CN114920333B - Treatment method of high-concentration ammonia nitrogen wastewater - Google Patents
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Abstract
The invention discloses a treatment method of high-concentration ammonia nitrogen wastewater, which comprises the steps of loading a nickel-based metal organic framework material on a substrate electrode as a working electrode, applying positive voltage to the working electrode in an electrolytic tank, and performing electrocatalytic oxidation treatment on the high-concentration ammonia nitrogen wastewater to remove ammonia in the high-concentration ammonia nitrogen wastewater. The method can be used for treating wastewater which is difficult to treat by traditional biological methods, such as wastewater with unbalanced C/N ratio caused by overhigh ammonia nitrogen content, wastewater with biological treatment failure caused by other toxic pollutants, and the like, so as to realize effective removal of ammonia.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a treatment method of high-concentration ammonia nitrogen wastewater.
Background
Ammonia in wastewater is a ubiquitous and typical pollutant, and its entry into the ecological environment can not only cause environmental damage, but also threaten human health. Various wastewater discharge standards in China all use ammonia nitrogen as an index to limit the ammonia concentration in wastewater. Generally, the traditional biological treatment method can effectively remove ammonia nitrogen, but high-concentration ammonia nitrogen wastewater, wastewater with unbalanced C/N ratio caused by overhigh ammonia nitrogen content, wastewater with biological treatment failure caused by other toxic pollutants and the like are difficult to finish ammonia nitrogen removal by the biological method. The method for removing ammonia in the wastewater without microorganism has important application prospect.
The electrocatalytic technology can convert ammonia in the wastewater into nitrogen through electro-anodic oxidation, so that ammonia nitrogen is removed without generating other secondary pollution, and the method has a good application prospect. The reaction theoretical potential is 0.06V, the energy consumption is lower, and the cost advantage is obvious. However, the poor activity of typical anode materials in catalyzing the reaction often requires a high overpotential to drive the reaction, limiting its application. Therefore, the novel electrocatalyst capable of efficiently driving the reaction has wide prospect.
Nickel is a transition metal, costs are lower than noble metals, and nickel has shown some catalytic activity in electrocatalytically oxidizing ammonia in wastewater, but its performance is still to be further improved.
Disclosure of Invention
Therefore, the invention aims to provide a treatment method of high-concentration ammonia nitrogen wastewater, which has high ammonia nitrogen removal efficiency, and ammonia decomposition products mainly comprise nitrogen, so that the problem of secondary pollution is small.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the invention discloses a treatment method of high-concentration ammonia nitrogen wastewater, which comprises the steps of loading a nickel-based metal organic framework material on a substrate electrode as a working electrode, applying positive voltage to the working electrode in an electrolytic tank, and performing electrocatalytic oxidation treatment on the high-concentration ammonia nitrogen wastewater to remove ammonia in the high-concentration ammonia nitrogen wastewater; the organic ligand in the nickel-based metal organic framework material is one or a mixture of more of trimesic acid, 2-amino-terephthalic acid and 1, 4-terephthalic acid.
As a preferred technical solution, the method for loading the nickel-based metal organic framework material on the base electrode comprises the following steps: and dissolving nickel salt and an organic ligand in a solvent, performing hydrothermal reaction, mixing the obtained nickel-based metal organic frame material with a conductive adhesive, and loading the mixture on a substrate electrode.
As a preferred technical solution, the method for loading the nickel-based metal organic framework material on the base electrode comprises the following steps: and (3) dissolving nickel salt and an organic ligand in a solvent, immersing the substrate electrode in a reaction liquid for hydrothermal reaction, and loading the nickel-based metal-organic framework material on the substrate electrode.
As the preferable technical scheme, the nickel salt is one or a mixture of a plurality of nickel nitrate, nickel nitrite, nickel nitrate hexahydrate, nickel sulfate and nickel chloride.
As a preferable technical scheme, the weight ratio of the nickel salt to the organic ligand is 1:1-100.
As a preferable technical scheme, the temperature of the hydrothermal reaction is 120-200 ℃.
As a preferable technical scheme, the substrate electrode is carbon cloth, foam nickel, graphite sheet or stainless steel sheet.
As a preferable technical scheme, the positive voltage applied to the working electrode in the electrolytic tank is 0.35-10V based on the saturated calomel reference electrode.
As a preferable technical scheme, the high-concentration ammonia nitrogen wastewater is wastewater with ammonia nitrogen concentration of 1000-20000mg/L, pH 10-14.
