CN115739068A - Supported catalyst, preparation method thereof and photocatalytic treatment device using supported catalyst - Google Patents
Supported catalyst, preparation method thereof and photocatalytic treatment device using supported catalyst Download PDFInfo
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- CN115739068A CN115739068A CN202211443772.3A CN202211443772A CN115739068A CN 115739068 A CN115739068 A CN 115739068A CN 202211443772 A CN202211443772 A CN 202211443772A CN 115739068 A CN115739068 A CN 115739068A
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a supported catalyst, a preparation method thereof and a photocatalytic treatment device using the supported catalyst, wherein the supported catalyst comprises the following components in parts by weight: the supported catalyst comprises a titanium dioxide carrier with oxygen vacancies and rare earth element particles loaded on the titanium dioxide carrier, wherein the loading capacity of the rare earth element particles is 5-10%, the particle size of the rare earth element particles is 1-3nm, the raw materials of the supported catalyst are cheap and easy to obtain, the preparation process is simple, the effect is excellent, and the reaction time is obviously reduced; in addition, the invention provides a photocatalytic treatment device using the supported catalyst, which comprises a first reactor and a second reactor which are sequentially connected, wherein ultraviolet lamps are vertically arranged in the first reactor and the second reactor, the first reactor is connected with an ozone generator, and a supported catalyst filler made of the supported catalyst is arranged in the second reactor.
Description
Technical Field
The invention relates to the field of photocatalytic treatment, in particular to a supported catalyst, a preparation method thereof and a photocatalytic treatment device using the supported catalyst.
Background
The organic wastewater difficult to degrade has the characteristics of complex components, more toxic and harmful substances, great harm to the ecological environment and the like. The advanced oxidation technology has the advantages of high treatment rate, high degradation efficiency, wide application range and the like, and is one of the methods with the most application prospect for treating the organic wastewater difficult to degrade. Wherein, the waste water treatment tubular reactor based on ultraviolet photocatalysis is a device which is widely applied to degrade organic waste water.
Because the ultraviolet lamps in the existing ultraviolet light catalytic wastewater treatment tubular reactor are transversely arranged (namely the arrangement direction of the ultraviolet lamps is consistent with the extension direction of the length of the tubular body), the ultraviolet lamps are limited by the requirements of the size of the ultraviolet lamps and the turbulence degree, the single-section effective volume of the tubular reactor is small, and the sufficient treatment capacity can be achieved by adopting a mode of combining dozens of sections or even hundreds of sections and carrying out large-flow-rate circulating reaction. The multi-section combination can obviously increase the occupied area, a high-power flow pump is required for the circulating operation, and the energy loss is greatly increased. Meanwhile, the water flow direction is parallel to the ultraviolet lamp, so that turbulence is not easy to increase, and the ultraviolet lamp is not easy to disassemble, overhaul, clean and the like when being transversely placed.
In addition, the existing ultraviolet light catalysis wastewater treatment tubular reactor adopts a process of combining an ultraviolet light and an oxidant to degrade wastewater, but has the problem of low treatment efficiency.
Disclosure of Invention
The invention aims to provide a supported catalyst, a preparation method thereof and a photocatalytic treatment device using the supported catalyst.
In one embodiment, there is provided a supported catalyst comprising: the supported catalyst comprises a titanium dioxide carrier with oxygen vacancies and rare earth element particles loaded on the titanium dioxide carrier, wherein the loading capacity of the rare earth element particles is 5-10%, the particle size of the rare earth element particles is 1-3nm, the raw materials of the supported catalyst are cheap and easy to obtain, the preparation process is simple, the effect is excellent, and the reaction efficiency is remarkably improved.
In example two, it is provided that the rare earth element particles are lanthanide element particles, and the lanthanide element particles are supported on a titanium dioxide support having oxygen vacancies to produce the supported catalyst.
In a specific embodiment, the preparation method of the titanium dioxide carrier with oxygen vacancies comprises the following steps: with TiO 2 (B) Calcining the raw material at 500-800 ℃ for 3-6 h in an inert gas atmosphere to prepare the titanium dioxide carrier with the oxygen vacancy.
