CN110980892A - Method for removing nitrate nitrogen and nitrite nitrogen in water body by activated cathode nascent hydrogen rapid reduction - Google Patents
Method for removing nitrate nitrogen and nitrite nitrogen in water body by activated cathode nascent hydrogen rapid reduction Download PDFInfo
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- CN110980892A CN110980892A CN201911037364.6A CN201911037364A CN110980892A CN 110980892 A CN110980892 A CN 110980892A CN 201911037364 A CN201911037364 A CN 201911037364A CN 110980892 A CN110980892 A CN 110980892A
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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
- C02F1/46—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
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/166—Nitrites
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
Abstract
The invention belongs to the technical field of nitrate and nitrite removal in water pollution treatment, and particularly relates to a method for removing nitrate nitrogen and nitrite nitrogen in water by using a framework metal catalyst to activate cathode nascent hydrogen and rapidly reduce the nascent hydrogen. The method is characterized in that a water sample containing nitrate and nitrite is added into a cathode chamber, and the reduction removal of the nitrate and nitrite is rapidly realized by utilizing the catalytic generation of atomic hydrogen from hydrogen generated by a skeleton metal. The reaction is clean and efficient, can continuously run, and has obvious application advantages in the reduction removal of nitrate nitrogen and nitrite nitrogen.
Description
Technical Field
The invention belongs to the technical field of nitrate and nitrite treatment for environmental protection, and particularly relates to a method for removing nitrate nitrogen and nitrite nitrogen in water by activating cathode nascent hydrogen and rapidly reducing framework metal catalyst.
Background
Nitrate and nitrite are inevitably produced directly or indirectly in industrial and agricultural processes such as food processing, petrochemical, textile, electroplating and agricultural fertilization (Chemical engineering journal.2011.168.493-504) by human beings. Wherein, nitrate can be reduced into nitrite after being taken by human body in the environment, a large amount of nitrite can cause direct poisoning of human body, and a small amount of nitrite can act with human blood to form methemoglobin, which leads the blood to lose oxygen carrying capacity and endanger life. In addition, nitrites react with secondary amines to form nitrosamines, which are carcinogenic in sufficient quantities (Catalysis Science & technology.2013.3.879-899).
Most nitrates are very soluble in water and are stable and not easily adsorbed and co-precipitated for removal, so conventional water treatment techniques are not suitable for removing nitrate nitrogen. At present, the industrial treatment methods for (nitrite) are commonly as follows: electrodialysis, reverse osmosis, microbial reduction, chemical reduction, electrochemical reduction, and catalytic hydrogenation. The problems of membrane selectivity and membrane fouling are the major research issues facing electrodialysis and reverse osmosis, and the higher treatment costs are also obstacles to their scale-up (Desalination and Water treatment.2010.23.13-19). Microbial reduction is a biochemical treatment technique that utilizes denitrifying bacteria to reduce nitrate nitrogen to nitrogen under anaerobic conditions. At present, the culture and screening of strains are mature, but the technology has high requirements on the composition of a water body and is only suitable for denitrification treatment of partial wastewater (chemical engineering technology.2013.36.2101-2107). Chemical reduction represented by zero-valent metal is an emerging technology for removing nitrate (nitrite) nitrogen, but the stability and catalytic activity of the catalyst are still to be further researched and improved (Science, soft, Total environment, 2019, 671, 388-403). Electrochemical reduction and catalytic hydrogenation have attracted much attention because of their green and efficient properties, as compared with other technologies (Electrochimica acta.2005.50.5237-5241; Journal of molecular Catalysis A: chemical.2000.158.237-249). It is noted that the selection of noble metal catalyst in electrochemical reduction and the reaction conditions of high temperature and high pressure in catalytic hydrogenation still need further improvement. In order to overcome the defects of the prior art, a safe, green and efficient nitrate (nitrite) nitrogen reduction system needs to be established.
Disclosure of Invention
Aiming at the defects in the prior art, the method combines the advantages of electrochemical reduction and catalytic hydrogenation, provides a hydrogen source and an alkaline catalytic environment by using electrolyzed water to generate new hydrogen in situ, and selects cheap and easily-obtained framework metal as a hydrogenation catalyst. The improvement can rapidly realize the reduction removal of nitrate (nitrite) nitrogen at normal temperature and normal pressure.
