CN108975504B - Method for simultaneously removing nitrite and ammonia nitrogen by copper bismuthate-fullerene photocatalyst - Google Patents
Method for simultaneously removing nitrite and ammonia nitrogen by copper bismuthate-fullerene photocatalyst Download PDFInfo
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- CN108975504B CN108975504B CN201810855410.2A CN201810855410A CN108975504B CN 108975504 B CN108975504 B CN 108975504B CN 201810855410 A CN201810855410 A CN 201810855410A CN 108975504 B CN108975504 B CN 108975504B
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- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000010949 copper Substances 0.000 title claims abstract description 79
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 79
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 78
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 62
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000010865 sewage Substances 0.000 claims abstract description 32
- 230000001678 irradiating effect Effects 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 claims description 23
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 150000001621 bismuth Chemical class 0.000 claims description 10
- 150000001879 copper Chemical class 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical group [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical group Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
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- 238000006243 chemical reaction Methods 0.000 description 23
- 239000000243 solution Substances 0.000 description 21
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 20
- 239000002131 composite material Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 13
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- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000012295 chemical reaction liquid Substances 0.000 description 6
- 244000005700 microbiome Species 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000013048 microbiological method Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 3
- 229940124530 sulfonamide Drugs 0.000 description 3
- NULAJYZBOLVQPQ-UHFFFAOYSA-N N-(1-naphthyl)ethylenediamine Chemical compound C1=CC=C2C(NCCN)=CC=CC2=C1 NULAJYZBOLVQPQ-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
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- 229910052742 iron Inorganic materials 0.000 description 2
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 2
- WZRRZVUZWWMSKH-UHFFFAOYSA-N n'-naphthalen-1-ylethane-1,2-diamine;hydrochloride Chemical compound Cl.C1=CC=C2C(NCCN)=CC=CC2=C1 WZRRZVUZWWMSKH-UHFFFAOYSA-N 0.000 description 2
- 125000001477 organic nitrogen group Chemical group 0.000 description 2
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- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 206010017993 Gastrointestinal neoplasms Diseases 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 108010061951 Methemoglobin Proteins 0.000 description 1
- 241000108664 Nitrobacteria Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 244000088401 Pyrus pyrifolia Species 0.000 description 1
- 235000001630 Pyrus pyrifolia var culta Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 210000003743 erythrocyte Anatomy 0.000 description 1
- HCFPRFJJTHMING-UHFFFAOYSA-N ethane-1,2-diamine;hydron;chloride Chemical compound [Cl-].NCC[NH3+] HCFPRFJJTHMING-UHFFFAOYSA-N 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 229960003671 mercuric iodide Drugs 0.000 description 1
- YFDLHELOZYVNJE-UHFFFAOYSA-L mercury diiodide Chemical compound I[Hg]I YFDLHELOZYVNJE-UHFFFAOYSA-L 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 nitrite ions Chemical class 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- HELHAJAZNSDZJO-UHFFFAOYSA-L sodium tartrate Chemical compound [Na+].[Na+].[O-]C(=O)C(O)C(O)C([O-])=O HELHAJAZNSDZJO-UHFFFAOYSA-L 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
- C02F3/301—Aerobic and anaerobic treatment in the same reactor
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2101/166—Nitrites
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for simultaneously removing nitrite and ammonia nitrogen by using a copper bismuthate-fullerene photocatalyst. The method comprises the following steps: adding a copper bismuthate-fullerene photocatalyst into sewage containing nitrite and ammonia nitrogen, introducing nitrogen, and irradiating the obtained mixed system with ultraviolet visible light so as to simultaneously remove the nitrite and the ammonia nitrogen; then air is introduced, and the mixed system is continuously irradiated by ultraviolet and visible light to realize thorough denitrification. The invention creatively integrates the nitrite removal and the ammonia nitrogen removal into a whole, simultaneously removes the nitrite and the ammonia nitrogen under the radiation of sunlight, changes the traditional process flow of denitrification and nitrite removal, shortens the working condition time, reduces the time cost, saves the economic cost and has high removal rate.