In one embodiment, the preparation of the supported catalyst comprises the steps of: (1) adding the titanium dioxide carrier with the oxygen vacancy into a rare earth element precursor aqueous solution, keeping the rotating speed to be more than 1000r/min, stirring the titanium dioxide carrier and the rare earth element precursor until the titanium dioxide carrier and the rare earth element precursor are uniformly mixed, fully adsorbing the rare earth element precursor in pores of the titanium dioxide carrier, and then heating and stirring at 70-80 ℃ until the mixture is dried to obtain a solid mixture, wherein the rare earth element precursor solution is rare earth element nitrate or sulfate; (2) and (3) placing the solid mixture obtained in the step (1) into a tubular furnace, and roasting in a reducing atmosphere at the roasting temperature of 400-600 ℃ so that the rare earth element precursor is reduced into rare earth element particles, thus obtaining the supported catalyst.
The third embodiment provides a photocatalytic treatment device using the supported catalyst, which comprises a first reactor and a second reactor which are sequentially connected, wherein ultraviolet lamps are vertically arranged in the first reactor and the second reactor, the first reactor is connected with an ozone generator, and a supported catalyst filler made of the supported catalyst is arranged in the second reactor. Through the reactor I, the ultraviolet light and the ozone are utilized for concerted catalysis, functional groups of macromolecular organic matters can be effectively destroyed to be changed into micromolecular organic matters, and meanwhile, partial TOC is removed; reactor II throughUltraviolet light and catalyst are used for concerted catalysis to further mineralize small molecular organic matters into CO 2 And H 2 O, two sections reaction synergy, improve the device to the degradation efficiency and the removing capacity of pollutant in the waste water, in addition, through the ultraviolet lamp of vertical placing, compare with tubular generator and increased the reactor size, reduced area, and it is convenient to dismantle, and the easy access is washd, and secondly, the rivers direction is perpendicular with the ultraviolet lamp, is favorable to increasing the torrent, reinforcing reaction rate and ozone utilization ratio.
In a specific embodiment, the first reactor and the second reactor are internally provided with S-shaped flow channels, the S-shaped flow channels are formed by welding straight plates and bent plates, the S-shaped flow channels can increase the reaction path and weaken the influence of a water hammer phenomenon on an ultraviolet lamp tube, the service life of an ultraviolet lamp sleeve is prolonged, and the maintenance frequency is reduced.
In a specific embodiment, a first filter screen and a second filter screen are welded at water inlets of the first reactor and the second reactor from outside to inside, the aperture of the first filter screen is larger than that of the second filter screen, and the first filter screen and the second filter screen can enable the flow rates of wastewater at different positions in the device to be basically consistent, so that the wastewater entering the device can reach the expected retention time.
In a specific embodiment, the first filter and the second filter are made of PTFE, which has good acid and corrosion resistance, and is low in purchase cost.
In a specific embodiment, the supported catalytic filler and the ultraviolet lamp are arranged at intervals, so that the wastewater can be fully and uniformly degraded, and the degradation effect is good.
In a specific embodiment, the ozone generator is connected with a gas flowmeter, the gas flowmeter is connected to a venturi tube through a gas guide hose, and the venturi tube is connected with the first reactor through an inlet valve.
Has the beneficial effects that:
1. the supported catalyst has the advantages of cheap and easily-obtained raw materials, simple preparation process, excellent effect and remarkably improved reaction efficiency.
2. By passingThe first reactor utilizes ultraviolet light and ozone for concerted catalysis, can effectively destroy functional groups of macromolecular organic matters to enable the macromolecular organic matters to become micromolecular organic matters, and meanwhile removes partial TOC, and the second reactor further enables the micromolecular organic matters to be mineralized into CO through concerted catalysis of the ultraviolet light and the catalyst 2 And H 2 O, two sections reaction synergy, improve the device to the degradation efficiency and the removing capacity of pollutant in the waste water, in addition, through the ultraviolet lamp of vertical placing, compare with tubular generator and increased the reactor size, reduced area, and it is convenient to dismantle, and the easy access is washd, and secondly, the rivers direction is perpendicular with the ultraviolet lamp, is favorable to increasing the torrent, reinforcing reaction rate and ozone utilization ratio.