Specifically, the invention provides a method for removing nitrate nitrogen and nitrite nitrogen in a water body by activating nascent hydrogen and rapidly reducing the nascent hydrogen, which sequentially comprises the following steps:
the method comprises the following steps: adding an aqueous solution containing nitrate and nitrite into a cathode chamber containing a magnetic rotor, wherein the anode chamber is an aqueous solution with the same electrolyte concentration;
step two: inserting a cathode plate and an anode plate into the cathode chamber and the anode chamber respectively, and connecting a voltage-stabilizing direct-current power supply;
step three: starting magnetic stirring, adding proper amount of skeleton metal catalyst and connecting DC power supply.
According to the method, the nitrate and the nitrite are easily soluble inorganic salts, and the concentration of the nitrate and the nitrite is 0-10 mM.
In the method, the nitrate and the nitrite are sodium nitrate and sodium nitrite.
According to the method, the anode plate is a ruthenium-iridium electrode, a tin-antimony electrode or a lead dioxide electrode.
According to the method, the anode plate is a ruthenium-iridium electrode.
According to the method, the cathode plate is a pure titanium plate, a stainless steel plate or a graphite plate.
According to the method, the cathode plate is a pure titanium plate.
In the method, the catalyst is a framework metal (iron, cobalt, nickel and copper) catalyst.
In the method, the catalyst is framework metal catalyst and is framework nickel.
According to the method, the mass concentration ratio of the catalyst to the nitrate nitrogen or the nitrite nitrogen is 10:1-100: 1.
Compared with the prior art, the invention has the following advantages:
1. the invention has mild reaction conditions and cheap and easily-obtained and recyclable catalyst. The alkaline environment generated by cathode electrolysis of water obviously improves the stability and hydrogenation potential of Raney nickel skeleton metal catalyst, and avoids secondary pollution caused by catalyst dissolution.
2. The invention has wide selection range of the cathode plate, does not need to carry out rigorous modification and pretreatment, and has low cost and simple operation.
3. The invention has low requirement on water body composition, and can realize rapid and efficient reduction removal of NO in various toxic and harmful wastewater3 -And NO2 -。
Drawings
FIG. 1 shows NO in the reaction solution of example 1 at different current densities3 -And NO2 -Schematic diagram of the concentration change of (1).
FIG. 2 shows NO in the reaction solution in example 2 at different amounts of catalyst added3 -And NO2 -Schematic diagram of the concentration change of (1).
FIG. 3 shows NO in the reaction solution at different initial concentrations in example 33 -And NO2 -Schematic diagram of the concentration change of (1).
FIG. 4 shows NO in example 43 --N and NO2 --N reduction removal effect graph.
FIG. 5 is a graph showing the concentration of humic acid and calcium and magnesium ions in water versus NO in the reaction solution in example 53 -And NO2 -The effect of reduction.
FIG. 6 is a graph of the pair of NO in the reduction system of example 63 -Reproducibility of the reduction.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood by those skilled in the art, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a method for removing nitrate nitrogen and nitrite nitrogen in a water body by activating nascent hydrogen and rapidly reducing, which sequentially comprises the following steps:
the method comprises the following steps: adding an aqueous solution containing nitrate and nitrite into a cathode chamber containing a magnetic rotor, wherein the anode chamber is an aqueous solution with the same electrolyte concentration;
step two: inserting a cathode plate and an anode plate into the cathode chamber and the anode chamber respectively, and connecting a voltage-stabilizing direct-current power supply;
step three: starting magnetic stirring, adding proper amount of skeleton metal catalyst and connecting DC power supply.
According to the method, the nitrate and the nitrite are easily soluble inorganic salts, and the concentration of the nitrate and the nitrite is 0-10 mM.
In the method, the nitrate and the nitrite are sodium nitrate and sodium nitrite.
According to the method, the anode plate is a ruthenium-iridium electrode, a tin-antimony electrode or a lead dioxide electrode.
According to the method, the anode plate is a ruthenium-iridium electrode.
According to the method, the cathode plate is a pure titanium plate, a stainless steel plate or a graphite plate.
According to the method, the cathode plate is a pure titanium plate.