Description
Technical Field
The invention relates to a sewage treatment method, in particular to a method for simultaneously removing nitrite and ammonia nitrogen by adopting copper bismuthate-fullerene photocatalyst through photocatalysis, belonging to the technical field of photocatalysis.
Background
The main existing forms of nitrogen in water bodies are organic nitrogen and inorganic nitrogen. Organic nitrogen is converted into inorganic nitrogen under the action of microorganisms. Therefore, the method for removing inorganic nitrogen in the water body has important application value for sewage treatment. The inorganic nitrogen mainly comprises ammonia Nitrogen (NH)3-N), nitrate Nitrogen (NO)3 --N) and nitrous Nitrogen (NO)2 --N) three existing forms.
Due to excessive use of agricultural chemical fertilizer and large amount of discharge of industrial sewage and domestic sewageIn the release, the ammonia nitrogen often exceeds the standard. Under the aerobic condition of ammonia nitrogen, nitrosobacteria can convert the ammonia nitrogen into Nitrite (NO)2 -) Further oxidizable to Nitrate (NO)3 -). The content of ammonia nitrogen in the water body is often larger, and the toxicity of nitrite is one of the three forms with the highest toxicity. Nitrite is combined with hemoglobin to form methemoglobin in vivo, and the oxygen carrying capacity of erythrocytes is reduced. Furthermore, nitrite and nitrate can be converted into nitrosamine in human body, which can cause various diseases such as gastrointestinal cancer, leukemia, hypertension, etc. Therefore, how to reduce nitrite and ammonia nitrogen in water is an important subject in front of researchers in the field.
The prior art always treats nitrite and ammonia nitrogen respectively. For example, the Chinese patent with the patent application number of CN99100739.5 eliminates the pollution problem of nitrite in drinking water by a biological method; chinese patent with patent application number CN200510112131.X discloses a microbial nitrite degradation agent and a preparation method thereof; chinese patent application No. CN200610023388.2 describes a method for denitrifying nitrite using granular sludge. These methods are all microbiological methods. In the chemical method, the Chinese patent with the patent application number of CN200710144384.4 realizes the denitrification of the high-concentration nitrite wastewater by adopting a microwave-assisted treatment method; in Chinese patent with the patent application number of CN200910060734.8, the degradation of nitrite in water in aquaculture is realized by taking sulfamic acid as a reagent; redditional Red et al (Redditional Red, Yanfan, in Ben. sulfite removes nitrite from wastewater of nitroxide, chemical world, 2000, 11: 575-. The Chinese patent 'catalytic iron and biological coupling short-cut denitrification process' (patent application number: CN201510187814.5) takes iron as a reducing agent to realize sewage denitrification. The utility model with the patent number of CN201620767248.5 discloses a circulating water denitrification device in an ozone method flue gas desulfurization and denitrification purification system. Chinese patent CN201010603906.4 discloses a technical process for denitration by using sulfite and nitrite reaction. Although these documents disclose methods for removing nitrite ions (nitrite), they do not relate to methods for simultaneously removing ammonia nitrogen.
In the aspect of ammonia nitrogen removal, the denitrification method comprises a microbiological method and a physicochemical method. The microbiological method is that ammonia nitrogen is firstly converted into nitrite and nitrate by nitrobacteria, and then the nitrate and nitrite are converted into nitrogen by denitrifying bacteria to be discharged. Patents with application numbers of CN201611242635.8, CN201611242599.5, CN201610632670.4, CN201610632620.6, CN201610632354.7, CN201610632666.8, CN201610633033.9, CN201510007561.9 and the like respectively disclose a method for removing ammonia nitrogen by photocatalysis. However, these methods do not involve a technique for simultaneous removal of nitrite and ammonia nitrogen.
