CN110787784A - Silk screen type TiO2Device and method for photocatalytic degradation of VOCs (volatile organic compounds) by nanotube array - Google Patents
Silk screen type TiO2Device and method for photocatalytic degradation of VOCs (volatile organic compounds) by nanotube array Download PDFInfo
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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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- 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
- B01D53/007—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 by irradiation
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- 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
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/804—UV light
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
Abstract
The invention belongs to the technical field of waste gas treatment and discloses a silk screen type TiO2A device and a method for degrading VOCs by nanotube array photocatalysis. The device comprises a box body, wherein one end of the box body is provided with an air inlet, and the other end of the box body is provided with an air outlet; multilayer surface-covering TiO is fixedly arranged in the box body in the direction vertical to the air inlet and the air outlet2The titanium silk screen film of the nanotube array has no gap between the titanium silk screen film and the box body, and an ultraviolet lamp is arranged between two adjacent layers of the titanium silk screen films. The invention of the wire mesh type TiO2The nanotube array can be used as a novel core catalytic material of an air purifying agent, is applied to actual air purifying work, and effectively solves the problem that indoor formaldehyde harms human bodies.
Description
Technical Field
The invention belongs to the technical field of waste gas treatment, and particularly relates to a silk screen type TiO2A device and a method for degrading VOCs by nanotube array photocatalysis.
Background
Titanium dioxide is used as an environment-friendly pollution treatment material, has wide attention on application prospects in the aspects of environmental protection and energy conservation, and is mainly applied to the fields of wastewater and waste gas treatment, development of antibacterial and self-cleaning products and the like. Titanium dioxide has three main forms: anatase, rutile, and brookite. The photocatalytically active forms generally used predominantly are both the ruthenite and rutile types. Currently, indoor air pollution has become the third pollution era following soot-type pollution and photochemical pollution. The indoor decoration material is mainly characterized in that the hidden danger of generating indoor air pollutants such as benzene, toluene, formaldehyde and the like exists in most modern indoor decoration materials, so that the indoor air quality is reduced, the human health is harmed, and a series of uncomfortable symptoms caused by indoor decoration are collectively called as indoor building syndromes. Formaldehyde is one of the major pollutants in indoor air and was identified as a suspected carcinogen by the international cancer research institute in 1955. At present, formaldehyde discharged into air by fuel, decoration materials and the like is increased year by year, and particularly, formaldehyde pollution caused by indoor decoration has attracted great attention.
In 1972, FujiShima and Honda reported the light irradiation of TiO in photovoltaic cells2Redox reaction of sustainable water to produce H2And O2Frank et al made a breakthrough in the use of semiconductor materials to catalyze photolysis of pollutants in 1976. The photocatalytic oxidation method has simple structure, easy control of operation conditions, strong oxidation capacity and no secondary pollution, and the TiO is added2High chemical stability, no poison and low cost, so TiO2The photocatalytic oxidation method used as a catalyst is a new water treatment technology with wide application prospect at home and abroad, and then scientists gradually expand the effect of the photocatalytic oxidation method to more fields.
Kasuga et al prepared TiO in 1998 by hydrothermal method2Since nanotubes, TiO prepared by hydrothermal synthesis have been discovered2The nanotube has high yield, small diameter, large specific surface area, uniform diameter, good dispersibility, and specific TiO ratio2Has the characteristics of higher photocatalytic activity, easy recovery and the like, and TiO2The research of the nanotube becomes a hot spot of research of researchers. But due to TiO2The nanotube array is grown on a Ti substrate and cannot be used for air filtration, resulting in TiO2Few research reports on the application of nanotube arrays to the degradation of pollutants in air have been reported.