In the method, the catalyst is a framework metal (iron, cobalt, nickel and copper) catalyst.
In the method, the catalyst is framework metal catalyst and is framework nickel.
According to the method, the mass concentration ratio of the catalyst to the nitrate nitrogen or the nitrite nitrogen is 10:1-100: 1.
The invention belongs to the technical field of nitrate and nitrite removal in water pollution treatment, and particularly relates to a method for removing nitrate nitrogen and nitrite nitrogen in water by using a framework metal catalyst to activate cathode nascent hydrogen and rapidly reduce the nascent hydrogen. According to the invention, a water sample containing nitrate and nitrite is added into the cathode chamber, and the reduction removal of the nitrate and nitrite is rapidly realized by utilizing the skeleton metal to catalyze the nascent hydrogen to form atomic hydrogen.
The method has clean and efficient reaction, can continuously run, and has obvious application advantages in the reduction removal of nitrate nitrogen and nitrite nitrogen.
According to the method of the invention, the reduction removal of nitrate (nitrite) nitrogen can be rapidly realized at normal temperature and normal pressure.
In detail, the treatment method for removing nitrate (nitrite) nitrogen in water environment by rapid hydrogenation through activating nascent hydrogen by using the framework metal catalyst sequentially comprises the following steps. Step 1: adding a solution containing nitrate (nitrite) nitrogen into a cathode chamber, wherein an anode chamber is an aqueous solution with the same electrolyte concentration; step 2: inserting a cathode plate and an anode plate into the cathode chamber and the anode chamber respectively; and step 3: connecting a voltage-stabilizing direct-current power supply and adjusting the current value; and 4, step 4: adding proper amount of Raney nickel catalyst and starting DC power supply.
In the invention, the nitrate (nitrite) nitrogen is soluble nitrate and nitrite, and sodium nitrate and sodium nitrite are preferably selected, and the concentration of the nitrate (nitrite) nitrogen is 3 mM.
In the present invention, the electrolyte is anhydrous sodium sulfate, and the concentration is 5-100mM, preferably 20 mM.
In the invention, the electrolytic cell is a bipolar chamber, an N211 type DuPont proton exchange membrane is used as a diaphragm, and the addition amount of the stock solution in the cathode chamber and the anode chamber is 90ml each time.
In the invention, the anode plate is a ruthenium-iridium electrode, a tin-antimony electrode or a lead dioxide electrode, preferably a ruthenium-iridium electrode, and the effective area of the anode plate is 9cm2。
In the invention, the cathode plate is a pure titanium plate, a stainless steel plate or a graphite plate, preferably a pure titanium plate, and the effective area of the cathode plate is 9cm2。
In the present invention, the skeletal metal catalyst is commercial raney nickel.
In the present invention, the mass ratio of the catalyst to the (nitrite) salt is 10:1-100: 1.
the invention utilizes the hydrogen precipitated by the Raney nickel activated cathode to form high-activity atomic hydrogen which is combined with the hydrogen to act as-N-O-bond in (nitrite) nitrate radical, thereby realizing NO3 -And NO2 -The rapid reduction of (2).
Example 1
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps:
the method comprises the following steps: measuring pre-configured 3mM NO3 -Or NO2 -90ml of the solution is added into a cathode chamber, the same amount of deionized water is measured in an anode chamber, and electrolyte is added to ensure that the electrolyte concentration in the anode chamber and the cathode chamber is 20 mM. The anode chamber is inserted into a ruthenium iridium electrode, the cathode chamber is inserted into a pure titanium plate, and the direct current stabilized voltage supply is connected with the electrode.
Step two: under magnetic stirring, adding Raney nickel catalyst into cathode chamber, with the catalyst amount of 1g/L, starting power supply rapidly, pressing stopwatch, sucking certain reaction solution with injector and passing through 0.22 μm microporous filter membrane rapidly when reaction time is 0min, 5min, 10min, 20min, 30min, 45min, 60min, and 90min, respectively, and testing the obtained filtrates.
Test 1: the obtained filtrate is directly subjected to ion chromatography for NO determination3 -Or NO2 -Concentration (detection conditions: 30mM sodium hydroxide solution as mobile phase, flow rate 1.2ml/min, conductivity detector).
