CN114920333A - Treatment method of high-concentration ammonia nitrogen wastewater - Google Patents
Treatment method of high-concentration ammonia nitrogen wastewater Download PDFInfo
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- CN114920333A CN114920333A CN202210608502.7A CN202210608502A CN114920333A CN 114920333 A CN114920333 A CN 114920333A CN 202210608502 A CN202210608502 A CN 202210608502A CN 114920333 A CN114920333 A CN 114920333A
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
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Abstract
The invention discloses a method for treating high-concentration ammonia nitrogen wastewater, which loads a nickel-based metal organic framework material on a substrate electrode as a working electrode, applies positive voltage to the working electrode in an electrolytic bath, and carries out 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 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 which are difficult to treat by the traditional biological method, and realizes the 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
The ammonia in the wastewater is a ubiquitous typical pollutant, and the ammonia entering the ecological environment can not only damage the environment, but also threaten the health of human beings. The ammonia concentration in the wastewater is limited by taking ammonia nitrogen as an index in various wastewater discharge standards in China. Generally speaking, the traditional biological treatment method can effectively remove ammonia nitrogen, but high-concentration ammonia nitrogen wastewater, wastewater with unbalanced C/N ratio due to overhigh content of ammonia nitrogen, wastewater with biological treatment failure due to other toxic pollutants and the like are difficult to remove ammonia nitrogen by a biological method. The method for removing ammonia in wastewater without the aid of microorganisms has important application prospects.
The electro-catalysis technology can convert ammonia in the wastewater into nitrogen through the electric anodic oxidation, so that other secondary pollution is not generated while ammonia nitrogen is removed, and the electro-catalysis technology has a good application prospect. The theoretical potential of the reaction is 0.06V, the energy consumption is low, and the cost advantage is obvious. However, the poor activity of the general anode material in catalyzing the reaction usually requires a high overpotential to drive the reaction, which limits the application. Therefore, the novel electrocatalyst capable of efficiently driving the reaction has wide prospects.
Nickel is a transition metal, and is lower in cost than noble metals, and has shown some catalytic activity in electrocatalytic oxidation of ammonia in wastewater, but its performance still needs to be further improved.
Disclosure of Invention
In view of this, the invention aims to provide a method for treating high-concentration ammonia nitrogen wastewater, which has high ammonia nitrogen removal efficiency, mainly uses nitrogen as an ammonia decomposition product, and has small secondary pollution problem.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention discloses a method for treating 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 bath, and carrying out 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 several of trimesic acid, 2-amino-terephthalic acid and 1, 4-terephthalic acid.
As a preferred technical scheme, the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: dissolving nickel salt and an organic ligand in a solvent, then carrying out hydrothermal reaction, mixing the obtained nickel-based metal organic framework material with a conductive binder, and loading the mixture on a substrate electrode.
As a preferred technical scheme, the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: dissolving nickel salt and organic ligand in a solvent, then immersing the substrate electrode in a reaction solution for hydrothermal reaction, and loading the nickel-based metal organic framework material generated by the reaction on the substrate electrode.
As a preferred technical scheme, the nickel salt is one or a mixture 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, foamed nickel, a graphite sheet or a stainless steel sheet.
As a preferable technical proposal, the positive voltage applied to the working electrode in the electrolytic bath 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 and particularly 2-amino-terephthalic acid) to construct the nickel-based metal organic framework material, so that the efficiency of electrically catalyzing ammonia oxide can be greatly improved, and the ammonia decomposition product is mainly nitrogen, so that the secondary pollution problem is low.
The method can be used for treating high-concentration ammonia nitrogen wastewater, wastewater with unbalanced C/N ratio due to overhigh content of ammonia nitrogen, wastewater with biological treatment failure due to other toxic pollutants and the like which are difficult to treat by the traditional biological method, and realizes effective removal of ammonia.
Drawings
In order to make the purpose, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
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 ammonia-containing wastewater and ammonia-free control water.
Detailed Description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Example 1
(1) Synthetic nickel-based metal organic framework material
Dissolving 10 parts by weight of nickel nitrate and 30 parts by weight of 1, 4-terephthalic acid in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, placing the reaction solution in a pressure-bearing hydrothermal reaction kettle, heating to 120 ℃, preserving heat for 10 hours, naturally cooling, washing and drying the obtained product to obtain the nickel-based metal organic framework material which takes 1, 4-terephthalic acid as an organic ligand, and is named as Ni-BDC;
(2) construction of working electrodes
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic framework material, fully stirring to prepare uniform suspension, and coating the obtained suspension on a carbon cloth electrode with an electrode area of 4cm 2 Oven drying with a load of 1mg/cm 2 A catalyst-loaded working electrode, named Ni-BDC working electrode, was obtained.
Example 2
(1) Synthetic nickel-based metal organic framework material
Dissolving 10 parts by weight of nickel nitrate and 30 parts by weight of trimesic acid in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, placing the reaction liquid in a pressure-bearing hydrothermal reaction kettle, heating to 120 ℃, preserving heat for 10 hours, naturally cooling, washing and drying the obtained product to obtain a nickel-based metal organic framework material which takes trimesic acid as an organic ligand, and naming the nickel-based metal organic framework material as Ni-BTC;
(2) construction of working electrodes
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic framework material, fully stirring to prepare uniform suspension, and coating the obtained suspension on a carbon cloth electrode with an electrode area of 4cm 2 Oven drying with 1mg/cm loading 2 And obtaining a working electrode which is named as a Ni-BTC working electrode and is loaded with a catalyst.