Since Zwilling et al first reported that nanotubes were prepared by anodic oxidation in 1999, among nanotube preparation methods, anodic oxidation has attracted researchers' great interest because of the highly ordered, controllable size of the prepared nanotubes and the ability to integrate nanotubes into titanium nanotube arrays. The titanium nanotube array prepared by the anodic oxidation method grows perpendicular to a titanium substrate, the top end of the titanium nanotube array is open, a titanium sheet is used as a receptor of a tunner, a photogenerated carrier is conveniently and rapidly separated before compounding, the propagation of sudden scattered photons on the inner surface and the outer surface of the whole nanotube in the length direction is facilitated, the absorbance is improved, the penetration path of electrons of the nanotube array is shortened due to the high order of the nanotube array, and the separation efficiency and the total light conversion efficiency of electron hole pairs are improved. Nanotube arrays prepared by anodic oxidation are complete, fixed arrays immobilized on large surfaces, which facilitate continuous or batch placement into photocatalytic reactors without the need for expensive solid-liquid separation steps. Incipient TiO2The length of the nanotube is only hundreds of nanometers, the orderliness is not high, and the nanotube has high specific surface area and high order and the length of the nanotube reaches hundreds of micrometers. In addition, the inner diameter, wall thickness and length of the nanotube can be designed and controlled to adjust the transmission and absorption of visible light.
2001, Grimes, an American scientist, prepares TiO by utilizing an electrochemical anodic oxidation method2Nano array materials attract great attention. TiO prepared by anode oxidation technology2The nanotubes are uniformly distributed and uniformly arranged in a very regular array form, and the nanotubes are directly connected with the metal titanium conductive substrate through Schottky barriers, so that the combination is firm and the nanotubes are not easy to wash and fall off. The material has extremely high ordered structure and extremely low agglomeration degree, and simultaneously has very high quantum effect.
Overall, foreign countries have discovered TiO2After the photocatalytic reaction can take place, the research on the reaction efficiency of the photocatalytic reaction is more expanded, namely TiO2Modification studies of nanotubes are currently the mainstream direction.
Earlier patent application 201811016004.3 discloses a wire mesh type TiO2The technology for treating organic wastewater by nano material photoelectrocatalysis needs to adopt a direct current power supply to assist a photocatalysis material, realizes photoelectricity field coupling photocatalysis, and is mainly used for treating organic wastewater; it does not disclose achieving degradation of VOCs, particularly formaldehyde.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide the silk screen type TiO2A device for degrading VOCs by nanotube array photocatalysis.
Another object of the present invention is to provide a wire mesh type TiO2A method for degrading VOCs by nanotube array photocatalysis.
The purpose of the invention is realized by the following technical scheme:
silk screen type TiO2The device for degrading VOCs (volatile organic compounds) through the photocatalysis of the nanotube array comprises a box body, wherein one end of the box body is provided with an air inlet, and the other end of the box body is provided with an air outlet; multilayer surface-covering TiO is fixedly arranged in the box body in the direction vertical to the air inlet and the air outlet2The titanium silk screen film of the nanotube array has no gap between the titanium silk screen film and the box body, and an ultraviolet lamp is arranged between two adjacent layers of the titanium silk screen films.
Further, an exhaust fan is arranged in the exhaust port.
Further, the surface is coated with TiO2The titanium silk screen membrane of the nanotube array is prepared by the following method:
the pretreated titanium wire mesh is connected with an anode of direct current, a graphite plate is connected with a cathode of the direct current, and NH is added into the graphite plate4F, carrying out anodic oxidation reaction in electrolyte consisting of water and glycerol, and growing on a titanium wire mesh to obtain TiO2Cleaning and drying the nanotube array, and heating to 390-410 ℃ for heat treatment to obtain surface-coated TiO2Titanium silk net film of nanotube array.
Furthermore, the aperture of the titanium wire mesh is 95-100 meshes.
Further, the pretreatment is to sequentially perform deionized water cleaning, hydrofluoric acid solution soaking to remove oxides, deionized water cleaning and drying.
Further, the mass percentage of each component in the electrolyte is NH40.22-0.26% of F, 1-1.5% of water and 98.24-98.78% of glycerol.
Further, the voltage of direct current of the anodic oxidation reaction is 20-25V, and the reaction time is 1.8-2.2 h.
Further, the TiO2The tube diameter of the nanotube array is 80-100 nm.
Further, the heating rate of the heat treatment is 5-7 ℃/min; the heat treatment time is 3.8-4.1 h.
Silk screen type TiO2The method for degrading VOCs by the device for degrading VOCs by using the nanotube array photocatalysis comprises the following steps:
VOCs-containing gas passing through the wire mesh type TiO2The air inlet of the device for degrading VOCs by nanotube array photocatalysis enters the box body, and the contact surface is covered with TiO2TiO of nanotube array2The titanium silk net film is subjected to photocatalytic reaction under the action of an ultraviolet lamp to degrade VOCs, and degraded gas is discharged from an exhaust port.
