CN109465014B - Double-effect catalyst capable of regulating and controlling decomposition rate of ozone and hydrogen peroxide, preparation method and application thereof - Google Patents
Double-effect catalyst capable of regulating and controlling decomposition rate of ozone and hydrogen peroxide, preparation method and application thereof Download PDFInfo
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- 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
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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Abstract
The invention discloses a double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide, which is of a core-shell structure, wherein a core is aluminum oxide loaded with manganese, and a shell is aluminum oxide loaded with iron oxyhydroxide, wherein the content of manganese is 5-10 wt% based on the aluminum oxide loaded with manganese, the content of iron is 5-10 wt% based on the aluminum oxide loaded with iron oxyhydroxide, and the mass ratio of the aluminum oxide loaded with manganese to the aluminum oxide loaded with iron oxyhydroxide is 10: 1-1: 1. the preparation method of the catalyst is simple and can realize large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide, and a preparation method and application thereof.
Background
The advanced oxidation technology is a main means for treating the degradation-resistant wastewater due to strong oxidation capability, high pollutant removal rate and stable process operation. The ozone catalytic oxidation technology is used as an advanced oxidation technology which is efficient, practical and free of secondary pollution, and is applied to the aspect of treating refractory wastewater in an engineering way.
With the improvement of the emission standard, the single ozone catalytic oxidation technology has met the bottleneck, and the Chemical Oxygen Demand (COD) of a lot of waste water after the ozone catalytic oxidation treatment still can not reach the emission standard. Therefore, the technology is combined with methods such as hydrogen peroxide, light, ultrasound, microwave and the like, such as O3/H2O2、UV/O3Ultrasonic catalytic ozonation, microwave catalytic ozonation and other composite catalytic oxidation technologies.
However, the combination of ozone and electrochemical technology is less studied, and the electrochemical technology is a clean advanced oxidation technology, however, the conventional electrochemical technology only utilizes anodic oxidation to degrade pollutants, and the cathode generally generates hydrogen evolution reaction. Moreover, ozone is typically produced by ozone generators in an amount not exceeding 10%, with the remaining about 90% of the high purity oxygen being discharged directly into the atmosphere, all the while being pitot. In an electrochemical reactor, oxygen can be converted into hydrogen peroxide through a reduction reaction at a cathode, the hydrogen peroxide has certain oxidizing power, but the oxidizing power is not strong enough, the hydrogen peroxide can be further converted into hydroxyl radicals with stronger oxidizing power by adding a heterogeneous Fenton catalyst, the reaction rate of hydrogen peroxide decomposition is slow usually, the ozone decomposition rate is fast, so that substances which can be oxidized after ozone and hydrogen peroxide are decomposed cannot be decomposed due to slow hydrogen peroxide decomposition in a sewage treatment reactor, and only ozone plays an oxidizing role in the reactor, so that the decomposition rates of the hydrogen peroxide and the ozone need to be balanced, and the problem needs to be solved.
Disclosure of Invention
In order to solve the problems, the invention discloses a double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide, a preparation method and application thereof.
The invention provides a double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide, which is of a core-shell structure, wherein a core is aluminum oxide loaded with manganese, and a shell is aluminum oxide loaded with iron oxyhydroxide, wherein the content of manganese is 5-10 wt% based on the aluminum oxide loaded with manganese, the content of iron is 5-10 wt% based on the aluminum oxide loaded with iron oxyhydroxide, and the mass ratio of the aluminum oxide loaded with manganese to the aluminum oxide loaded with iron oxyhydroxide is 10: 1-1: 1.
the shell of the double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide has a thickness of 10-100 mu m, and the equivalent diameter of the core is 2-5 mm.
The shell of the double-effect catalyst capable of regulating the decomposition rate of the ozone and the hydrogen peroxide is of a porous structure, the average pore diameter is 0.2-2 microns, when wastewater passes through the catalyst layer, the wastewater is firstly diffused to the shell, the hydrogen peroxide generates catalytic decomposition reaction, when the wastewater is further diffused to a reaction core, the ozone generates catalytic decomposition reaction, and the rate of the two reactions is regulated and controlled through the thickness of the shell.
The double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide can be used for treating refractory sewage generated in various fields such as coking wastewater, refining wastewater, medical wastewater, printing and dyeing wastewater, garbage percolate, pesticide wastewater and the like.