Drawings
FIG. 1 is a schematic view showing the structure of a photocatalytic treatment apparatus according to a third embodiment;
FIG. 2 is a schematic view of the structure of the reactor II in the third example;
FIG. 3 is an SEM image of a supported catalyst;
fig. 4 is a TEM image of the supported catalyst.
Wherein: the device comprises a 1-ozone generator, a 2-gas flowmeter, a 3-gas guide hose, a 4-gas inlet, a 5-Venturi tube, a 6-inlet valve, a 7-first filter screen, a 8-second filter screen, a 9-sealing gasket, a 10-fixing screw, an 11-ultraviolet lamp, a 12-ultraviolet lamp sealing piece, a 14-reaction tank top cover, a 16-tank bottom groove, a 17-bottom emptying valve, an 18-outlet valve, a 19-pp pipeline, a 20-supported catalyst filler, a 21-tetrafluoro straight plate, a 22-tetrafluoro bent plate and a 23-S-shaped flow channel.
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 reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "center", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "counterclockwise", "clockwise", "axial", "radial", "circumferential", etc., indicate orientations and positional relationships based on those shown in the drawings, and are used merely for convenience of description and for 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 therefore, should not be considered as limiting the present invention. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; they may be mechanically or electrically connected, directly or indirectly through intervening media, or 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.
Example one
Referring to fig. 3 and 4, in this embodiment, a supported catalyst includes: the supported catalyst comprises a titanium dioxide carrier with oxygen vacancies and rare earth element particles loaded on the titanium dioxide carrier, wherein the loading amount of the rare earth element particles is 5-10%, the particle size of the rare earth element particles is 1-3nm, the raw materials of the supported catalyst are cheap and easy to obtain, the preparation process is simple, the effect is excellent, and the reaction efficiency is remarkably improved, wherein the rare earth element particles are preferably Pr or La particles.
Example two
In order to produce the supported catalyst mentioned in the examples, this example provides a production method in which the lanthanoid element particles are first used as the rare earth element particles, and the lanthanoid element particles are supported on a titania support having an oxygen vacancy to produce the supported catalyst.
Specifically, the preparation method of the titanium dioxide carrier with the oxygen vacancy comprises the following steps: and (3) calcining TiO2 (B) serving as a raw material at the temperature of 500-800 ℃ for 3-6 h in an inert gas atmosphere to prepare the titanium dioxide carrier with the oxygen vacancy, wherein the inert gas is preferably argon.
Further, the preparation of the supported catalyst comprises the following steps: (1) adding the titanium dioxide carrier with the oxygen vacancy into a rare earth element precursor aqueous solution, keeping the rotating speed to be more than 1000r/min, stirring the titanium dioxide carrier and the rare earth element precursor until the titanium dioxide carrier and the rare earth element precursor are uniformly mixed, fully adsorbing the rare earth element precursor in pores of the titanium dioxide carrier, and then heating and stirring at 70-80 ℃ until the mixture is dried to obtain a solid mixture, wherein the rare earth element precursor solution is rare earth element nitrate or sulfate, and preferably the rare earth element precursor solution is nitrate; (2) and (2) placing the solid mixture obtained in the step (1) into a tubular furnace, and roasting in a reducing atmosphere at the roasting temperature of 400-600 ℃ so that the rare earth element precursor is reduced into rare earth element particles, namely the supported catalyst is prepared, wherein the reducing gas is preferably hydrogen.
EXAMPLE III
Referring to fig. 1 and 2, the present embodiment provides a photocatalytic treatment apparatus using the supported catalyst, which includes a first reactor and a second reactor connected in sequence, wherein ultraviolet lamps 11 are vertically disposed in the first reactor and the second reactor, the first reactor is connected to an ozone generator 1, and a supported catalyst filler 20 made of a supported catalyst is disposed in the second reactor.