Further, the VOCs refers to formaldehyde.
Preferably, the power of the ultraviolet lamp is 100-200W.
The principle of the device and the method of the invention is as follows: air enters the box body through the air inlet, and the contact surface is covered with TiO2TiO of nanotube array2The titanium silk net film is subjected to photocatalytic reaction under the action of an ultraviolet light source, and VOCs (volatile organic compounds), particularly formaldehyde, can be directly degraded without the assistance of a direct-current power supply.
The device and the method of the invention have the following advantages and beneficial effects:
(1) in the aspect of indoor VOCs degradation, the wire mesh type TiO2The nanotube array can rapidly filter gas, has the characteristic of large specific area, and can be used as an excellent catalytic material for degrading VOCs (volatile organic compounds) through photocatalysis;
(2) silk screen type TiO2Nanotube and method of manufacturing the sameThe array can be used as a novel core catalytic material of an air purifying agent, is applied to actual air purifying work, and effectively solves the problem that indoor formaldehyde harms human bodies;
(3) the device and the method of the invention have the advantages that the important active factors generated by photocatalysis are directly utilized to degrade VOCs without the assistance of a direct current power supply; meanwhile, the total energy consumption is basically from the ultraviolet lamp tube and the fan, and the overall energy consumption is low;
(4) silk screen type TiO used by the device2The nanotube array photocatalytic film is easy to prepare, can maintain performance for a long time, is convenient to replace, is green, safe and nontoxic, and has no pollution to the environment.
Drawings
FIG. 1 shows a mesh type TiO film according to an embodiment of the present invention2The structural schematic diagram of the device for degrading VOCs by the nanotube array photocatalysis;
FIG. 2 is a surface coated TiO of an example of the present invention2A real object diagram of a titanium silk net film of the nanotube array;
FIG. 3 is a scanning electron microscope image of an array of TiO2 nanotubes on a titanium silk screen film obtained in example 1 of the present invention;
FIG. 4 is a scanning electron microscope image of an array of TiO2 nanotubes on a titanium silk screen film obtained in example 2 of the present invention;
fig. 5 is a graph of the degradation rate of VOCs treated with the apparatus of example 1 of the present invention as a function of time.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
The structural schematic diagram of the device for photocatalytic degradation of VOCs by using the silk-screen TiO2 nanotube array of the present embodiment is shown in fig. 1. The air-conditioning box comprises a box body, wherein one end of the box body is provided with an air inlet, the other end of the box body is provided with an air outlet, and an exhaust fan is arranged in the air outlet; three layers of surface-covered TiO are fixedly arranged in the box body in the direction vertical to the air inlet and the air outlet2The titanium silk screen film of the nanotube array has no gap between the titanium silk screen film and the box body, and two adjacent titanium silk screen films are arrangedAn ultraviolet lamp is arranged between the titanium screen mesh films.
The titanium wire mesh film with the surface covered with the TiO2 nanotube array in the embodiment is prepared by the following method:
(1) pretreatment of a titanium wire mesh: using 100 mesh titanium mesh, cut into four pieces of 20 × 25 cm. Preparing 5L of hydrofluoric acid with the concentration of 0.5% in a self-made organic glass jar, putting a titanium wire mesh cleaned by deionized water into the organic glass jar until the titanium wire mesh is immersed for about 20s, immediately taking out the titanium wire mesh after a little bubble is observed to be generated, cleaning the titanium wire mesh by the deionized water, and finally drying.
(2) Anodic oxidation method for preparing TiO2Nanotube array: 4L of NH4F with the mass concentration of 0.25%, 1% of water and 98.75% of glycerol electrolyte are prepared in a self-made glass cylinder, then a graphite plate is placed in the middle of the glass cylinder, a titanium wire mesh subjected to pretreatment in the step (1) and 3cm away from the graphite plate is respectively placed on two sides of the graphite plate, the two titanium wire meshes are connected with an anode of 20V direct current, the graphite plate is connected with a cathode of 20V direct current, the titanium wire mesh is fixed and placed by an iron stand, and electrolysis is carried out for 2 hours. And after the electrolysis is finished, cleaning the titanium wire mesh with deionized water and waiting for the titanium wire mesh to be naturally dried (the nanotube on the titanium wire can not be easily damaged by wiping with external force). Drying, heating to 400 deg.C in muffle furnace at a temperature rise rate of 5 deg.C/min, and heating at 400 deg.C for 4 hr to obtain surface-coated TiO2Titanium silk net film of nanotube array.
