CN114853112B - Application of titanium dioxide nano-catalyst in removing nitrate nitrogen in water body through photocatalysis - Google Patents

Application of titanium dioxide nano-catalyst in removing nitrate nitrogen in water body through photocatalysis Download PDF

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CN114853112B
CN114853112B CN202210282530.4A CN202210282530A CN114853112B CN 114853112 B CN114853112 B CN 114853112B CN 202210282530 A CN202210282530 A CN 202210282530A CN 114853112 B CN114853112 B CN 114853112B
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titanium dioxide
nitrate nitrogen
nitrogen
dioxide nano
water body
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CN114853112A (en
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叶正芳
秦疆洲
刘能胜
赵泉林
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Peking University
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    • 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
    • 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
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/16—Nitrogen compounds, e.g. ammonia
    • C02F2101/163—Nitrates
    • 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
    • C02F2305/08—Nanoparticles or nanotubes
    • 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
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)

Abstract

The application relates to the technical field of environmental functional materials, and discloses application of a titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis. The titanium dioxide nano catalyst can be used for efficiently degrading nitrate nitrogen, and finally, nitrite nitrogen accumulation is avoided, so that the harm to organisms and human bodies after water body discharge can be reduced.

Description

Application of titanium dioxide nano-catalyst in removing nitrate nitrogen in water body through photocatalysis
Technical Field
The application relates to the technical field of environmental functional materials, in particular to application of a titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis.
Background
The nitrogen cycle is the most basic element cycle in the biosphere, in which nitrate nitrogen (NO 3 - ) Nitrite Nitrogen (NO) 2 - ) And ammonium Nitrogen (NH) 4 + ) Is the main nitrogen-containing species that maintains a delicate nitrogen balance. However, this balance is broken due to human intervention, including the use of agrochemicals, urban surface rain runoff and the discharge of industrial or process wastewater, resulting in nitrate pollution of surface and ground water. To prevent excessive discharge of nitrate from causing drinking water safety and public health problems, for example: water eutrophication and serious human diseases ("blue infant" syndrome, etc.), world health organization (World Health Organization, WHO) limits the highest concentration of acceptable nitrate in drinking water to 10mg/L. Therefore, many restoration methods such as reverse osmosis, ion exchange, electrodialysis, catalytic denitrification and biochemical techniques have been used to remove nitrate. There are also some unavoidable drawbacks, however, that biological denitrification is a mature and cost-effective technique, but requires a high carbon-nitrogen ratioThe proper pH and temperature can successfully enrich denitrifying bacteria, so that the denitrifying bacteria are not applicable to groundwater and industrial wastewater, and the biodegradable organic matters are limited. As for physical removal methods such as reverse osmosis and ion exchange, they are concerned with substitution rather than elimination, and thus the resulting brine containing secondary nitrate needs to be post-treated and increases costs. Catalytic denitration technology has high reaction speed and does not need organic carbon, but depends on the large use of hydrogen or Fe 0 As a reducing agent, thus causing safety hazards during storage, transportation and use. Therefore, the search for a green and economical nitrate reduction process has become an environmental field leading research topic.
Titanium dioxide (TiO) 2 ) The photoelectrode can photoelectrocatalyze under the irradiation of ultraviolet light, and the phenomenon of decomposing water into hydrogen and oxygen is a phenomenon that semiconductor photocatalysis technology has attracted a great deal of attention. The photocatalytic reduction method for removing nitrate is a novel denitrification method which has been rising for the last thirty years, and has wide application prospect in the aspect of nitrate removal. Compared with the ion exchange method, the photocatalysis reduction method can thoroughly remove nitrate from water; compared with Fe 0 Reduction method, photocatalytic reduction method has higher N pair 2 Selectivity of (2); compared with the catalytic reduction method, the reaction process is safer; compared with biological denitrification, the operation is not affected by carbon nitrogen ratio, pH value and reaction temperature. This process is advantageous from an environmental point of view for converting nitrate to harmless nitrogen.
However, the existing nano titanium dioxide-based photocatalytic reduction nitrate nitrogen removal technology generally needs to be doped with other metal elements, so that the synthesis cost is greatly increased, and the nitrate degradation performance and nitrogen selectivity are required to be improved.
Disclosure of Invention