To better study the current density versus reduced NO3 -Or NO2 -The following five experiments were performed: and before the power supply is started in the second step, the power supply is adjusted to a constant current mode, the currents are respectively adjusted to be 0A, 0.04A, 0.08A, 0.12A and 0.16A, and the other conditions are not changed. The results obtained are shown in FIG. 1. FIG. 1 shows that the Raney nickel catalyst itself has a certain catalytic effect due to the adsorption of hydrogen, and 16.04% and 31.80% of NO can be reduced by Raney nickel with an addition of 1g/L in one hour under the condition of NO current3 -And NO2 -. As the current density increases, the cathode hydrogen production increases, NO3 -And NO2 -The reduction rate is enhanced and NO is obtained after the current reaches 0.12A3 -And NO2 -All reduction can be achieved within one hour.
Example 2
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps:
the difference from example 1 is: in the second step, a constant current mode is adopted, the current is 0.12A, and the addition amount of the Raney nickel is 0g/L, 0.2g/L, 0.5g/L, 1g/L and 1.5g/L each time, so that the addition amount of the Raney nickel to NO is obtained3 -And NO2 -The reduction rate was not affected, and the rest of the conditions were unchanged. The results are shown in FIG. 2. FIG. 2 shows that hydrogen gas separated out from a pure titanium plate has a certain catalytic effect, and 17.45% and 20.10% of NO are respectively contained in one hour under the condition of NO catalyst addition3 -And NO2 -Reduced, and the catalytic activity is obviously increased along with the increase of the addition of the Raney nickel.
Example 3
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps:
the difference from the embodiment 2 is that: step one of regulating NO3 -And NO2 -Was 1mM, 2mM, 3mM, 4mM, 5mM, the fixed current in step two was 0.12A, and the catalyst addition amount was 1 g/L. Catalyzing reaction for one hour, detecting NO in the reacted solution by ion chromatography3 -And NO2 -The concentration of (c). The results are shown in FIG. 3. FIG. 3 shows the following NO3 -And NO2 -Initial concentration increase of (2), Ct/C0A downward trend is exhibited.
Example 4
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps:
the method comprises the following steps: measuring pre-configured 3mM NO3 -And NO2 -90ml of the solution is added into a cathode chamber, the same amount of deionized water is measured in an anode chamber, and electrolyte is added to ensure that the electrolyte concentration in the anode chamber and the cathode chamber is 20 mM. Inserting ruthenium iridium electrode into anode and pure titanium plate into cathode, and mixingThe DC voltage-stabilized source is connected with the electrode, and the current is adjusted to 0.12A.
Step two: under magnetic stirring, adding Raney nickel catalyst into cathode chamber, with the catalyst amount of 1g/L, starting power supply rapidly, pressing stopwatch, sucking certain reaction solution with injector at reaction time of 0min, 30min, 60min, 90min, and passing through 0.22 μm microporous membrane rapidly, and testing the obtained filtrates.
Test 1: the obtained filtrate is directly subjected to ion chromatography for NO determination3 -Or NO2 -Concentration (detection conditions: 30mM sodium hydroxide solution as mobile phase, flow rate 1.2ml/min, conductivity detector).
And (3) testing 2: the filtrate was directly subjected to ion chromatography for NH determination4 +Concentration (detection conditions: 20mM methane sulfonic acid solution as mobile phase, flow rate 1.5ml/min, conductivity detector).
And (3) testing: the total nitrogen measurement was directly performed on 10mL of each of the filtrates obtained at 0min, 30min, 60min and 90 min. As can be seen from FIG. 4, when NO is present3 -And NO2 -The total nitrogen and ammonium nitrogen contents are substantially the same at full reduction, and we therefore believe that NO is present3 -And NO2 -The reduction products of (a) are mainly nitrogen and ammonium radicals,
example 5
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps:
the difference from example 4 is: in step two with NO3 -For example, a constant current mode is adopted, the current is 0.1A, the addition amount of Raney nickel is 1g/L each time, humic acid and calcium magnesium ions with different concentrations are respectively added into a cathode chamber, and the other conditions are not changed. The results are shown in FIG. 5.