Thus, the first reactor can effectively destroy functional groups of macromolecular organic matters by utilizing the concerted catalysis of ultraviolet light and ozone, so that the macromolecular organic matters are changed into micromolecular organic matters, and meanwhile, partial TOC (total organic carbon) is removed; the second reactor further mineralizes the small molecular organic matters into CO through the concerted catalysis of ultraviolet light and a catalyst 2 And H 2 O, the two-stage reaction is synergistic, the degradation efficiency and the removal capacity of the device to pollutants in the wastewater are improved, and in addition, the reaction is increased compared with a tubular generator through the ultraviolet lamp 11 which is vertically arrangedThe ware size, reduced area, and dismantle the convenience, the easy access is washd, and secondly, rivers direction is perpendicular with ultraviolet lamp 11, is favorable to increasing the torrent, reinforcing reaction rate and ozone utilization ratio.
Wherein, a reactor and ozone generator 1's concrete connection does ozone generator 1 is connected with gas flowmeter 2, and gas flowmeter 2 is connected to venturi 5 through air guide hose 3, venturi 5 is connected with a reactor through inlet valve 6, and is same, and venturi 5, first filter screen 7 and second filter screen 8 are established equally in the import of No. two reactors, and the tail end of a reactor and No. two reactors all is connected with outlet valve 18.
Referring to fig. 1, it should be noted that, the connection mode of the ultraviolet lamp 11 and the first and second reactors is specifically that, the reaction tank top cover 14 is connected with the wall of the reaction tank through a screw in a sealing manner, a sealing gasket 9 is filled between the reaction tank top cover 14 and the wall of the reaction tank, and is fixed in a sealing manner by using a fixing screw 10, the reaction tank is provided with an outlet valve 18, the ultraviolet lamp 11 is inserted into the reaction tank through a screw hole reserved in the top cover, the top is connected with the reaction tank top cover 14 through an ultraviolet lamp sealing piece 12 in a sealing manner, and the bottom is embedded into a groove bottom 16 of the reaction tank for fixing, wherein, a sealing gasket is arranged between the reaction tank top cover 14 and the wall of the reaction tank, so as to avoid overflow of high-speed flowing waste water.
The wall of the reaction tank is made of a material which is resistant to acid, alkali, ultraviolet and has enough hardness, preferably, the wall of the reaction tank is made of a steel-lined tetrafluoro tank wall 15 made of steel-lined tetrafluoro, and in addition, the ultraviolet lamp 11 consists of a quartz sleeve and a light-emitting tube.
Referring to fig. 2, the first reactor and the second reactor are internally provided with an S-shaped flow passage 23, the S-shaped flow passage 23 is formed by welding a straight plate and a bent plate, the S-shaped flow passage 23 can increase a reaction path and weaken the influence of a water hammer phenomenon on the ultraviolet lamp 11 tube, prolong the service life of the ultraviolet lamp 11 sleeve and reduce the maintenance frequency.
The reactor I and the reactor II are welded with a first filter screen 7 and a second filter screen 8 at water inlets from outside to inside, the aperture of the first filter screen 7 is larger than that of the second filter screen 8, and the first filter screen 7 and the second filter screen 8 can enable the flow rates of wastewater at different positions in the device to be basically consistent, so that the wastewater entering the device can reach the expected retention time.
Specifically, the first filter 7 and the second filter 8 are made of PTFE, which has good acid resistance and corrosion resistance, and low purchase cost.
The supported catalytic filler 20 and the ultraviolet lamp 11 are arranged at intervals, so that the wastewater can be fully and uniformly degraded, and the degradation effect is good.
The following table compares experimental data for the inventive apparatus with the supported catalyst packing 20 and without the supported catalyst packing for the same other parameters.
The flow of the photocatalytic treatment device is further explained below, the ozone generator 1 is connected with the gas flowmeter 2, the flow of ozone is controlled by the gas flowmeter 2, the ozone is connected to the gas inlet 4 of the venturi tube 5 through the gas guide hose 3, the wastewater containing high-concentration ozone mixed by the venturi tube 5 is dispersed into fluid with uniform flow velocity by the first filter screen 7 and the second filter screen and flows into the first reactor, then flows through the S-shaped flow channel 23 formed by the tetrafluoro straight plate 21 and the tetrafluoro bent plate 22, oxidation reaction occurs under the action of the ultraviolet lamp 11, then enters the second reactor through the pp pipeline 19, mineralization reaction is performed under the action of ultraviolet light and a catalyst, and after the reaction is finished, the bottom vent valve 17 is opened to discharge the wastewater.