The invention has the beneficial effects that:
the invention discovers that the nickel metal is combined with specific organic ligands (trimesic acid, 2-amino-terephthalic acid, 1, 4-terephthalic acid, especially 2-amino-terephthalic acid) to construct the nickel-based metal organic framework material, so that the efficiency of electrocatalytic oxidation of ammonia can be greatly improved, and ammonia decomposition products are mainly nitrogen, so that the problem of secondary pollution is small.
The method can be used for treating wastewater which is difficult to treat by traditional biological methods, such as wastewater with unbalanced C/N ratio caused by overhigh ammonia nitrogen content, wastewater with biological treatment failure caused by other toxic pollutants, and the like, so as to realize effective removal of ammonia.
Drawings
In order to make the objects, technical solutions and advantageous effects of the present invention more clear, the present invention provides the following drawings for description:
fig. 1 is an XRD pattern of three nickel-based metal-organic framework materials.
FIG. 2 is a graph of the current response of three nickel-based metal organic framework materials in an ammonia-containing wastewater and an ammonia-free control water body.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to limit the invention, so that those skilled in the art may better understand the invention and practice it.
Example 1
(1) Synthetic nickel-based metal organic framework materials
10 parts by weight of nickel nitrate and 30 parts by weight of 1, 4-terephthalic acid are dissolved in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, the reaction solution is placed in a pressure-bearing hydrothermal reaction kettle, heated to 120 ℃ and kept for 10 hours, then naturally cooled, and the obtained product is recovered, cleaned and dried to obtain a nickel-based metal organic framework material taking 1, 4-terephthalic acid as an organic ligand, which is named as Ni-BDC;
(2) Construction of working electrode
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic frame material, stirring thoroughly to prepare uniform suspension, coating the obtained suspension on carbon cloth electrode, and making electrode area 4cm 2 Drying, wherein the loading capacity is 1mg/cm 2 A catalyst-supported working electrode, designated as a Ni-BDC working electrode, was obtained.
Example 2
(1) Synthetic nickel-based metal organic framework materials
10 parts by weight of nickel nitrate and 30 parts by weight of trimesic acid are dissolved in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, the reaction solution is placed in a pressure-bearing hydrothermal reaction kettle, heated to 120 ℃ and kept for 10 hours, then naturally cooled, and the obtained product is recovered, cleaned and dried to obtain a nickel-based metal organic framework material taking trimesic acid as an organic ligand, which is named as Ni-BTC;
(2) Construction of working electrode
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic frame material, stirring thoroughly to prepare uniform suspension, coating the obtained suspension on carbon cloth electrode, and making electrode area 4cm 2 Drying, wherein the loading capacity is 1mg/cm 2 Obtaining a catalyst-supported working electrodeNamed as Ni-BTC working electrode.
Example 3
(1) Synthetic nickel-based metal organic framework materials
10 parts by weight of nickel nitrate and 30 parts by weight of 2-amino-terephthalic acid are dissolved in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, the reaction solution is placed in a pressure-bearing hydrothermal reaction kettle, heated to 120 ℃ and kept for 10 hours, then naturally cooled, and the obtained product is recovered, cleaned and dried to obtain a nickel-based metal-organic framework material taking 2-amino-terephthalic acid as an organic ligand, which is named as Ni-NH 2 -BDC；
(2) Construction of working electrode
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic frame material, stirring thoroughly to prepare uniform suspension, coating the obtained suspension on carbon cloth electrode, and making electrode area 4cm 2 Drying, wherein the loading capacity is 1mg/cm 2 Obtaining a catalyst-supported working electrode, designated Ni-NH 2 -a BDC working electrode.
Comparative example 1
(1) Synthetic nickel-based metal organic framework materials
10 parts by weight of nickel nitrate and 30 parts by weight of 2-methylimidazole are dissolved in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, the reaction solution is placed in a pressure-bearing hydrothermal reaction kettle, heated to 120 ℃ and kept for 10 hours, then naturally cooled, and the obtained product is recovered, cleaned and dried to obtain a nickel-based metal organic frame material taking 2-methylimidazole as an organic ligand, which is named as Ni-2MI;
(2) Construction of working electrode
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic frame material, stirring thoroughly to prepare uniform suspension, coating the obtained suspension on carbon cloth electrode, and making electrode area 4cm 2 Drying, wherein the loading capacity is 1mg/cm 2 Obtaining a catalyst-supported working electrode designated Ni-2MI workAn electrode.