In order to solve the defects in the prior art, the application aims to provide the application of the titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis, and the nitrate nitrogen in water body can be degraded more efficiently.
The application provides an application of a titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis.
Preferably, 100mL of a nitrate nitrogen solution with a concentration of 50mg/L and 100-500 mu L of formic acid are mixed, 10mg of titanium dioxide nano catalyst is added into the mixed solution, and then the mixed solution is stirred and then is placed under simulated sunlight for irradiation for 4 hours.
Preferably, nitrogen is introduced into the reaction solution to be aerated for 10 minutes before being exposed to the simulated sunlight.
Preferably, the nitrogen gas is introduced in an amount of 10 to 20mL/min, and the purity of the nitrogen gas is 90% or more.
Preferably, the light-emitting spectrum range of the simulated sunlight is 300-1100 nm, and the illumination intensity of the light source is 8000-10000 lux.
Preferably, the preparation method of the titanium dioxide nano catalyst comprises the following steps:
2mL TiCl was taken 4 Putting into 30mL of ethylene glycol, stirring for 30min at room temperature, then adding 2mL of deionized water, and continuing stirring to obtain a mixed solution;
placing the mixed solution into a stainless steel high-pressure reaction kettle, and heating for 4 hours at 150 ℃;
and (3) washing the heated product with deionized water and ethanol for 4-5 times, and vacuum drying at 45-75 ℃ for 8-16 h.
Preferably, the preparation method of the titanium dioxide nano catalyst further comprises calcining the obtained product after vacuum drying at a high temperature of 0-800 ℃ for 2 hours.
Preferably, the calcination temperature is 500 ℃ and the temperature rising rate is 10 ℃/min.
Preferably, in the preparation method of the titanium dioxide nano catalyst, stirring is continuously performed until no hydrogen chloride gas is generated before the mixed solution is obtained, and the mixed solution is in a uniform white emulsion.
Preferably, the washing of the heated product with deionized water and ethanol for 4-5 times comprises:
centrifuging the heated product to obtain solid;
adding deionized water or ethanol, centrifuging for several times, and removing supernatant.
Compared with the existing nano titanium dioxide-based photocatalytic reduction technology for removing nitrate nitrogen, the method has the advantages that: (1) any metal element does not need to be doped, so that the synthesis cost is greatly reduced; (2) the simulated sunlight is adopted to avoid ultraviolet light or a high-pressure mercury lamp, so that the energy is saved, and the degradation performance in a natural environment is simulated more truly; (3) the performance of degrading nitrate is more efficient, the nitrogen selectivity reaches 100%, so that the low-concentration nitrate nitrogen wastewater (initial NO 3 - -N concentration below 50 mg/L) of NO 3 - N is reduced to below 3mg/L in 3h and is almost completely removed, and finally nitrite nitrogen is not accumulated, so that the harm to organisms and human bodies after water body discharge can be reduced.
Drawings
FIG. 1 is a TiO according to an embodiment of the present application 2 X-ray diffraction pattern (XRD) of the nanocatalyst;
FIG. 2 is a TiO according to an embodiment of the present application 2 Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) of the nanocatalyst (TO-500);
FIG. 3 is a TiO according to an embodiment of the present application 2 Ultraviolet-visible light absorption spectrum (DRS) of the nanocatalyst;
FIG. 4 shows TiO according to an embodiment of the application 2 Performance diagram of photocatalyst for photocatalytic degradation of nitrate nitrogen.
Detailed Description
The application is further described below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present application, and are not intended to limit the scope of the present application.
Example 1
2mL TiCl was taken 4 Adding 30mL of ethylene glycol, stirring at room temperature for 30min, adding 2mL of deionized water, stirring for 30min until no hydrogen chloride gas is generated, adding the mixed solution into a stainless steel high-pressure reaction kettle, and stirring at 150deg.CHeating for 4h, centrifuging to obtain solid, washing with deionized water and ethanol for several times, and vacuum drying at 60deg.C for 12h to obtain TiO 2 Nanocatalyst (TO).
And TO is used as a catalyst TO photo-catalytically degrade nitrate nitrogen. Weighing 10mg of TO nano catalyst, placing into a quartz container, and adding 100mL of NO with the concentration of 50mg/L 3 - Stirring the N solution and 100 mu L of formic acid, introducing nitrogen into the quartz container, aerating for 10min, wherein the nitrogen introducing amount is 10mL/min, the purity of the nitrogen is 90%, and then, putting the quartz container under simulated sunlight for irradiation for 4h, wherein the degradation effect of nitrate nitrogen is shown in figure 4, the degradation rate of nitrate nitrogen reaches 10%, and no ammonia nitrogen and nitrite nitrogen are generated.
Example 2