Example 3
(1) Synthetic nickel-based metal organic framework material
Dissolving 10 parts by weight of nickel nitrate and 30 parts by weight of 2-amino-terephthalic acid 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, the temperature is raised to 120 ℃, the reaction solution is kept for 10 hours, then the reaction solution is naturally cooled, the temperature is reduced, the obtained product is recovered, cleaned and dried, and the nickel-based metal organic framework material taking 2-amino-terephthalic acid as an organic ligand is obtained, and is named as Ni-NH 2 -BDC；
(2) Construction of working electrode
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic framework material, fully stirring to prepare uniform suspension, and coating the obtained suspension on a carbon cloth electrode with an electrode area of 4cm 2 Oven drying with a load of 1mg/cm 2 Obtaining a working electrode carrying a catalyst, named Ni-NH 2 -a BDC working electrode.
Comparative example 1
(1) Synthetic nickel-based metal organic framework material
Dissolving 10 parts by weight of nickel nitrate and 30 parts by weight of 2-methylimidazole in a solvent consisting of N, N-dimethylformamide and water;
after the solid raw materials are dissolved, placing the reaction solution in a pressure-bearing hydrothermal reaction kettle, heating to 120 ℃, preserving heat for 10 hours, then naturally cooling, washing and drying the obtained product to obtain the nickel-based metal organic framework material which takes 2-methylimidazole as the organic ligand, and is named as Ni-2 MI;
(2) construction of working electrodes
Adding isopropanol solution containing naphthol into the obtained nickel-based metal organic framework material, fully stirring to prepare uniform suspension, and coating the obtained suspension on a carbon cloth electrode with an electrode area of 4cm 2 Oven drying with a load of 1mg/cm 2 A catalyst-supported working electrode was obtained, named Ni-2MI working electrode.
The nickel-based metal organic framework materials obtained in examples 1 to 3 were analyzed by an X-ray diffractometer, and the results are shown in fig. 1, and all three samples showed a plurality of crystallization peaks, which indicates that the materials have a crystal structure, and thus, the successful synthesis of the nickel-based metal organic framework materials with different ligands was confirmed.
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. Respectively adding ammonia-containing wastewater and ammonia-free wastewater into an electrolytic bath for electrochemical scanning contrast. The voltage regulator was started to perform linear voltammetric sweep of the working electrode with increasing positive voltage, the result is shown in fig. 2. In ammonia-containing wastewater, the working electrodes prepared by the three samples all showed stronger oxidation current in a partial voltage region than that in the ammonia-free solution control group, which indicates that the three samples all have the capability of electrocatalytic oxidation of ammonia in a relatively lower voltage region (0.35-0.8V). In particular, the oxidation current of example 3 was significantly higher than that of examples 1 and 2, indicating that the Ni-NH of example 3 2 The electrocatalytic oxidation of ammonia at BDC is significantly better than in examples 1 and 2.
Will carry outWorking electrodes of example 3 and comparative example 1 were placed in an electrolytic cell, and a platinum sheet cathode, a saturated calomel reference electrode, and a regulated power supply were connected to form a closed circuit. Adding wastewater which contains 1500mg/L ammonia nitrogen, has high ammonia nitrogen concentration and pH of 13 and is difficult to biologically treat into an electrolytic bath. The voltage-stabilized power supply was started, 0.5V was applied to the working electrode, and the ammonia nitrogen concentration in the wastewater and the concentrations of the generated nitrate nitrogen and nitrite nitrogen were sampled and detected over time, with the results shown in table 1. As can be seen, the Ni-NH of example 3 2 The capability of BDC electrocatalytic oxidation of ammonia is obviously better 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 have lower concentrations and smaller secondary pollution.
TABLE 1 results of electrocatalytic oxidation treatment of ammonia-containing wastewater
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the 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 framework material on a substrate electrode as a working electrode, applying positive voltage to the working electrode in an electrolytic bath, and carrying out 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 several of trimesic acid, 2-amino-terephthalic acid and 1, 4-terephthalic acid.
2. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, characterized by comprising the following steps: the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: dissolving nickel salt and an organic ligand in a solvent, then carrying out hydrothermal reaction, mixing the obtained nickel-based metal organic framework material with a conductive binder, and loading the mixture on a substrate electrode.
3. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, which is characterized in that: the method for loading the nickel-based metal organic framework material on the substrate electrode comprises the following steps: dissolving nickel salt and organic ligand in a solvent, then immersing the substrate electrode in a reaction solution for hydrothermal reaction, and loading the nickel-based metal organic framework material generated by the reaction on the substrate electrode.
4. The method for treating high-concentration ammonia nitrogen wastewater according to claim 2 or 3, characterized by comprising the following steps: the nickel salt is one or a mixture 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, characterized by comprising the following steps: 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, characterized by comprising the following steps: the temperature of the hydrothermal reaction is 120-200 ℃.
7. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, characterized by comprising the following steps: the substrate electrode is carbon cloth, foam nickel, a graphite sheet or a stainless steel sheet.
8. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, which is characterized in that: the positive voltage applied to the working electrode in the electrolytic cell is 0.35-10V based on a saturated calomel reference electrode.
9. The method for treating high-concentration ammonia nitrogen wastewater according to claim 1, which is characterized in that: the high-concentration ammonia nitrogen wastewater is wastewater with ammonia nitrogen concentration of 1000-.
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