CN112473639A - Composite nano photocatalytic material and preparation method thereof - Google Patents
Composite nano photocatalytic material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 53
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000001154 acute effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
-
- B01J35/39—
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
Abstract
The invention provides a composite nano photocatalytic material and a preparation method thereof, wherein multi-walled carbon nanotubes and nano-scale titanium dioxide are used for preparing a net-shaped tube from the multi-walled carbon nanotubes, and the nano-scale titanium dioxide is mixed on the carbon nanotubes to obtain the composite nano photocatalytic material which is used for a purifier for removing formaldehyde. The invention maintains the original MwCNTs fiberMorphology, TiO2The coating and the carrier MWCNTs are tightly combined, and Ti-O-C bonds are formed, the existence of the carrier MWCNTs can effectively improve the specific surface area of the composite nano photocatalytic material, enhance the adsorption capacity to pollutants, and promote TiO2The transfer of the charged electrons to MWCNTs, the formation of Ti-O-C bonds being such that in TiO2Impurity levels are formed near the valence band to improve absorption and utilization of visible light, thus producing TiO2The MWCNTs composite photocatalytic material has higher visible light catalytic activity. The air purifier can realize no material consumption and reduce the cost.
Description
Technical Field
The invention mainly relates to the technical field of new photocatalytic materials, in particular to a composite nano photocatalytic material and a preparation method thereof.
Background
Among the numerous types of photocatalysts, there are,TiO2the compound has the characteristics of high activity, good thermal property, long persistence, low price, no toxicity, no harm and the like, and is favored by people.
How to prepare a catalyst which can maintain high catalytic activity and can be uniformly and firmly loaded on the surfaces of different materials is one of the key points of current photocatalyst research. But due to TiO2The absorption spectrum range is limited to ultraviolet light, and the recombination rate of photo-generated electrons and holes is high, which influence the photocatalytic efficiency. It is realized that the development of composite nano TiO with new properties2The importance of the material is improved, and the nano TiO2The absorption range of the nano-particle, the recombination time of charges is prolonged, the interface free energy is improved, and the form of the nano-particle is changed.
The carbon nano tube has special specific surface area and a special gap structure, the bonding state and the electronic state of the surface of the carbon nano tube are different from those of the interior of the particle, and the atomic coordination on the surface of the carbon nano tube is incomplete, so that the active position of the surface is increased, the carbon nano tube has certain degradation performance on organic matters, and basic conditions are provided for the carbon nano tube to be used as a catalyst. The carbon nanotube used as the TiO2 carrier has three advantages: firstly, the reaction rate is increased; secondly, the method has excellent selectivity for determining a reaction path; and thirdly, the reaction temperature is reduced.
Disclosure of Invention
The invention mainly provides a composite nano photocatalytic material and a manufacturing method thereof, which are used for solving the technical problems in the background technology.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a composite nano photocatalytic material, which comprises a multi-walled carbon nano-tube and nano-scale titanium dioxide, wherein the multi-walled carbon nano-tube is customized into a net-shaped tube, and the nano-titanium dioxide is mixed on the carbon nano-tube to obtain the composite nano photocatalytic material, and the composite nano photocatalytic material is used for a purifier for removing formaldehyde.
The invention provides a method for preparing a composite nano photocatalytic material, which specifically comprises the following steps:
s1, preparing materials
Multi-wall carbon nano-tube with purity over 95%, external diameter greater than 50nm, internal diameter of 5-15 nm and length of 10-20 um,
the length of the sharp TiO2 is 3-5 nm;
s2 purified multi-wall carbon nano-tube
Calcining a multi-walled carbon nanotube at a constant temperature of 450 ℃ for 1h under the protection of nitrogen atmosphere, placing the calcined multi-walled carbon nanotube in a sand core crucible, then placing nitric acid at the bottom of a polytetrafluoroethylene liner, then placing the sand core crucible in the polytetrafluoroethylene liner, finally transferring the liner to a hydrothermal kettle, reacting for 3h in a drying oven at 120 ℃, cooling to room temperature after the reaction is finished, taking out, repeatedly centrifuging and washing with deionized water to be neutral, drying and collecting for later use;
s3, weighing anhydrous KCI and LiCl according to a certain ratio, placing the weighed anhydrous KCI and LiCl into a grinding machine, uniformly mixing, and adding the multi-walled carbon nano tube and titanium powder;
s4, uniformly grinding and mixing the materials, then putting the mixture into a corundum crucible, putting the corundum crucible into a tubular molten salt furnace after covering, introducing argon with the purity of 99.99 percent as protective gas, and preserving heat for 3 hours at 700-850 ℃;
s5, taking out the crucible after the furnace temperature is reduced to room temperature, repeatedly washing the crucible by distilled water until no chloride ion Cl & lt- & gt exists, and separating an intermediate product, namely the titanium carbide coated multi-walled carbon nanotube;
s6, drying at a constant temperature of 60 ℃ by using drying equipment to obtain the multi-walled carbon nanotube coated with titanium carbide;
s7, placing the dried product in a container, placing the container in a tubular resistance furnace, introducing mixed air to provide an oxidizing atmosphere, keeping the flow rate at 0.2L/min and the heating rate at 5 ℃/min to reach a preset oxidizing temperature, preserving the temperature for a period of reaction time, and cooling to room temperature to obtain a product with the surface coated with TiO: the multi-wall carbon nano tube is obtained.