2mL TiCl was taken 4 Adding 30mL of ethylene glycol, stirring at room temperature for 30min, adding 2mL of deionized water, continuously stirring for 30min until no hydrogen chloride gas is generated, heating the mixed solution in a stainless steel high-pressure reaction kettle at 150 ℃ for 4h, centrifugally separating out solid, washing with deionized water and ethanol for multiple times, vacuum drying at 60 ℃ for 12h, and heating the vacuum dried mixture to 500 ℃ at a speed of 10 ℃/min for calcining for 2h to obtain TiO 2 Nanocatalyst (TO-500).
TO-500 is used as a catalyst for photocatalytic degradation of nitrate nitrogen. Weighing 10mg of TO-500 nm catalyst, placing into a quartz container, and adding 100mL of 50mg/L NO 3 - Stirring the N solution and 100 mu L of formic acid, introducing nitrogen into the quartz container, aerating for 10min, wherein the nitrogen introducing amount is 10mL/min, the purity of the nitrogen is 90%, and then, putting the quartz container under simulated sunlight for irradiation for 4 hours, wherein the degradation effect of nitrate nitrogen is shown in figure 4, the degradation rate of nitrate nitrogen reaches 99.5%, and no ammonia nitrogen and nitrite nitrogen are generated.
Example 3
2mL TiCl was taken 4 Adding 30mL of ethylene glycol, stirring at room temperature for 30min, adding 2mL of deionized water, stirring for 30min until no hydrogen chloride gas is generated, adding the mixed solution into a stainless steel high-pressure reaction kettle, heating at 150deg.C for 4 hr, and stirring for 30minAfter centrifugal separation to obtain solid, washing the solid for multiple times by deionized water and ethanol, vacuum drying the solid for 12 hours at 60 ℃, heating the mixture after vacuum drying to 800 ℃ at a speed of 10 ℃/min, and calcining the mixture for 2 hours to obtain TiO 2 Nanocatalyst (TO-800).
TO-800 is used as a catalyst TO photo-catalyze and degrade nitrate nitrogen. Weighing 10mg TO-800 nanometer catalyst, placing into a quartz container, adding 100mL 50mg/L NO 3 - Stirring the N solution and 100 mu L of formic acid, introducing nitrogen into the quartz container, aerating for 10min, wherein the nitrogen introducing amount is 10mL/min, the purity of the nitrogen is 90%, and then, putting the quartz container under simulated sunlight for irradiation for 4h, wherein the degradation effect of nitrate nitrogen is shown in figure 4, the degradation rate of nitrate nitrogen reaches 30%, and no ammonia nitrogen and nitrite nitrogen are generated.
Analysis of the structure and application of the titanium dioxide nanocatalyst prepared in the examples:
from fig. 1, it can be seen that TiO corresponding to the anatase phase at 25.3 °,37.7 °,48.0 °,53.8 ° and 51.0 ° 2 Five crystal planes (101), (004), (200), (105), (211), and in addition, at 27.4 °,36.0 °,39.2 °,41.2 °, tiO corresponding to the rutile phase 2 (110), (101), (111), (210). TiO not calcined at high temperature in example 1 2 The nanocatalyst (TO) did not have a distinct characteristic peak, indicating TO as amorphous particles, example 2 was a TiO calcined at 500℃ 2 Nanocatalyst (TO-500) has a typical anatase phase of TiO 2 Lattice, TO-500 is described as anatase TiO 2 TiO calcined at 800℃in example 3 2 Nanocatalyst (TO-800) with both anatase and rutile phases of TiO 2 Lattice composition, TO-800, is a mixed crystal of anatase and rutile phases.
The synthetic TiO can be seen in FIG. 2 2 The nano catalyst has the particle size of about 10nm and obvious anatase phase TiO 2 Lattice spacing.
As can be seen from FIG. 3, TO-500 and TO-800 all have significant absorption peaks at 300nm, indicating synthesized TiO 2 The nanocatalyst can have a photoresponsive capability at 300-400nm, furthermoreThe TO-500 absorption peak is the widest, which indicates that the absorption capacity of the TO-500 is the greatest, and the TO-500 has the best light energy utilization rate.
FIG. 4 shows different TiO 2 As can be seen from the time-dependent change curve of the performance of the nano catalyst in degrading nitrate nitrogen, TO-500 has the best performance in degrading nitrate nitrogen, after 3 hours of reaction, nitrate nitrogen can be reduced from 50mg/L TO 3mg/L, ammonia nitrogen and nitrite nitrogen are not generated, and TO degradation performance is the worst.
The application has the beneficial effects that compared with the prior art: (1) any metal element does not need to be doped, so that the synthesis cost is greatly reduced; (2) the simulated sunlight is adopted to avoid ultraviolet light or a high-pressure mercury lamp, so that the energy is saved, and the degradation performance in a natural environment is simulated more truly; (3) the performance of degrading nitrate is more efficient, the nitrogen selectivity reaches 100%, so that the low-concentration nitrate nitrogen wastewater (initial NO 3 - -N concentration below 50 mg/L) of NO 3 - N is reduced to below 3mg/L in 3h and is almost completely removed, and finally nitrite nitrogen is not accumulated, so that the harm to organisms and human bodies after water body discharge can be reduced.
While the applicant has described and illustrated the embodiments of the present application in detail with reference to the drawings, it should be understood by those skilled in the art that the above embodiments are only preferred embodiments of the present application, and the detailed description is only for the purpose of helping the reader to better understand the spirit of the present application, and not to limit the scope of the present application, but any improvements or modifications based on the spirit of the present application should fall within the scope of the present application.