Biological denitrification has many defects, the growth environment and conditions of microorganisms must be strictly controlled, carbon sources must be artificially added, and the denitrification efficiency is easily influenced by seasons, weather and temperature. The activity of the microorganisms is significantly reduced or even inactivated at low temperatures, and the microorganisms may be "burned" at high temperatures.
Disclosure of Invention
In order to overcome the above-mentioned existing disadvantages, we propose the following invention.
The invention aims to provide a method for simultaneously removing nitrite and ammonia nitrogen by using a copper bismuthate-fullerene photocatalyst so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for simultaneously removing nitrite and ammonia nitrogen by using a copper bismuthate-fullerene photocatalyst, which comprises the following steps:
adding a copper bismuthate-fullerene photocatalyst into sewage containing nitrite and ammonia nitrogen, and irradiating a mixed system of the nitrite and the ammonia nitrogen by ultraviolet and visible light under anaerobic conditions and aerobic conditions, thereby removing the nitrite and the ammonia nitrogen simultaneously.
Further, the method comprises: and adjusting the mixed system to be alkaline, introducing nitrogen, and irradiating the mixed system by ultraviolet visible light to simultaneously remove nitrite and ammonia nitrogen in the sewage.
Further, the method further comprises: and after the step of irradiating the mixed system with ultraviolet visible light under the nitrogen condition is completed, introducing air into the mixed system, and irradiating the mixed system with ultraviolet visible light to realize the complete removal of nitrite and ammonia nitrogen in sewage.
The embodiment of the invention also provides a method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst, which comprises the following steps: oxidizing or biologically treating the sewage containing ammonia nitrogen to convert part of the ammonia nitrogen into nitrite nitrogen, adding a copper bismuthate-fullerene photocatalyst, introducing nitrogen to remove oxygen to create anaerobic conditions, and irradiating the obtained mixed system with ultraviolet and visible light to simultaneously remove nitrite and ammonia nitrogen.
The embodiment of the invention also provides a method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst, which comprises the following steps: mixing sewage containing ammonia nitrogen and sewage containing nitrite, adding a copper bismuthate-fullerene photocatalyst, introducing nitrogen to remove oxygen to create anaerobic conditions, and irradiating the obtained mixed system with ultraviolet visible light to simultaneously remove the nitrite and the ammonia nitrogen.
In some exemplary embodiments, the method comprises: and adjusting the mixed system to be alkaline, and irradiating the mixed system by ultraviolet visible light to remove nitrite and ammonia nitrogen in the sewage at the same time.
Further, the method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst comprises the following steps: adding a copper bismuthate-fullerene photocatalyst into sewage containing nitrite and ammonia nitrogen, introducing nitrogen, deoxidizing, irradiating with ultraviolet and visible light to obtain a mixed system, oxygenating the mixed system, and irradiating with ultraviolet and visible light to completely degrade the ammonia nitrogen in the water into N2Thereby simultaneously removing nitrite and ammonia nitrogen.
Compared with the prior art, the method creatively integrates the nitrite removal and the ammonia nitrogen removal, simultaneously removes the nitrite and the ammonia nitrogen under the radiation of sunlight, changes the technological process of the nitrite removal and the traditional denitrification, shortens the working condition time, reduces the time cost, saves the economic cost, has high removal rate, and has obvious technical progress compared with the prior art; the preparation method of the copper bismuthate-fullerene photocatalyst adopted by the invention is simple, the raw materials are low in price, and the conditions are easy to control.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a reaction apparatus for preparing a copper bismuthate-fullerene photocatalyst in example 1 of the present invention.
FIG. 2 is an XRD diffraction pattern of fullerene, copper bismuthate and copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention.
Fig. 3 is a raman spectrum of a fullerene, copper bismuthate, or copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention.
FIGS. 4a to 4d are TEM images of fullerene, copper bismuthate-fullerene composite semiconductor material, copper bismuthate, and copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention, respectively.
