CN113019382A - Electrocatalytic oxidation catalyst for landfill leachate and preparation method and application thereof - Google Patents
Electrocatalytic oxidation catalyst for landfill leachate and preparation method and application thereof Download PDFInfo
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- CN113019382A CN113019382A CN201911407920.4A CN201911407920A CN113019382A CN 113019382 A CN113019382 A CN 113019382A CN 201911407920 A CN201911407920 A CN 201911407920A CN 113019382 A CN113019382 A CN 113019382A
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- 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
- B01J23/83—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 rare earths or actinides
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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
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
- C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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Abstract
The invention discloses an electrocatalytic oxidation catalyst for landfill leachate, and a preparation method and application thereof. The electrocatalytic oxidation catalyst for landfill leachate comprises a carrier and metal active components, wherein the metal active components comprise copper and one or two of lanthanum or nickel; the metal active component accounts for 1-11 wt% of the total weight of the carrier. The preparation method comprises the steps of preparing a mixed solution of metal active component salt and ammonium nitrate, soaking a carrier in the mixed solution, roasting, and treating with nitrogen to obtain the catalyst. The electrocatalytic oxidation catalyst for the landfill leachate has high reaction rate, greatly reduces the power consumption in the reaction, can realize harmlessness and reclamation by adopting the electrocatalytic oxidation process, and has high organic matter removal efficiency, low operation cost and good effluent quality.
Description
Technical Field
The invention relates to the field of landfill leachate treatment, in particular to an electrocatalytic oxidation catalyst for landfill leachate, a preparation method and application thereof.
Background
The landfill leachate mainly comes from water produced by the garbage, water contained in a covering soil layer and rain and snow water flowing into a landfill area, and the water quality is characterized by high concentration of organic pollutants, high concentration of suspended matters, high salt content and high concentration of ammonia nitrogen. At present, the treatment of the landfill leachate mainly adopts a process of pretreatment, a biological system and advanced treatment of a membrane system, the effluent of the membrane process can basically reach the pollutant control standard of a landfill (GB16889-2008), and concentrated solution with the water amount of 20-30 percent of the total water amount still needs to be further treated. The concentrated solution has complex components, high salinity, high concentration and poor biodegradability, and is difficult to treat by a conventional biochemical method. How to make the concentrated solution harmless is a great problem to be solved urgently.
Currently, the treatment processes of concentrated diafiltrate can be roughly divided into two categories: one is to separate the contaminants from the water; another is to decompose or degrade the contaminants directly. Because the separated pollutants still need to be further treated, the ideal scheme is to directly adopt the advanced oxidation technology for decomposition and degradation. However, the Fenton oxidation and ozone oxidation methods require a large amount of chemicals or produce considerable amounts of by-products after treatment. In addition, the high content of chloride ions in the concentrated solution can be directly used as an electrolyte of an electrochemical oxidation technology, the efficiency is improved, no medicament is added, and no secondary pollution is generated. Therefore, the invention provides a catalyst for treating the landfill leachate concentrated solution electrocatalytic oxidation process, which adopts the electrocatalytic oxidation process as the treatment of the concentrated solution and aims at reducing the energy consumption of the electrocatalytic oxidation technology and improving the degradation efficiency.
Disclosure of Invention
Aiming at the characteristics of large water amount, complex components, high salinity, high concentration and poor biodegradability of concentrated solution generated by landfill leachate, the invention provides an electrocatalytic oxidation catalyst for treating landfill leachate concentrated solution and a preparation method thereof. It is known that the conventional advanced oxidation method requires a large amount of a chemical agent to be added or produces a considerable amount of by-products after treatment. However, the concentrated solution contains high-concentration chloride ions, can be directly used as an electrolyte of an electrochemical oxidation technology, does not contain a medicament, and does not generate secondary pollution. Therefore, the invention adopts the electrocatalytic oxidation process as the treatment technology of the concentrated solution, and provides the catalyst for treating the concentrated solution of the landfill leachate in order to further reduce the energy consumption and improve the degradation efficiency.