FIG. 5 shows that the addition of humic acid is substantially free of NO3 -Has an effect on the reduction of NO3 -Has good selectivity. Calcium and magnesium ion pair NO in water sample3 -Has an inhibitory effect, mainly due to the following anionsThe strong alkalinity, the calcium and magnesium ions are precipitated and separated out, and the active sites of the Raney nickel are reduced.
Example 6
A method for removing nitrate nitrogen and nitrite nitrogen in a water body by activated cathode nascent hydrogen rapid reduction comprises the following steps: the difference from the example 5 is that: magnetically recovering Raney nickel catalyst after each reaction, washing with deionized water, and then carrying out NO again3 -Reduction removal experiment of (1). The experiment was repeated 5 times, and the filtrate after 90min of reaction was measured by ion chromatography and NO was calculated3 -The remaining amount of (c). The experimental result is shown in fig. 6, the raney nickel catalyst is repeatedly used for 5 times, and the reaction activity is not obviously reduced, which indicates that the raney nickel catalyst has good stability under the reduction system.
Compared with the prior art, the invention has the following advantages:
1. the invention has mild reaction conditions and cheap and easily-obtained and recyclable catalyst. The alkaline environment generated by cathode electrolysis of water obviously improves the stability and hydrogenation potential of Raney nickel skeleton metal catalyst, and avoids secondary pollution caused by catalyst dissolution.
2. The invention has wide selection range of the cathode plate, does not need to carry out rigorous modification and pretreatment, and has low cost and simple operation.
3. The invention has low requirement on water body composition, and can realize rapid and efficient reduction removal of NO in various toxic and harmful wastewater3 -And NO2 -。
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for activating nascent hydrogen to rapidly reduce and remove nitrate nitrogen and nitrite nitrogen in a water body sequentially comprises the following steps:
the method comprises the following steps: adding an aqueous solution containing nitrate and nitrite into a cathode chamber containing a magnetic rotor, wherein the anode chamber is an aqueous solution with the same electrolyte concentration;
step two: inserting a cathode plate and an anode plate into the cathode chamber and the anode chamber respectively, and connecting a voltage-stabilizing direct-current power supply;
step three: starting magnetic stirring, adding proper amount of skeleton metal catalyst and connecting DC power supply.
2. The method of claim 1, wherein the nitrate and nitrite are readily soluble inorganic salts and the concentration of the nitrate and nitrite is 0-10 mM.
3. The method of claim 2, wherein the nitrates and nitrites are sodium nitrate and sodium nitrite.
4. The method of claim 1, wherein the anode plate is a ruthenium iridium electrode, a tin antimony electrode, or a lead dioxide electrode.
5. The method of claim 4, wherein the anode plate is a ruthenium iridium electrode.
6. A method according to claim 1, characterized in that the cathode plate is a pure titanium plate, a stainless steel plate or a graphite plate.
7. The method of claim 6, wherein the cathode plate is a pure titanium plate.
8. The method of claim 1, wherein the catalyst is a skeletal metal (iron, cobalt, nickel, copper) catalyst.
9. The method of claim 8, wherein the catalyst is a skeletal metal catalyst is skeletal nickel.
10. The method according to claim 1, wherein the mass concentration ratio of the catalyst to the nitrate nitrogen or nitrite nitrogen is 10:1-100: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112237927A (en) * | 2020-09-27 | 2021-01-19 | 东莞理工学院 | Catalyst for electrocatalytic reduction of nitrate and preparation method and application thereof |
| CN112429844A (en) * | 2020-10-23 | 2021-03-02 | 同济大学 | Method and system for deep denitrification of sewage |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112237927A (en) * | 2020-09-27 | 2021-01-19 | 东莞理工学院 | Catalyst for electrocatalytic reduction of nitrate and preparation method and application thereof |
| CN112237927B (en) * | 2020-09-27 | 2024-03-29 | 东莞理工学院 | Catalyst for electrocatalytic reduction of nitrate as well as preparation method and application thereof |
| CN112429844A (en) * | 2020-10-23 | 2021-03-02 | 同济大学 | Method and system for deep denitrification of sewage |
| CN112429844B (en) * | 2020-10-23 | 2022-07-26 | 同济大学 | Method and system for deep denitrification of sewage |
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