The second aspect of the invention provides a preparation method of a double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide, which comprises the following steps:
(1) preparation of manganese-loaded alumina: selecting an alumina pellet with the diameter of 3-5 mm as a catalyst carrier, cleaning, drying, soaking in a manganese-containing solution, drying, and roasting to obtain a manganese-loaded alumina pellet;
(2) preparation of aluminum hydroxide slurry: dissolving aluminum hydroxide powder in a solvent, wherein the solvent is water and ethanol, the volume ratio of the ethanol to the water is 1: 1-1: 3, and the content of the aluminum hydroxide is 10-25 wt%;
(3) uniformly mixing iron oxyhydroxide powder with the aluminum hydroxide slurry prepared in the step (2) to prepare iron oxyhydroxide-loaded aluminum oxide mixed slurry, wherein the iron element content is 5-6 wt%;
(4) spraying and soaking the mixed slurry prepared in the step (3) into the manganese-loaded alumina balls, and controlling the mass ratio of the manganese-loaded alumina to the iron oxyhydroxide-loaded alumina to be 10: 1-1: 1, and drying and roasting to obtain the double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide.
In the preparation method of the double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide, in the step (1), the cleaning times are 2 times, the drying temperature is 120 ℃, the drying time is 2 hours, the catalyst is soaked in a manganese-containing solution for 12 hours, the drying temperature is 120 ℃, the drying time is 2 hours, the roasting temperature is 500 ℃, and the roasting time is 4 hours, so that the manganese-loaded alumina pellets are obtained.
According to the preparation method of the double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide, in the step (4), the drying temperature is 80-120 ℃, the drying time is 2-12 hours, the roasting temperature is 350-550 ℃, and the roasting time is 2-4 hours.
The third aspect of the invention provides application of a double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide, which can be used for catalytically oxidizing refractory wastewater.
The invention has the beneficial effects that:
1. the catalyst carrier adopted by the invention is alumina and modified products thereof, and the cost of raw materials is low.
2. According to the invention, through the structural design of the shell and the core, the shell is a hydrogen peroxide catalyst layer, the core is an ozone catalyst layer, the ozone catalyst layer with a high oxidation rate is used as the core, and the hydrogen peroxide catalyst layer with a low oxidation decomposition rate is used as the shell, so that sewage firstly contacts the hydrogen peroxide catalyst, the oxidation decomposition rate of the hydrogen peroxide is accelerated, the oxidation decomposition rate of ozone is reduced, meanwhile, the reaction rate of two reactions can be effectively regulated and controlled by controlling the thickness of the shell, the decomposition of an ineffective oxidant is avoided, and the utilization efficiency of the oxidant is improved.
3. The catalyst can be independently used for an ozone catalytic oxidation system or a Fenton oxidation system, and can also be used for a composite advanced oxidation system simultaneously containing ozone and hydrogen peroxide.
4. The preparation method of the catalyst is simple and can realize large-scale industrial production.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, steps, structures, characteristics and effects according to the present invention is provided in conjunction with the preferred embodiments, but the scope of the present invention is not limited by the following contents.
Example 1
1. A preparation method of a double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide comprises the following steps:
(1) preparing manganese oxide loaded gamma-alumina:
selecting gamma-alumina pellets with the diameter of 3-5 mm as a catalyst carrier, cleaning the catalyst carrier for 3 times by using clear water, drying the catalyst carrier for 2 hours at 120 ℃, soaking the catalyst carrier in a 1mol/L manganese nitrate solution for 24 hours, drying the catalyst carrier for 2 hours in a drying oven at 120 ℃, and roasting the catalyst carrier for 4 hours at 400 ℃ to obtain the gamma-alumina pellets loaded with manganese oxide.
(2) Preparation of aluminum hydroxide slurry: dissolving aluminum hydroxide powder in a solvent, wherein the solvent is water and ethanol, the volume ratio of the ethanol to the water is 1:1, and the content of the aluminum hydroxide is 10 wt%;
(3) preparation of mixed slurry:
uniformly mixing iron oxyhydroxide powder and aluminum hydroxide slurry, controlling the content of iron element to be 6 wt%, preparing mixed slurry,
(4) and (4) spraying and soaking the mixed slurry prepared in the step (3) into the manganese-loaded alumina balls, controlling the mass ratio of the manganese-loaded alumina to the iron oxyhydroxide-loaded alumina to be 5:1, drying and roasting to obtain the double-effect catalyst of ozone and hydrogen peroxide, wherein the drying temperature is 100 ℃, the drying time is 2 hours, the roasting temperature is 450 ℃, and the roasting time is 4 hours, so as to finally obtain the catalyst.
The prepared catalyst is added into an ozone/electrochemical synergetic catalytic oxidation wastewater treatment device to treat biochemical effluent of certain pig raising wastewater, and the experimental conditions are as follows:
the adding amount of the catalyst is 1000g, the ozone reaction is carried out for continuous aeration, the ozone flow is 2.4L/h, the ozone concentration is 100-120 mg/L, the water inlet flow is 1L/h, a direct current power supply is adopted, and the voltage is 3-4V. Initial water quality index of wastewater: CODCr126.0mg/L and 80 times of chroma; COD in the treated waterCrThe removal rate of (2) is 85.0%, and the removal rate of chroma is 90.0%; the concentration of ozone at the water outlet is 0.52mg/L, and the concentration of hydrogen peroxide is 1.2 mg/L.