Surface-coated TiO obtained in this example2A physical representation of the titanium silk mesh film of the nanotube array is shown in fig. 2. TiO on titanium silk screen film2A scanning electron micrograph of the nanotube array is shown in fig. 3.
The device of the embodiment is adopted to degrade VOCs, and comprises the following specific steps:
the synthetic glass simulation room is filled with mixed gas of nitrogen and formaldehyde with the concentration of 20mg/L and doped with formaldehyde, and then the mixed gas is put into the wire mesh type TiO of the embodiment2The device for degrading VOCs through nanotube array photocatalysis is characterized in that ultraviolet light is turned on for photocatalysis, the power of ultraviolet lamps is set to be 100W, 125W, 150W, 175W and 200W respectively, samples are taken once per hour to measure the degradation rate of VOCs, and the degradation rate is drawn to change along with timeThe results are shown in FIG. 5. As can be seen from the results in FIG. 5, the degradation rate reached 4% within 1 hour and 38% after 6 hours of reaction at an ultraviolet lamp power of 100W. When the power of the ultraviolet lamp is 125W, the degradation rate reaches 6% within 1 hour, and the degradation rate reaches 42% after 6 hours of reaction. When the power of the ultraviolet lamp is 150W, the degradation rate reaches 2% within 1 hour, and the degradation rate reaches 51% after 6 hours of reaction. When the power of the ultraviolet lamp is 175W, the degradation rate reaches 5% within 1 hour, and the degradation rate reaches 55% after 6 hours of reaction. When the power of the ultraviolet lamp is 200W, the degradation rate reaches 10% within 1 hour, and the degradation rate reaches 63% after 6 hours of reaction.
According to the results, the degradation efficiency of the device can be effectively improved by properly improving the power of the ultraviolet lamp under the same other degradation conditions, and the device has great superiority in effectively treating VOCs and can greatly improve the degradation rate and the degradation rate of organic matters.
Example 2
A mesh type TiO of this example2The structural schematic diagram of the device for degrading VOCs by using the nanotube array through photocatalysis is shown in figure 1. The air-conditioning box comprises a box body, wherein one end of the box body is provided with an air inlet, the other end of the box body is provided with an air outlet, and an exhaust fan is arranged in the air outlet; three layers of surface-covered TiO are fixedly arranged in the box body in the direction vertical to the air inlet and the air outlet2The titanium silk screen film of the nanotube array has no gap between the titanium silk screen film and the box body, and an ultraviolet lamp is arranged between two adjacent layers of the titanium silk screen films.
In this example, the surface was coated with TiO2The titanium silk screen membrane of the nanotube array is prepared by the following method:
(1) pretreatment of a titanium wire mesh: using 100 mesh titanium mesh, cut into four pieces of 20 × 25 cm. Preparing 5L of hydrofluoric acid with the concentration of 0.5% in a self-made organic glass jar, putting a titanium wire mesh cleaned by deionized water into the organic glass jar until the titanium wire mesh is immersed for about 20s, immediately taking out the titanium wire mesh after a little bubble is observed to be generated, cleaning the titanium wire mesh by the deionized water, and finally drying.
(2) Anodic oxidation method for preparing TiO2Nanotube array: 4L of mass concentration is arranged in a self-made glass cylinder0.26% NH4F, 1.2% of water and 98.54% of glycerol electrolyte, then placing a graphite plate in the middle of the glass cylinder, respectively placing a titanium wire mesh which is 3cm away from the graphite plate and is pretreated in the step (1) on two sides of the graphite plate, connecting the two titanium wire meshes with an anode of 20V direct current, connecting the graphite plate with a cathode of 20V direct current, fixing and placing the two titanium wire meshes with an iron support, and electrolyzing for 2 hours. And after the electrolysis is finished, cleaning the titanium wire mesh with deionized water and waiting for the titanium wire mesh to be naturally dried (the nanotube on the titanium wire can not be easily damaged by wiping with external force). Drying, heating to 400 deg.C in muffle furnace at a temperature rise rate of 5 deg.C/min, and heating at 400 deg.C for 4 hr to obtain surface-coated TiO2Titanium silk net film of nanotube array.