Preferably, in step S3, the molar ratio of the multi-walled carbon nanotubes to the titanium powder is 1: 5.
Preferably, in step S2, the ratio of the multi-walled carbon nanotubes in the nitric acid solution is 1.6 g/mL.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the multi-walled carbon nano-tube as a reactive template to prepare the catalyst with MWCNTs as a carrier and uniform TiO on the surface2The composite nanometer photocatalytic material of the coating.
The invention keeps the fibrous shape of the original MwCNTs, TiO2The coating and the carrier MWCNTs are tightly combined, and Ti-O-C bonds are formed, the existence of the carrier MWCNTs can effectively improve the specific surface area of the composite nano photocatalytic material, enhance the adsorption capacity to pollutants, and promote TiO2The transfer of the charged electrons to MWCNTs, the formation of Ti-O-C bonds being such that in TiO2Impurity levels are formed near the valence band to improve absorption and utilization of visible light, thus producing TiO2The MWCNTs composite photocatalytic material has higher visible light catalytic activity.
The present invention will be explained in detail below with reference to the drawings and specific embodiments.
Drawings
FIG. 1 is a schematic diagram of the reaction of the present invention;
FIG. 2 is a molecular structure diagram of the composite nano photocatalytic material of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in different forms and not limited to the embodiments described herein, but which are provided so as to provide a more thorough and complete disclosure of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the knowledge of the terms used herein in the specification of the present invention is for the purpose of describing particular embodiments and is not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Examples
The embodiment provides a composite nano photocatalytic material, namely a multi-walled carbon nanotube and nano-scale titanium dioxide, a reticular tube is customized by the multi-walled carbon nanotube, and the nano-scale titanium dioxide is mixed on a carbon nanotube to obtain the composite nano photocatalytic material, wherein the composite nano photocatalytic material is used for a purifier for removing formaldehyde.
The embodiment provides a method for preparing a composite nano photocatalytic material, which specifically comprises the following steps:
s1, preparing materials
Multi-wall carbon nano-tube with purity over 95%, external diameter greater than 50nm, internal diameter of 5-15 nm and length of 10-20 um,
acute form of TiO2The length is 3-5 nm;
s2 purified multi-wall carbon nano-tube
Calcining a multi-walled carbon nanotube at a constant temperature of 450 ℃ for 1h under the protection of nitrogen atmosphere, placing the calcined multi-walled carbon nanotube in a sand core crucible, then placing nitric acid at the bottom of a polytetrafluoroethylene liner, then placing the sand core crucible in the polytetrafluoroethylene liner, finally transferring the liner to a hydrothermal kettle, reacting for 3h in a drying oven at 120 ℃, cooling to room temperature after the reaction is finished, taking out, repeatedly centrifuging and washing with deionized water to be neutral, drying and collecting for later use;
s3, weighing anhydrous KCI and LiCl according to a certain ratio, placing the weighed anhydrous KCI and LiCl into a grinding machine, uniformly mixing, and adding the multi-walled carbon nano tube and titanium powder;
s4, uniformly grinding and mixing the materials, then putting the mixture into a corundum crucible, putting the corundum crucible into a tubular molten salt furnace after covering, introducing argon with the purity of 99.99 percent as protective gas, and preserving heat for 3 hours at 700-850 ℃;
s5, taking out the crucible after the furnace temperature is reduced to room temperature, and repeatedly washing the crucible by distilled water until no chloride ions Cl exist-The intermediate product, namely the titanium carbide coated multi-wall carbon nano-tube, exists and is separated from the intermediate product;
s6, drying at a constant temperature of 60 ℃ by using drying equipment to obtain the multi-walled carbon nanotube coated with titanium carbide;
s7, placing the dried product in a container, placing the container in a tubular resistance furnace, introducing mixed air to provide an oxidizing atmosphere, keeping the flow rate at 0.2L/min and the heating rate at 5 ℃/min to reach a preset oxidizing temperature, preserving the temperature for a period of reaction time, and cooling to room temperature to obtain a product with the surface coated with TiO: the multi-wall carbon nano tube is obtained.
