapped Fe core–shell nanoparticles anchored on graphene as pH-universal electrocatalyst for oxygen reduction reaction | |
Yang et al. | Silica nanosphere supported palladium nanoparticles encapsulated with graphene: high-performance electrocatalysts for methanol oxidation reaction | |
CN108772092B (en) | Ag3PO4/g-C3N4 composite tubular nano powder and preparation method thereof | |
Zhong et al. | Ti3C2 MXene/Ag2ZnGeO4 Schottky heterojunctions with enhanced photocatalytic performances: efficient charge separation and mechanism studies | |
Liang et al. | General synergistic capture-bonding superassembly of atomically dispersed catalysts on micropore-vacancy frameworks | |
Cheng et al. | In situ prepared nanosized Pt-Ag/PDA/PVA-co-PE nanofibrous membrane for highly-efficient catalytic reduction of p-nitrophenol | |
Ali et al. | Cobalt coordinated two-dimensional covalent organic framework a sustainable and robust electrocatalyst for selective CO2 electrochemical conversion to formic acid | |
Xi et al. | Probing activity enhancement of photothermal catalyst under near-infrared irradiation | |
Piri et al. | Silver nanoparticles supported on P, Se-codoped g-C3N4 nanosheet as a novel heterogeneous catalyst for reduction of nitroaromatics to their corresponding amines | |
Chen et al. | Interface engineering: Surface hydrophilic regulation of LaFeO3 towards enhanced visible light photocatalytic hydrogen evolution | |
CN109926054A (en) | A kind of preparation method of high dispersive NiCo alloy-graphene nano composite catalyst | |
Zhang et al. | Enhanced photocatalytic activities of CdS-BiOCl/PAN composites towards photocatalytic hydrogen evolution | |
CN108823601A (en) | A kind of preparation method of metal oxide/graphene composite film |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201120 |
|
RJ01 | Rejection of invention patent application after publication |