Fig. 5 is an ultraviolet-visible diffuse reflectance spectrum of the copper bismuthate and copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention.
Fig. 6 is a schematic diagram showing a variation curve of nitrite nitrogen and ammonia nitrogen in the reaction process of the copper bismuthate-fullerene composite semiconductor material in embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
One aspect of the embodiments of the present invention provides a method for simultaneously removing nitrite and ammonia nitrogen by using a copper bismuthate-fullerene photocatalyst, which comprises: adding a copper bismuthate-fullerene photocatalyst into sewage containing nitrite and ammonia nitrogen, and irradiating a mixed system of the nitrite and the ammonia nitrogen by ultraviolet and visible light under anaerobic conditions and aerobic conditions, thereby removing the nitrite and the ammonia nitrogen simultaneously.
In some exemplary embodiments, the method comprises: and adjusting the mixed system to be alkaline, introducing nitrogen, and irradiating the mixed system by ultraviolet visible light to simultaneously remove nitrite and ammonia nitrogen in the sewage.
Further, the pH value of the mixed system is 9.0-10.5.
Further, the method further comprises: and after the step of irradiating the mixed system with ultraviolet visible light under the nitrogen condition is completed, introducing air into the mixed system, and irradiating the mixed system with ultraviolet visible light to realize the complete removal of nitrite and ammonia nitrogen in sewage.
The embodiment of the invention also provides a method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst, which comprises the following steps: oxidizing or biologically treating the sewage containing ammonia nitrogen to convert part of the ammonia nitrogen into nitrite nitrogen, adding a copper bismuthate-fullerene photocatalyst, introducing nitrogen to remove oxygen to create anaerobic conditions (or respectively under the anaerobic and aerobic conditions), and irradiating the obtained mixed system with ultraviolet visible light to simultaneously remove nitrite and ammonia nitrogen.
In some exemplary embodiments, the method comprises: and adjusting the mixed system to be alkaline, and irradiating the mixed system by ultraviolet visible light to remove nitrite and ammonia nitrogen in the sewage at the same time.
Further, the pH value of the mixed system is 9.0-10.5.
The embodiment of the invention also provides a method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst, which comprises the following steps: mixing sewage containing ammonia nitrogen and sewage containing nitrite, then adding copper bismuthate-fullerene photocatalyst, introducing nitrogen to remove oxygen to create anaerobic condition (or respectively under anaerobic and aerobic conditions), and irradiating the obtained mixed system with ultraviolet visible light so as to simultaneously remove the nitrite and the ammonia nitrogen.
In some exemplary embodiments, the method for simultaneously removing nitrite and ammonia nitrogen by using the copper bismuthate-fullerene photocatalyst comprises the following steps: adding the copper bismuthate-fullerene photocatalyst into the mixed system, irradiating the mixed system with ultraviolet visible light under anaerobic and aerobic conditions respectively, and simultaneously removing nitrite and ammonia nitrogen; and oxygenating the mixed system, and irradiating by ultraviolet and visible light to completely degrade ammonia nitrogen in the sewage into N2And the nitrite and ammonia nitrogen in the sewage can be removed simultaneously.
In some exemplary embodiments, the method comprises: and adjusting the mixed system to be alkaline, and irradiating the mixed system with ultraviolet visible light under anaerobic and aerobic conditions respectively to remove nitrite and ammonia nitrogen in the sewage simultaneously.
Further, the pH value of the mixed system is 9.0-10.5.
In some more specific exemplary embodiments, the method may further include: performing oxidation treatment or biological treatment on sewage containing ammonia nitrogen, for example, degrading ammonia nitrogen in the sewage by using microorganisms to convert part of the ammonia nitrogen in the sewage into nitrite nitrogen, then adding a copper bismuthate-fullerene photocatalyst into the sewage, and irradiating the obtained mixed system with ultraviolet visible light under anaerobic and aerobic conditions respectively so as to simultaneously remove nitrite and ammonia nitrogen in the sewage.