Claims (7)

1. The application of the titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis is characterized in that the titanium dioxide nano catalyst is adopted, nitrate nitrogen aqueous solution is used as raw material, and photocatalysis reaction is carried out under simulated sunlight irradiation to remove nitrate nitrogen in water body; the preparation method of the titanium dioxide nano catalyst comprises the following steps:
taking 2mLTiCl 4 Put into 30mL of ethylene glycol and stirred at room temperature for 30min, then 2mL was addedDeionized water, and continuing stirring to obtain a mixed solution;
placing the mixed solution into a stainless steel high-pressure reaction kettle, and heating for 4 hours at 150 ℃;
washing the heated product with deionized water and ethanol for 4-5 times, and vacuum drying at 45-75 deg.c for 8-16 hr;
calcining the obtained product after vacuum drying at a high temperature of 500 ℃ for 2 hours; the calcining temperature is 500 ℃, and the heating rate is 10 ℃/min.
2. The application of the titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis according to claim 1, which is characterized in that 100mL of 50mg/L nitrate nitrogen solution and 100-500 mu L formic acid are mixed, 10mg of titanium dioxide nano catalyst is added into the mixed solution, and then the mixed solution is stirred and then is placed under simulated sunlight for irradiation for 4 hours.
3. The use of a titanium dioxide nano-catalyst according to claim 2 for removing nitrate nitrogen in water body by photocatalysis, wherein nitrogen is introduced into the reaction solution for aeration for 10min before the reaction solution is irradiated under simulated sunlight.
4. The application of the titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis according to claim 3, wherein the introducing amount of nitrogen is 10-20 mL/min, and the purity of the nitrogen is more than 90%.
5. The application of the titanium dioxide nano catalyst in the photocatalytic removal of nitrate nitrogen in water body according to claim 2, wherein the light-emitting spectrum range of the simulated sunlight is 300-1100 nm, and the illumination intensity of the light source is 8000-10000 lux.
6. The use of a titanium dioxide nanocatalyst according to claim 1 for photocatalytic removal of nitrate nitrogen from water, wherein in the preparation of the titanium dioxide nanocatalyst, stirring is continued until no hydrogen chloride gas is formed before a mixed solution is obtained, said mixed solution being in the form of a uniform white emulsion.
7. The application of the titanium dioxide nano catalyst in removing nitrate nitrogen in water body by photocatalysis according to claim 1, which is characterized in that the heated product is washed by deionized water and ethanol for 4-5 times, and the application comprises the following steps:
centrifuging the heated product to obtain solid;
adding deionized water or ethanol, centrifuging for several times, and removing supernatant.
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