The invention provides an electrocatalytic oxidation catalyst for treating landfill leachate concentrated solution and a preparation method and application thereof, aiming at the characteristics of large water amount, complex components, high salinity, high concentration and poor biodegradability of the concentrated solution generated by landfill leachate.
One of the purposes of the invention is to provide an electrocatalytic oxidation catalyst for landfill leachate, which comprises a carrier and a metal active component, wherein the metal active component comprises copper and one or two of lanthanum or nickel;
the metal active component accounts for 1-11 wt% of the total weight of the carrier, and preferably 1.5-6 wt%.
The carrier is preferably an alumina/activated carbon carrier, and the particle size of the carrier is preferably 1-2 mm.
The alumina/activated carbon support is preferably prepared from components including alumina, activated carbon, and a gelling agent, wherein based on the total weight of the alumina/activated carbon support: 50-70 wt% of aluminum oxide, 15-30 wt% of active carbon and 4-15 wt% of gelling agent; preferably, the weight percentage of the alumina is 55-70%, the weight percentage of the activated carbon is 20-30%, and the weight percentage of the gelling agent is 5-10%.
The gelling agent is preferably at least one of lime or cement.
The carrier can be prepared by the method common in the field, and the carrier can be added with the auxiliary agent common in the field. Preferably, the carrier can be prepared by the following steps: mixing the components including the alumina powder, the activated carbon and the gelling agent, granulating to obtain balls with the particle size of 1-2 mm, sealing and standing for 12-24 h, roasting at 100-105 ℃ for 3-5 h, and cooling to room temperature to obtain the carrier.
The invention also aims to provide a preparation method of the electrocatalytic oxidation catalyst for the landfill leachate, which comprises the following steps:
preparing a mixed solution of metal active component salt and ammonium nitrate, soaking a carrier in the mixed solution, roasting, and treating with nitrogen to obtain the catalyst.
Among them, the metal active component salt is preferably a nitrate of a metal active component, such as copper nitrate, lanthanum nitrate, nickel nitrate.
In the preparation method, the amount of the metal active component salt is 5-25 wt% of the carrier, and preferably 5-12 wt%.
When the carrier is impregnated, the carrier is preferably stirred at a speed of 60-100 rpm for 40-80 min and then soaked for 3-5 h.
The roasting preferably comprises roasting at 100-105 ℃ for 3-5 h and roasting at 450-600 ℃ for 1-2 h.
And (3) performing nitrogen treatment when roasting is performed at the temperature of 450-600 ℃, and preferably introducing nitrogen with the volume 2-10 times that of the catalyst.
According to a preferred technical scheme of the invention, the method specifically comprises the following steps:
(1) weighing 50-70% of alumina powder, 15-30% of activated carbon powder and 4-15% of gelling agent by mass, wherein the total mass is 100%. Uniformly mixing the powder in a cloth bag, adding the mixture into a granulator, and rolling until the particle size of the balls is 1-2 mm; the gelling agent is one of lime powder or cement;
(2) putting the catalyst carrier which is pelletized into balls with the diameter of 1-2 mm in the step (1) into a sealing bag and standing for 12-24 hours;
(3) roasting the catalyst carrier after standing in the step (2) in a kiln at 100-105 ℃ for 3-5 hours;
(4) taking out the carrier roasted in the step (3) and cooling to room temperature;
(5) preparing a metal active component salt into a solution with the mass concentration of 5-20% for later use, and mixing the solution with ammonium nitrate to obtain a mixed solution;
(6) soaking the carrier in the step (4) in the solution in the step (5), stirring at the speed of 60-100 rpm for 40-80 minutes, and then soaking for 3-5 hours;
(7) taking out the catalyst in the step (6), and roasting in a kiln at 100-105 ℃ for 3-5 h;
(8) and (3) continuously roasting the catalyst in the step (7) in a kiln at the temperature of 450-600 ℃ for 1-2 h, and introducing nitrogen with the volume of 2-10 of the catalyst to obtain the electrocatalytic oxidation catalyst for the landfill leachate.