Comparative example 1
This comparative example differs from example 1 in that: mixing a gamma-alumina catalyst loaded with manganese oxide and an alumina catalyst loaded with iron oxyhydroxide into a double-effect catalyst mixture with a non-core-shell structure, and treating biochemical effluent of the pig wastewater in the example 1; COD of treated waterCrThe removal rate of (2) is 63% and the removal rate of chromaticity is 82%; the concentration of ozone at the water outlet is 0.23mg/L, and the concentration of hydrogen peroxide is 8.9 mg/L.
Example 2
1. A preparation method of a double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide comprises the following steps:
(1) preparing manganese oxide loaded beta-alumina:
selecting beta-alumina pellets with the diameter of 3-5 mm as a catalyst carrier, washing the catalyst carrier for 2 times by using clear water, drying the catalyst carrier for 2 hours at 120 ℃, soaking the catalyst carrier in a 1mol/L manganese acetate solution for 24 hours, drying the catalyst carrier for 2 hours in a drying oven at 120 ℃, and roasting the catalyst carrier for 4 hours at 400 ℃ to obtain the manganese oxide-loaded beta-alumina pellets.
(2) Preparation of aluminum hydroxide slurry:
dissolving aluminum hydroxide powder in a solvent, wherein the solvent is water and ethanol, the volume ratio of the ethanol to the water is 1:2, and the content of the aluminum hydroxide is 15 wt%;
(3) preparation of mixed slurry:
uniformly mixing iron oxyhydroxide powder and aluminum hydroxide slurry, controlling the content of iron element to be 6 wt%, preparing mixed slurry,
(4) and (4) spraying and soaking the mixed slurry prepared in the step (3) into the manganese-loaded alumina balls, controlling the mass ratio of the manganese-loaded alumina to the iron oxyhydroxide-loaded alumina to be 10:1, drying and roasting to obtain the double-effect catalyst of ozone and hydrogen peroxide, wherein the drying temperature is 100 ℃, the drying time is 2 hours, the roasting temperature is 350 ℃, and the roasting time is 4 hours, so as to finally obtain the catalyst.
The prepared catalyst is added into an ozone catalytic oxidation reactor to treat biochemical effluent of certain coking wastewater, and the experimental conditions are as follows:
the catalyst dosage is 1000g, the addition amount of hydrogen peroxide is 60mg/L, the catalyst is added into the inlet water at one time, the inlet water flow is 1L/h, the ozone reaction is continuously aerated, and the addition amount of ozone is 120 mg/L. Initial water quality index of wastewater: CODCr202mg/L and 80 times of chroma; COD of treated waterCrThe removal rate of (a) is 82.0%, and the removal rate of the chromaticity is 90.0%; the concentration of ozone at the water outlet is 0.52mg/L, and the concentration of hydrogen peroxide is 1.5 mg/L.
Comparative example 2
This comparative example differs from example 2 in that: mixing a manganese oxide-loaded beta-alumina catalyst and a ferric oxyhydroxide-loaded alumina catalyst into a double-effect catalyst mixture with a non-core-shell structure, and treating the coking wastewater biochemical effluent in the embodiment 2; COD of treated waterCrThe removal rate of (2) was 61%, and the removal rate of chroma was 83%; the concentration of ozone at the water outlet is 0.28mg/L, and the concentration of hydrogen peroxide is 10.8 mg/L.
Example 3
1. A preparation method of a double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide comprises the following steps:
(1) preparing manganese oxide loaded alpha-alumina:
selecting alpha-alumina pellets with the diameter of 3-5 mm as a catalyst carrier, washing the catalyst carrier for 2 times by using clear water, drying the catalyst carrier for 2 hours at 120 ℃, soaking the catalyst carrier in a 1mol/L manganese acetate solution for 24 hours, drying the catalyst carrier for 2 hours in a drying oven at 120 ℃, and roasting the catalyst carrier for 4 hours at 400 ℃ to obtain the alpha-alumina pellets loaded with manganese oxide;
(2) preparation of aluminum hydroxide slurry: dissolving aluminum hydroxide powder in a solvent, wherein the solvent is water and ethanol, the volume ratio of the ethanol to the water is 1:3, and the content of the aluminum hydroxide is 25 wt%;
(3) preparation of mixed slurry:
uniformly mixing iron oxyhydroxide powder and aluminum hydroxide slurry, controlling the content of iron element to be 6 wt%, preparing mixed slurry,
(4) and (4) spraying and soaking the mixed slurry prepared in the step (3) into the manganese-loaded alumina balls, controlling the mass ratio of the manganese-loaded alumina to the iron oxyhydroxide-loaded alumina to be 10:1, drying and roasting to obtain the double-effect catalyst of ozone and hydrogen peroxide, wherein the drying temperature is 100 ℃, the drying time is 2 hours, the roasting temperature is 350 ℃, and the roasting time is 4 hours, so as to finally obtain the catalyst.