Surface-coated TiO obtained in this example2A physical representation of the titanium silk mesh film of the nanotube array is shown in fig. 2. TiO on titanium silk screen film2A scanning electron micrograph of the nanotube array is shown in fig. 4.
The device of the embodiment is adopted to degrade VOCs, and comprises the following specific steps: the synthetic glass simulation room is filled with mixed gas of nitrogen and formaldehyde with the concentration of 20mg/L and doped with formaldehyde, and then the mixed gas is put into the wire mesh type TiO of the embodiment2The device for degrading VOCs through the nanotube array photocatalysis is characterized in that ultraviolet light is turned on for photocatalysis, the power of an ultraviolet lamp is set to be 200W, a sample is taken once per hour to measure the degradation rate of VOCs, a graph of the degradation rate changing along with time is drawn, when the power of the ultraviolet lamp is 200W, the degradation rate reaches 11% within 1 hour, the degradation rate reaches 28% within 2 hours of reaction, and the degradation rate reaches 81% within 6 hours of reaction.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. Silk screen type TiO2The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: the device comprises a box body, wherein one end of the box body is provided with air inletThe other end of the port is provided with an exhaust port; multilayer surface-covering TiO is fixedly arranged in the box body in the direction vertical to the air inlet and the air outlet2The titanium silk screen film of the nanotube array has no gap between the titanium silk screen film and the box body, and an ultraviolet lamp is arranged between two adjacent layers of the titanium silk screen films.
2. The wire mesh type TiO of claim 12The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: an exhaust fan is arranged in the exhaust port.
3. The wire mesh type TiO of claim 12The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: the surface is covered with TiO2The titanium silk screen membrane of the nanotube array is prepared by the following method:
the pretreated titanium wire mesh is connected with an anode of direct current, a graphite plate is connected with a cathode of the direct current, and NH is added into the graphite plate4F, carrying out anodic oxidation reaction in electrolyte consisting of water and glycerol, and growing on a titanium wire mesh to obtain TiO2Cleaning and drying the nanotube array, and heating to 390-410 ℃ for heat treatment to obtain surface-coated TiO2Titanium silk net film of nanotube array.
4. The TiO of claim 3, in the form of a wire mesh2The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: the aperture of the titanium wire mesh is 95-100 meshes; the pretreatment is to sequentially carry out deionized water cleaning, hydrofluoric acid solution soaking to remove oxides, deionized water cleaning and drying.
5. The TiO of claim 3, in the form of a wire mesh2The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: the mass percentage of each component in the electrolyte is NH40.22-0.26% of F, 1-1.5% of water and 98.24-98.78% of glycerol.
6. The TiO of claim 3, in the form of a wire mesh2Nanotube and method of manufacturing the sameThe device of array photocatalytic degradation VOCs which characterized in that: the voltage of direct current of the anodic oxidation reaction is 20-25V, and the reaction time is 1.8-2.2 h; the TiO is2The tube diameter of the nanotube array is 80-100 nm.
7. The TiO of claim 3, in the form of a wire mesh2The device for degrading VOCs by the photocatalysis of the nanotube array is characterized in that: the heating rate of the heat treatment is 5-7 ℃/min; the heat treatment time is 3.8-4.1 h.
8. A method for degrading VOCs according to any of claims 1 to 7, comprising the steps of:
VOCs-containing gas passing through the wire mesh type TiO2The air inlet of the device for degrading VOCs by nanotube array photocatalysis enters the box body, and the contact surface is covered with TiO2TiO of nanotube array2The titanium silk net film is subjected to photocatalytic reaction under the action of an ultraviolet lamp to degrade VOCs, and degraded gas is discharged from an exhaust port.
9. The method of claim 8, wherein the apparatus degrades VOCs by: the VOCs refer to formaldehyde.
10. The method of claim 8, wherein the apparatus degrades VOCs by: the power of the ultraviolet lamp is 100-200W.
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