Wherein, the technology for degrading ammonia nitrogen by microorganisms can refer to the prior art in the field, such as CN107244742A, CN107974416A, CN106947709A, CN106676038A and the like.
In some more specific exemplary embodiments, the method specifically includes:
and (3) putting a certain amount of the copper bismuthate-fullerene photocatalyst into mixed reaction liquid containing nitrite and ammonia nitrogen, and adjusting the pH of the reaction liquid to be about 9.0-10.5 by using sodium hydroxide. The reaction is divided into two stages: the first stage is carried out in a closed reaction system, nitrogen is firstly introduced for 20min, and then nitrite and ammonia nitrogen are simultaneously removed under the irradiation of an ultraviolet lamp; and in the second stage, air is filled into the reaction liquid, and then ultraviolet and visible light irradiation is carried out to remove nitrogen which is not removed in the first stage. The method can simultaneously remove nitrite and ammonia nitrogen in the water body, and effectively utilizes sunlight to remove nitrogen in the water body. The catalyst is irradiated by ultraviolet and visible light, and the removal rate of the copper bismuthate-fullerene composite photocatalyst for simultaneously removing nitrite and ammonia nitrogen in water can reach about 90%.
Furthermore, the copper bismuthate-fullerene photocatalyst contains 0.01-10.0wt% of fullerene and 90.00-99.99wt% of copper bismuthate.
In some exemplary embodiments, the method for preparing the copper bismuthate-fullerene photocatalyst comprises:
dissolving soluble bismuth salt, soluble copper salt and fullerene in a solvent, uniformly mixing, then adjusting the mixed solution to be alkaline, and reacting the mixed solution at 180 ℃ for 8 hours to obtain the copper bismuthate-fullerene photocatalyst.
In some exemplary embodiments, the preparation method specifically includes: dissolving soluble bismuth salt, soluble copper salt and fullerene in a solvent, uniformly mixing, then adjusting the mixed solution to be alkaline, and reacting the mixed solution at 180 ℃ for 8 hours to obtain the copper bismuthate-fullerene photocatalyst.
Further, the molar ratio of the soluble bismuth salt to the soluble copper salt is 2: 1.
further, the mass ratio of the fullerene to the copper bismuthate is 1-9: 100.
further, the soluble bismuth salt includes bismuth nitrate, but is not limited thereto.
Further, the soluble copper salt includes, but is not limited to, copper nitrate.
Further, the solvent includes deionized water, but is not limited thereto.
Further, the alkaline substance for adjusting the mixed solution to be alkaline includes, but is not limited to, sodium hydroxide.
Further, the preparation method further comprises the following steps: and (2) reacting the mixed solution for 8 hours at the temperature of 180 ℃, washing with deionized water, filtering, and drying in an oven at the temperature of 40-60 ℃ for 24 hours to obtain the copper bismuthate-fullerene photocatalyst.
By the technical scheme, the method creatively integrates the nitrite removal and the ammonia nitrogen removal, simultaneously removes the nitrite and the ammonia nitrogen under the radiation of sunlight, changes the technological processes of the nitrite removal and the traditional denitrification, shortens the working condition time, reduces the time cost, saves the economic cost, has high removal rate, and has obvious technical progress compared with the prior art.
The technology of the present invention is further explained below with reference to the drawings and examples.
Example 1
Bismuth nitrate and copper nitrate are used as raw materials, and the molar ratio Bi: 2 of Cu: 1, respectively dissolving in deionized water, and uniformly mixing. Adding the fullerene which is dried for 2 hours and at 120 ℃ into the mixed solution according to the mass of 1-9% of the copper bismuthate, carrying out ultrasonic treatment for 60-90 minutes, and stirring for 60 minutes. Then adding a certain amount of sodium hydroxide, stirring for 60-90 minutes, moving to a high-pressure reaction kettle, and heating for 8 hours at 180 ℃ in a sealed manner. After the sample was cooled to room temperature, it was washed with deionized water, filtered, and the sodium hydroxide and other electrolytes were removed. Drying in an oven at 40-60 ℃ for 24 hours to obtain the copper bismuthate-fullerene composite semiconductor material.