The tetrafluoro bent plate 22 is made of an acid-base-resistant and ultraviolet-resistant material, and preferably, the tetrafluoro bent plate 22 is made of PTFE.
In this example, the tetrafluoro bent plate 22 has a 1/4 arc shape, and the diameter thereof is equal to the width of the S-shaped flow path 23, and the width of the reaction channel not covered by the tetrafluoro straight plate 21 is equal to the width of the S-shaped flow path 23.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A supported catalyst, comprising: the titanium dioxide carrier with the oxygen vacancy and the rare earth element particles loaded on the titanium dioxide carrier are provided, the loading amount of the rare earth element particles is 5-10%, and the particle size of the rare earth element particles is 1-3nm.
2. A process for preparing a supported catalyst according to claim 1, characterized in that: the rare earth element particles adopt lanthanide element particles, and the lanthanide element particles are loaded on a titanium dioxide carrier with oxygen vacancies to prepare the supported catalyst.
3. A process for preparing a supported catalyst according to claim 2, wherein: the preparation method of the titanium dioxide carrier with the oxygen vacancy comprises the following steps: tiO2 (B) is used as a raw material and is calcined for 3 to 6 hours at the temperature of between 500 and 800 ℃ in an inert gas atmosphere to prepare the titanium dioxide carrier with the oxygen vacancy.
4. A process for preparing a supported catalyst according to claim 3, comprising the steps of:
(1) adding the titanium dioxide carrier with the oxygen vacancy into a rare earth element precursor aqueous solution, keeping the rotating speed to be more than 1000r/min, stirring the titanium dioxide carrier and the rare earth element precursor until the titanium dioxide carrier and the rare earth element precursor are uniformly mixed, fully adsorbing the rare earth element precursor in pores of the titanium dioxide carrier, and then heating and stirring at 70-80 ℃ until the mixture is dried to obtain a solid mixture, wherein the rare earth element precursor solution is rare earth element nitrate or sulfate.
(2) And (3) placing the solid mixture obtained in the step (1) into a tubular furnace, and roasting in a reducing atmosphere at the roasting temperature of 400-600 ℃ so that the rare earth element precursor is reduced into rare earth element particles, thus obtaining the supported catalyst.
5. A photocatalytic treatment apparatus using the supported catalyst according to claim 1, comprising a first reactor and a second reactor connected in series, wherein ultraviolet lamps are vertically arranged in the first reactor and the second reactor, the first reactor is connected with an ozone generator, and a supported catalyst filler made of a supported catalyst is arranged in the second reactor.
6. A photocatalytic treatment apparatus as set forth in claim 5, characterized in that: the reactor I and the reactor II are internally provided with an S-shaped flow channel, and the S-shaped flow channel is formed by welding a straight plate and a bent plate.
7. A photocatalytic treatment apparatus as set forth in claim 6, characterized in that: the reactor I and the reactor II have a water inlet welded with a first filter screen and a second filter screen from outside to inside, and the aperture of the first filter screen is larger than that of the second filter screen.
8. A photocatalytic treatment apparatus as set forth in claim 7, characterized in that: the first filter screen and the second filter screen are made of PTFE materials.
9. A photocatalytic treatment apparatus as set forth in claim 5, characterized in that: the supported catalytic filler and the ultraviolet lamp are arranged at intervals.
10. A photocatalytic treatment apparatus as set forth in claim 5 wherein: the ozone generator is connected with a gas flowmeter, the gas flowmeter is connected to a Venturi tube through a gas guide hose, and the Venturi tube is connected with the first reactor through an inlet valve.
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| KR20220048338A (en) * | 2020-10-12 | 2022-04-19 | 김여일 | Air sterilization and purification device with photocatalyst plate modules arranged in zigzag form |
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2022
- 2022-11-18 CN CN202211443772.3A patent/CN115739068A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105381797A (en) * | 2015-10-16 | 2016-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of catalytic ozonation supported catalyst used for treating sewage and doped with dual rare earth elements |
| CN111068669A (en) * | 2020-01-14 | 2020-04-28 | 浙江工业大学 | Heterogeneous catalyst for selective hydrogenation reaction of quinoline compounds and application thereof |
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