The invention also aims to provide the application of the catalyst or the catalyst obtained by the preparation method in treating the landfill leachate concentrated solution.
Preferably, the specific treatment process may include: and adjusting the pH of the landfill leachate concentrated solution to 2-3, adding the catalyst, then carrying out electrocatalytic oxidation reaction, carrying out activated carbon adsorption on the obtained reaction supernatant, adjusting the pH of the effluent clear solution to 8-9, and finishing concentrated solution treatment, wherein the volume of the catalyst is 30-60% of that of the landfill leachate concentrated solution.
During the electrocatalytic oxidation reaction, the anode is a titanium-based plate, and the distance between anode plates is 15-20 mm; the cathode is made of 316L stainless steel plates, and the distance between the cathode plates is 15-20 mm.
The current density is 10-20 mA/cm2。
According to a preferred embodiment of the present invention, the processing may comprise: and (3) feeding the landfill leachate concentrated solution into an adjusting tank through a water inlet lifting pump, and adding hydrochloric acid to adjust the pH value of the landfill leachate concentrated solution to 2-3. And then the concentrated solution is lifted to the bottom of an electrocatalytic oxidation reactor by a pump, the reactor is filled with 30-60% by volume of the catalyst, after the reaction is finished, the supernatant enters an activated carbon adsorption reaction column for reaction for 10-30 min, the pH of the effluent is adjusted to 8-9 by 2-5% sodium hydroxide solution, and the supernatant enters a clear solution tank to finish the treatment of the concentrated solution.
The anode in the electrocatalytic oxidation reactor is a titanium-based plate, and the distance between the polar plates is 15-20 mm; the cathode is made of 316L stainless steel plates, and the distance between the polar plates is 15-20 mm;
the operating current density in the electrocatalytic oxidation reactor is 10-20 mA/cm2。
By adopting the technical scheme, the invention discloses an electrocatalytic oxidation catalyst for treating landfill leachate concentrated solution, a preparation method and application thereof, so that the electrocatalytic oxidation catalyst simultaneously has the following beneficial effects:
(1) aiming at the characteristics of macromolecular organic matters in the concentrated solution, an electrocatalytic oxidation catalyst for landfill leachate with high strength and high reaction rate is developed, so that the power consumption in the reaction is greatly reduced;
(2) the method fully utilizes the characteristic of high chloride ion concentration in the concentrated solution, realizes harmlessness and recycling by adopting an electrocatalytic oxidation process, and does not need to additionally add any medicament;
(3) the water quality control device has the characteristic of strong load impact resistance, and can adapt to the fluctuation of the water quantity and the water quality of tap water;
(4) stable operation, high organic matter removing efficiency, low operation cost and good effluent quality.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The starting materials used in the embodiments of the present invention are commercially available.
Example 1:
the preparation method of the electrocatalytic oxidation catalyst for landfill leachate specifically comprises the following steps:
(1) weighing 70% of alumina powder, 20% of activated carbon powder and 10% of gelling agent by mass, wherein the total mass is 100%. Mixing the above powder in cloth bag, adding into granulator, and rolling until the particle size of the ball is 1mm, wherein the gelatinizer is lime powder;
(2) putting the catalyst carrier which is pelletized to 1mm in the step (1) into a sealing bag and standing for 12 hours;
(3) roasting the catalyst carrier which is kept stand in the step (2) in a kiln at the temperature of 100 ℃ for 3 hours;
(4) taking out the carrier roasted in the step (3) and cooling to room temperature;
(5) respectively preparing copper nitrate and lanthanum nitrate into solutions with mass concentration of 8%, and mixing the solutions with ammonium nitrate to obtain a mixed solution, wherein the mass of the copper nitrate and the mass of the lanthanum nitrate are respectively 4.3% and 4.3% of the total amount of the carrier;
(6) soaking the carrier in the step (4) in the solution in the step (5) and stirring at the speed of 80 rpm for 50 minutes for 4 hours;
(7) taking out the catalyst in the step (6), and putting the catalyst in a kiln at 100 ℃ for roasting for 3 hours;
(8) and (3) continuously roasting the catalyst in the step (7) in a kiln at 450 ℃ for 2h, wherein nitrogen with the volume twice that of the catalyst is introduced to obtain the electrocatalytic oxidation catalyst for the landfill leachate, wherein the copper content is 1.46 wt% of the total weight of the carrier, and the lanthanum content is 1.84 wt% of the total weight of the carrier.