The nickel-based metal organic framework materials obtained in examples 1-3 were analyzed by an X-ray diffractometer, and the results are shown in FIG. 1, wherein three samples all show a plurality of crystallization peaks, which indicate that the materials have crystal structures, and the successful synthesis of the nickel-based metal organic framework materials with different ligands is proved.
The working electrodes of examples 1-3 were placed in an electrolytic cell, respectively, and a platinum sheet cathode, a saturated calomel reference electrode and a regulated power supply were connected to form a closed circuit. And respectively adding the ammonia-containing wastewater and the ammonia-free wastewater into an electrolytic tank for electrochemical scanning comparison. The regulated power supply was started to perform linear voltammetry scanning on the working electrode, and a positive voltage was applied gradually increasing, and the result was shown in fig. 2. In ammonia-containing wastewater, the working electrodes prepared by the three samples all exhibited stronger oxidation current in the partial voltage region than in the ammonia-free solution control group, indicating that the three samples all had the ability to electrocatalytically oxidize ammonia in the relatively lower voltage region (0.35-0.8V). In particular, example 3 has significantly higher oxidation current than examples 1 and 2, illustrating the Ni-NH of example 3 2 The ability of BDC to electrocatalytically oxidize ammonia is significantly stronger than in examples 1 and 2.
The working electrodes of example 3 and comparative example 1 were placed in an electrolytic cell, respectively, and a platinum sheet cathode, a saturated calomel reference electrode and a regulated power supply were connected to form a closed circuit. Wastewater containing 1500mg/L ammonia nitrogen, having a pH of 13 and a high ammonia nitrogen concentration and being difficult to biologically treat is added to the electrolytic tank. And starting a regulated power supply, applying 0.5V voltage to the working electrode, sampling and detecting the ammonia nitrogen concentration in the wastewater and the generated nitrate nitrogen and nitrite nitrogen concentration along with time, and the results are shown in table 1. It can be seen that Ni-NH of example 3 2 The BDC electrocatalytic ammonia oxidation capability is obviously stronger than that of comparative example 1, ammonia nitrogen in wastewater can be effectively removed by electrocatalytic oxidation, and meanwhile, the generated nitric acid nitrogen and nitrous acid nitrogen are low in concentration and low in secondary pollution.
TABLE 1 electrocatalytic oxidation treatment of Ammonia-containing wastewater results
The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. A method for treating high-concentration ammonia nitrogen wastewater is characterized by comprising the following steps: loading a nickel-based metal organic frame material on a substrate electrode as a working electrode, applying a positive voltage to the working electrode in an electrolytic tank, and performing electrocatalytic oxidation treatment on high-concentration ammonia nitrogen wastewater to remove ammonia in the high-concentration ammonia nitrogen wastewater;
the organic ligand in the nickel-based metal organic framework material is 2-amino-terephthalic acid.
2. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, wherein: the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: and dissolving nickel salt and an organic ligand in a solvent, performing hydrothermal reaction, mixing the obtained nickel-based metal organic frame material with a conductive adhesive, and loading the mixture on a substrate electrode.
3. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, wherein: the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: and (3) dissolving nickel salt and an organic ligand in a solvent, immersing the substrate electrode in a reaction liquid for hydrothermal reaction, and loading the nickel-based metal-organic framework material on the substrate electrode.
4. The method for treating high-concentration ammonia-nitrogen wastewater according to claim 2 or 3, wherein: the nickel salt is one or a mixture of a plurality of nickel nitrate, nickel nitrite, nickel nitrate hexahydrate, nickel sulfate and nickel chloride.
5. The method for treating high-concentration ammonia-nitrogen wastewater according to claim 2 or 3, wherein: the weight ratio of the nickel salt to the organic ligand is 1:1-100.
6. The method for treating high-concentration ammonia-nitrogen wastewater according to claim 2 or 3, wherein: the temperature of the hydrothermal reaction is 120-200 ℃.
7. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, wherein: the substrate electrode is carbon cloth, foam nickel, graphite sheet or stainless steel sheet.
8. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, wherein: the positive voltage applied to the working electrode in the electrolytic cell is 0.35-10V based on the saturated calomel reference electrode.
9. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, wherein: the high-concentration ammonia nitrogen wastewater is wastewater with ammonia nitrogen concentration of 1000-20000mg/L, pH 10-14.
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