0.3750g of copper bismuthate-fullerene photocatalyst prepared by the method is taken, placed into 250mL of reaction liquid containing 50mg/L nitrite nitrogen and 100mg/L ammonia nitrogen (deionized water used in the reaction liquid is introduced with nitrogen for 30min to remove dissolved oxygen in water), added with a proper amount of NaOH, the pH value of the solution is kept between 9.5 and 10.0, placed in a photocatalytic reactor, and stirred by a magnetic stirrer under the irradiation of ultraviolet visible light to carry out photocatalytic reaction. And measuring the absorbance of the residual ammonia nitrogen, nitrite nitrogen and nitrate nitrogen every 30 min. The reaction conditions of ammonia nitrogen, nitrite nitrogen and nitrate nitrogen are calculated. In the first stage (a closed reactor, see figure 1), the nitrite nitrogen removal rate reaches 89%, the ammonia nitrogen removal rate reaches 56% and no nitrate nitrogen is generated after 5 hours of illumination; in the second stage (oxygenation), the light irradiation is continued for 8 hours (total 13 hours), the nitrite nitrogen removal rate is 90 percent, the ammonia nitrogen removal rate reaches 83 percent, and no nitrate nitrogen is generated.
In the reaction process, nitrite nitrogen, nitrate nitrogen and ammonia nitrogen are respectively detected, so that mutual interference is avoided. The determination of the content of nitrite nitrogen adopts an N- (1-naphthyl) ethylenediamine photometry, the determination of the content of nitrate nitrogen adopts an ultraviolet spectrophotometry, and the determination of ammonia nitrogen adopts a Nashin reagent colorimetry. And respectively measuring the absorbencies of nitrite nitrogen, nitrate nitrogen and ammonia nitrogen by using an ultraviolet visible spectrophotometer so as to track the changes of the nitrite nitrogen, the nitrate nitrogen and the ammonia nitrogen in the reaction.
Wherein the degradation rate of ammonia nitrogen is (1-C)t/C0)×100％＝(1-At/A0)×100％
In the formula: c0Is the initial concentration of ammonia nitrogen in the reaction solution, CtIn order to degrade the concentration of ammonia nitrogen in the reaction solution after t hours, A0Is the initial absorbance of ammonia nitrogen in the reaction solution, AtIs the absorbance of ammonia nitrogen in the reaction liquid after t hours of degradation.
Nitrite nitrogen degradation rate (1-C)t/C0)×100％＝(1-At/A0)×100％
In the formula: c0Is the initial concentration of nitrite nitrogen in the reaction solution, CtIn order to degrade the concentration of nitrite nitrogen in the reaction solution after t hours, A0Is the initial absorbance of the nitrite nitrogen in the reaction solution, AtFor degradationAbsorbance of nitrite nitrogen in the reaction solution after t hours.
Nitrate nitrogen degradation rate (1-C)t/C0)×100％＝(1-At/A0)×100％
In the formula: c0Is the initial concentration of nitrate nitrogen in the reaction solution, CtIn order to degrade the concentration of nitrate nitrogen in the reaction solution after t hours, A0Is the initial absorbance of nitrate nitrogen in the reaction solution, AtThe absorbance of the nitrate nitrogen in the reaction solution after t hours of degradation.
a. Ammonia nitrogen is measured by adopting a Nassner reagent colorimetric method:
the method comprises the following specific steps: 1.0mL of the reaction mixture was transferred to a 50mL colorimetric tube, diluted to 50mL and shaken well. 1.0mL of potassium sodium tartrate was added and shaken well. Then 1.0mL of Nashi reagent was added and shaken well. Standing for 10min, and measuring the absorbance at the wavelength of 382nm to calculate the ammonia nitrogen removal rate according to the formula.