And (3) feeding the landfill leachate concentrated solution into an adjusting tank through a water inlet lifting pump, and adding hydrochloric acid to adjust the pH value of the landfill leachate concentrated solution to 3. And then the concentrated solution is lifted to the bottom of an electrocatalytic oxidation reactor by a pump, the reactor is filled with a catalyst with the volume of 30% of the concentrated solution, after the reaction is finished, the supernatant enters an activated carbon adsorption reaction column for reaction for 15min, the pH of the effluent is adjusted to 8-9 by 2% -5% sodium hydroxide solution, and the supernatant enters a clear solution tank to finish the treatment of the concentrated solution.
The anode in the electrocatalytic oxidation reactor is a titanium-based plate, and the distance between the polar plates is 15 mm; the cathode is made of 316L stainless steel plates, and the distance between the polar plates is 15 mm;
the operating current density in the electrocatalytic oxidation reactor is 10mA/cm2；
Example 2:
the preparation method of the electrocatalytic oxidation catalyst for landfill leachate specifically comprises the following steps:
(1) weighing 60% of alumina powder, 30% of activated carbon powder and 10% of gelling agent by mass, wherein the total mass is 100%. Mixing the above powder in cloth bag, adding into granulator, and rolling until the particle size of the ball is 2mm, wherein the gelatinizer is cement;
(2) putting the catalyst carrier which is pelletized into 2mm in the step (1) into a sealing bag and standing for 12 hours;
(3) roasting the catalyst carrier which is kept stand in the step (2) in a kiln at 105 ℃ for 4 hours;
(4) taking out the carrier roasted in the step (3) and cooling to room temperature;
(5) respectively preparing copper nitrate and lanthanum nitrate into solutions with mass concentration of 5%, and mixing the solutions with ammonium nitrate to obtain a mixed solution, wherein the mass of the copper nitrate and the mass of the lanthanum nitrate are respectively 2.1% and 3.2% of the total amount of the carrier;
(6) soaking the carrier in the step (4) in the solution in the step (5) and stirring at the speed of 100 revolutions per minute for 60 minutes for 3 hours;
(7) taking out the catalyst in the step (6), and putting the catalyst in a kiln at 105 ℃ for roasting for 3 hours;
(8) and (3) continuously roasting the catalyst in the step (7) in a kiln at 550 ℃ for 1h, wherein nitrogen with the volume twice that of the catalyst is introduced to obtain the electrocatalytic oxidation catalyst for the landfill leachate, wherein the copper content is 0.71 wt% of the total weight of the carrier, and the lanthanum content is 1.37 wt% of the total weight of the carrier.
And (3) feeding the landfill leachate concentrated solution into an adjusting tank through a water inlet lifting pump, and adding hydrochloric acid to adjust the pH value of the landfill leachate concentrated solution to 3. And then the concentrated solution is lifted to the bottom of an electrocatalytic oxidation reactor by a pump, the reactor is filled with the catalyst with the volume of 30% of the concentrated solution, after the reaction is finished, the supernatant enters an activated carbon adsorption reaction column for reaction for 30min, the pH of the effluent is adjusted to 8-9 by 2% -5% sodium hydroxide solution, and the supernatant enters a clear solution tank to finish the treatment of the concentrated solution.