In step S3, the molar ratio of the multi-walled carbon nanotubes to the titanium powder is 1: 5.
In step S2, the ratio of the multi-walled carbon nanotubes to the nitric acid solution is 1.6 g/mL.
The principle of the invention is that MWCNTs are used as a carrier to prepare the catalyst with uniform TiO on the surface by using the multiwalled carbon nanotube as a reactive template2The prepared catalyst basically keeps the fibrous shape of the original MwCNTs, and TiO is used as a catalyst2The coating and the MWCNTs are tightly combined, and a Ti-o-C bond is formed, and the existence of the MWCNTs can effectively improve the specific surface area of the composite photocatalyst, enhance the adsorption capacity to pollutants and promote TiO2The transfer of the charged electrons to MWCNTs, the formation of Ti-O-C bonds being such that in TiO2Impurity levels are formed near the valence band to improve absorption and utilization of visible light, thus producing TiO2the/MwCNTs composite photocatalyst shows higher visible light catalytic activity.
The invention is described above with reference to the accompanying drawings, it is obvious that the invention is not limited to the above-described embodiments, and it is within the scope of the invention to adopt such insubstantial modifications of the inventive method concept and solution, or to apply the inventive concept and solution directly to other applications without modification.
Claims (4)
1. The composite nanometer photocatalytic material is characterized in that a multiwall carbon nanotube and nanometer titanium dioxide are adopted, a netted tube is customized by the multiwall carbon nanotube, and the nanometer titanium dioxide is mixed on the carbon nanotube to obtain the composite nanometer photocatalytic material, wherein the composite nanometer photocatalytic material is used for a purifier for removing formaldehyde.
2. The method for preparing a composite nano photocatalytic material according to claim 1, is characterized by comprising the following steps:
s1, preparing materials
Multi-wall carbon nano-tube with purity over 95%, external diameter greater than 50nm, internal diameter of 5-15 nm and length of 10-20 um,
acute form of TiO2The length is 3-5 nm;
s2 purified multi-wall carbon nano-tube
Calcining a multi-walled carbon nanotube at a constant temperature of 450 ℃ for 1h under the protection of nitrogen atmosphere, placing the calcined multi-walled carbon nanotube in a sand core crucible, then placing nitric acid at the bottom of a polytetrafluoroethylene liner, then placing the sand core crucible in the polytetrafluoroethylene liner, finally transferring the liner to a hydrothermal kettle, reacting for 3h in a drying oven at 120 ℃, cooling to room temperature after the reaction is finished, taking out, repeatedly centrifuging and washing with deionized water to be neutral, drying and collecting for later use;
s3, weighing anhydrous KCI and LiCl according to a certain ratio, placing the weighed anhydrous KCI and LiCl into a grinding machine, uniformly mixing, and adding the multi-walled carbon nano tube and titanium powder;
s4, uniformly grinding and mixing the materials, then putting the mixture into a corundum crucible, putting the corundum crucible into a tubular molten salt furnace after covering, introducing argon with the purity of 99.99 percent as protective gas, and preserving heat for 3 hours at 700-850 ℃;
s5, taking out the crucible after the furnace temperature is reduced to room temperature, and repeatedly washing the crucible by distilled water until no chloride ions Cl exist-The intermediate product, namely the titanium carbide coated multi-wall carbon nano-tube, exists and is separated from the intermediate product;
s6, drying at a constant temperature of 60 ℃ by using drying equipment to obtain the multi-walled carbon nanotube coated with titanium carbide;
s7, placing the dried product in a container, placing the container in a tubular resistance furnace, introducing mixed air to provide an oxidizing atmosphere, keeping the flow rate at 0.2L/min and the heating rate at 5 ℃/min to reach a preset oxidizing temperature, preserving the temperature for a period of reaction time, and cooling to room temperature to obtain a product with the surface coated with TiO: the multi-wall carbon nano tube is obtained.
3. The method of claim 2, wherein the molar ratio of the multi-walled carbon nanotubes to the titanium powder is 1: 5.
4. The composite nano-photocatalytic material and its manufacturing method according to claim 2, wherein in step S2, the ratio of the multi-walled carbon nanotubes to nitric acid solution is 1.6 g/mL.
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| CN109364902A (en) * | 2018-10-15 | 2019-02-22 | 天津工业大学 | A kind of preparation method of functionalized multi-wall carbonnanotubes/titanium dioxide optical catalyst |
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