Preparing the gardner tartrate: 50g of tartrate sodium is accurately weighed, dissolved in 100mL of deionized water, heated to boil, cooled to room temperature, added with water to a constant volume and stored in a 100mL volumetric flask.
Preparing a nano reagent: 16g of NaOH was accurately weighed, dissolved in 50mL of deionized water and cooled well to room temperature. Accurately weighed 10g of mercuric iodide and 7g of potassium iodide were dissolved in 20mL of deionized water and recorded as solution A. And dropwise adding the solution A into a NaOH solution which is continuously stirred and cooled to room temperature, adding water to a constant volume of 100mL, and storing in a volumetric flask.
b. The nitrite nitrogen is measured by adopting an N- (1-naphthyl) ethylenediamine photometry method:
the method comprises the following specific steps: 1.0mL of the reaction mixture was transferred to a 50mL colorimetric tube, diluted to 50mL and shaken well. 1.0mL of 10g/L sulfanilamide was added and shaken up. Standing for 5-8min, adding 1.0mL of 10g/L N- (1-naphthyl) ethylenediamine hydrochloride solution, and shaking up. Standing for 10min, and measuring the absorbance at 540nm to calculate the removal rate of the nitrite nitrogen according to the formula.
Preparing sulfanilamide: accurately weighing 1g of sulfanilamide, dissolving in a mixed solution of 50mL of deionized water and 10mL of concentrated hydrochloric acid with the mass fraction of 36%, adding water, diluting to a constant volume of 100mL, and storing in a volumetric flask.
Preparation of N- (1-naphthyl) ethylenediamine hydrochloride: 0.1g of ethylenediamine hydrochloride was accurately weighed and dissolved in 50mL of deionized water, and then water was added to the solution to a constant volume of 100mL in a brown volumetric flask and stored in a refrigerator.
c. The nitrate nitrogen is measured by adopting an ultraviolet spectrophotometry:
the method comprises the following specific steps: 1.0mL of the reaction solution was transferred to a 50mL colorimetric tube, and 1.0mL of 1mol/L HCl and 0.8 w% sulfamic acid solution were added thereto, diluted to 50mL, and shaken up. Standing for 10min, and measuring absorbance at 220nm to obtain nitrate nitrogen generation condition.
And (3) testing results:
referring to fig. 2, an XRD diffraction pattern of the fullerene, copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention is shown. Diffraction peaks of the curve copper bismuthate at 2 theta 20.90, 28.02, 29.68, 30.82, 33.30, 34.22, 37.38, 42.48, 45.12, 46.64, 47.71, 53.01, 55.61, 60.61, 63.77, 66.12, 68.01, 73.07, 74.23 and 78.07 correspond to (200), (211), (220), (002), (130), (112), (202), (400), (330), (141), (420), (123), (332), (521), (530), (413), (204), (451), (314) and (253) of the copper bismuthate respectively, and basically accord with a standard spectrum (JCPDS71-1774) of the copper bismuthate.
Referring to fig. 3, a raman spectrum of the fullerene, copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention is shown.
Referring to fig. 4 a-4 d, TEM images of fullerene, copper bismuthate-fullerene composite semiconductor material, copper bismuthate, and copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention are shown, respectively (fig. 4a. fullerene, fig. 4b. copper bismuthate-fullerene, fig. 4c. copper bismuthate, and fig. 4d. copper bismuthate-fullerene).
Referring to fig. 5, there is shown an ultraviolet-visible diffuse reflectance spectrum of the copper bismuthate and copper bismuthate-fullerene composite semiconductor material in example 1 of the present invention.