The anode in the electrocatalytic oxidation reactor is a titanium-based plate, and the distance between the polar plates is 15 mm; the cathode is made of 316L stainless steel plates, and the distance between the polar plates is 15 mm;
the operating current density in the electrocatalytic oxidation reactor is 15mA/cm2。
The concentrated solution is high-difficulty organic wastewater which is generated after NF and RO processes in the process of treating the landfill leachate and is difficult to biochemically degrade. The biomass fuel contains a large amount of organic matters, the main components of the biomass fuel are benzene series, chain hydrocarbon, acid and ester organic matters, the COD is 100-3500 mg/L, the biodegradability is poor, the BOD/COD is less than 10, the ammonia nitrogen content is 100-150 mg/L, and the chroma is generally 500-1500 times. After the electrocatalytic oxidation process is used for treatment, the effluent quality can reach the indexes shown in the following table 1:
Claims (10)
1. an electrocatalytic oxidation catalyst for landfill leachate comprises a carrier and a metal active component, wherein the metal active component comprises copper and one or two of lanthanum or nickel;
the metal active component accounts for 1-11 wt% of the total weight of the carrier, and preferably 1.5-6 wt%.
2. The electrocatalytic oxidation catalyst for landfill leachate according to claim 1, wherein:
the carrier is an alumina/activated carbon carrier, and the particle size of the carrier is preferably 1-2 mm.
3. The electrocatalytic oxidation catalyst for landfill leachate according to claim 2, wherein:
the alumina/activated carbon carrier is prepared from components including alumina, activated carbon and a gelling agent, wherein based on the total weight of the carrier: 50-70 wt% of aluminum oxide, 15-30 wt% of activated carbon and 4-15 wt% of gelling agent.
4. The electrocatalytic oxidation catalyst for landfill leachate according to claim 3, wherein:
the gelling agent is at least one of lime or cement.
5. A method for preparing the electrocatalytic oxidation catalyst for landfill leachate according to any one of claims 1 to 4, characterized by comprising the following steps:
preparing a mixed solution of metal active component salt and ammonium nitrate, soaking a carrier in the mixed solution, roasting, and treating with nitrogen to obtain the catalyst;
the metal active ingredient salt is preferably a nitrate salt of the metal active ingredient.
6. The method for preparing the electrocatalytic oxidation catalyst for landfill leachate according to claim 5, wherein the method comprises the following steps:
the amount of the metal active component salt is 5-25 wt% of the carrier, preferably 5-12 wt%.
7. The method for preparing the electrocatalytic oxidation catalyst for landfill leachate according to claim 5, wherein the method comprises the following steps:
when the carrier is soaked, stirring at the speed of 60-100 rpm for 40-80 min, and then soaking for 3-5 h; and/or the presence of a gas in the gas,
roasting for 3-5 h at 100-105 ℃ and for 1-2 h at 450-600 ℃; and/or the presence of a gas in the gas,
and (3) carrying out nitrogen treatment when roasting is carried out at the temperature of 450-600 ℃, and introducing nitrogen with the volume 2-10 times that of the catalyst.
8. Use of a catalyst according to any one of claims 1 to 4 or obtained by a method according to any one of claims 5 to 7 for the treatment of a landfill leachate concentrate.
9. Use of a catalyst according to claim 8 for the treatment of a landfill leachate concentrate, characterized in that:
and adjusting the pH of the landfill leachate concentrated solution to 2-3, adding the catalyst, then carrying out electrocatalytic oxidation reaction, carrying out activated carbon adsorption on the obtained reaction supernatant, adjusting the pH of the effluent clear solution to 8-9, and finishing concentrated solution treatment, wherein the volume of the catalyst is 30-60% of that of the landfill leachate concentrated solution.
10. Use of a catalyst according to claim 8 for the treatment of a landfill leachate concentrate, characterized in that:
during the electrocatalytic oxidation reaction, the anode is a titanium-based plate, and the distance between anode plates is 15-20 mm; the cathode is a 316L stainless steel plate, and the distance between cathode plates is 15-20 mm;
the current density is 10-20 mA/cm2。
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