The inventor also characterizes the change of nitrite nitrogen and ammonia nitrogen in the reaction process of the copper bismuthate-fullerene photocatalyst. Wherein, the change of nitrite nitrogen and ammonia nitrogen in the reaction process of the copper bismuthate-fullerene composite semiconductor material can be seen in figure 6.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (12)
1. A method for simultaneously removing nitrite and ammonia nitrogen by a copper bismuthate-fullerene photocatalyst is characterized by comprising the following steps: adding a copper bismuthate-fullerene photocatalyst into sewage containing nitrite and ammonia nitrogen to form a mixed system, adjusting the mixed system to a pH value of 9.0-10.5, introducing nitrogen, irradiating the mixed system with ultraviolet visible light, introducing air into the mixed system, and irradiating the mixed system of the nitrite and the ammonia nitrogen with the ultraviolet visible light, thereby completely removing the nitrite and the ammonia nitrogen in the sewage at the same time;
wherein, the copper bismuthate-fullerene photocatalyst contains 0.01 to 10.0 weight percent of fullerene and 90.00 to 99.99 weight percent of copper bismuthate; the preparation method of the copper bismuthate-fullerene photocatalyst comprises the following steps:
dissolving soluble bismuth salt, soluble copper salt and fullerene in a solvent, uniformly mixing, then adjusting the mixed solution to be alkaline, and reacting the mixed solution at 180 ℃ for 8 hours to obtain the copper bismuthate-fullerene photocatalyst, wherein the molar ratio of the soluble bismuth salt to the soluble copper salt is 2: 1, the mass ratio of the fullerene to the copper bismuthate is 1-9: 100.
2. the method of claim 1, wherein: the soluble bismuth salt is bismuth nitrate.
3. The method of claim 1, wherein: the soluble copper salt is copper nitrate.
4. The method of claim 1, wherein: the solvent is deionized water.
5. The method of claim 1, wherein: the alkaline substance for adjusting the mixed solution to be alkaline is sodium hydroxide.
6. The method of claim 1, wherein the method of making further comprises: and (2) reacting the mixed solution for 8 hours at the temperature of 180 ℃, washing with deionized water, filtering, and drying in an oven at the temperature of 40-60 ℃ for 24 hours to obtain the copper bismuthate-fullerene photocatalyst.
7. A method for simultaneously removing nitrite and ammonia nitrogen by a copper bismuthate-fullerene photocatalyst is characterized by comprising the following steps: performing oxidation treatment or biological treatment on sewage containing ammonia nitrogen to convert part of the ammonia nitrogen into nitrite nitrogen, adding a copper bismuthate-fullerene photocatalyst to form a mixed system, adjusting the pH value of the mixed system to 9.0-10.5, irradiating the mixed system with ultraviolet visible light under anaerobic and aerobic conditions to simultaneously remove nitrite and ammonia nitrogen in the sewage;
wherein, the copper bismuthate-fullerene photocatalyst contains 0.01 to 10.0 weight percent of fullerene and 90.00 to 99.99 weight percent of copper bismuthate; the preparation method of the copper bismuthate-fullerene photocatalyst comprises the following steps:
dissolving soluble bismuth salt, soluble copper salt and fullerene in a solvent, uniformly mixing, then adjusting the mixed solution to be alkaline, and reacting the mixed solution at 180 ℃ for 8 hours to obtain the copper bismuthate-fullerene photocatalyst, wherein the molar ratio of the soluble bismuth salt to the soluble copper salt is 2: 1, the mass ratio of the fullerene to the copper bismuthate is 1-9: 100.
8. the method of claim 7, wherein: the soluble bismuth salt is bismuth nitrate.
9. The method of claim 7, wherein: the soluble copper salt is copper nitrate.
10. The method of claim 7, wherein: the solvent is deionized water.
11. The method of claim 7, wherein: the alkaline substance for adjusting the mixed solution to be alkaline is sodium hydroxide.
12. The method of claim 7, wherein the method of making further comprises: and (2) reacting the mixed solution for 8 hours at the temperature of 180 ℃, washing with deionized water, filtering, and drying in an oven at the temperature of 40-60 ℃ for 24 hours to obtain the copper bismuthate-fullerene photocatalyst.
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