The prepared catalyst is added into an ozone catalytic oxidation reactor to treat biochemical effluent of certain printing and dyeing wastewater, and the experimental conditions are as follows:
the catalyst dosage is 1000g, the addition amount of hydrogen peroxide is 30mg/L, the catalyst is added into the inlet water at one time, the inlet water flow is 1L/h, the ozone reaction is continuously aerated, and the addition amount of ozone is 60 mg/L. Initial water quality index of wastewater: CODCr94mg/L and 64 times of chroma; COD of treated waterCrThe removal rate of (a) is 65.0%, and the removal rate of chromaticity is 80.0%; the concentration of ozone at the water outlet is 0.32mg/L, and the concentration of hydrogen peroxide is 0.30 mg/L.
Comparative example 3
This comparative example differs from example 3 in that: mixing an alpha-alumina catalyst loaded with manganese oxide and an alumina catalyst loaded with iron oxyhydroxide into a double-effect catalyst mixture with a non-core-shell structure, and treating biochemical effluent of the printing and dyeing wastewater in example 3; COD of treated waterCrThe removal rate of (a) is 42%, and the removal rate of chromaticity is 68%; the concentration of ozone at the water outlet is 0.15mg/L, and the concentration of hydrogen peroxide is 6.3 mg/L.
As can be seen from 3 embodiments and comparative examples thereof, by adopting the designed double-effect catalyst with the core-shell structure, the problems of high ozone oxidative decomposition rate and low hydrogen peroxide oxidative decomposition rate in the sewage treatment process are effectively balanced, the utilization rate of hydrogen peroxide in the sewage treatment device is improved, and the probability of the ozone and the hydrogen peroxide for synergistically oxidizing the compounds difficult to oxidize is improved.
Claims (5)
1. The double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide is characterized by being of a core-shell structure, a core is aluminum oxide loaded with manganese, and a shell is aluminum oxide loaded with iron oxyhydroxide, wherein the content of manganese is 5-10 wt% based on the aluminum oxide loaded with manganese, the content of iron is 5-10 wt% based on the aluminum oxide loaded with iron oxyhydroxide, and the mass ratio of the aluminum oxide loaded with manganese to the aluminum oxide loaded with iron oxyhydroxide is 10: 1-1: 1;
the shell is a porous structure, and the average pore diameter is 0.2-2 μm.
2. The dual-purpose catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide as claimed in claim 1, wherein the thickness of the shell is 10 μm to 100 μm, and the equivalent diameter of the core is 2mm to 5 mm.
3. A preparation method of a double-effect catalyst capable of regulating and controlling the decomposition rate of ozone and hydrogen peroxide is characterized by comprising the following steps:
(1) preparation of manganese-loaded alumina: selecting an alumina pellet with the diameter of 3-5 mm as a catalyst carrier, cleaning, drying, soaking in a manganese-containing solution, drying, and roasting to obtain a manganese-loaded alumina pellet;
(2) preparation of aluminum hydroxide slurry: dissolving aluminum hydroxide powder in a solvent, wherein the solvent is water and ethanol, the volume ratio of the ethanol to the water is 1: 1-1: 3, and the content of the aluminum hydroxide is 10-25 wt%;
(3) uniformly mixing iron oxyhydroxide powder with the aluminum hydroxide slurry prepared in the step (2) to prepare iron oxyhydroxide-loaded aluminum oxide mixed slurry, wherein the iron element content is 5-6 wt%;
(4) spraying and soaking the mixed slurry prepared in the step (3) into the manganese-loaded alumina balls, and controlling the mass ratio of the manganese-loaded alumina to the iron oxyhydroxide-loaded alumina to be 10: 1-1: 1, and drying and roasting to obtain the double-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide.
4. The preparation method of the dual-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide is characterized in that in the step (4), the drying temperature is 80-120 ℃, the drying time is 2-12 hours, the roasting temperature is 350-550 ℃, and the roasting time is 2-4 hours.
5. Use of the dual-effect catalyst capable of regulating the decomposition rate of ozone and hydrogen peroxide according to claim 1 for catalytic oxidation of refractory wastewater containing cyanide, phenol, nitrogen-containing heterocycle, oxygen-containing heterocycle, sulfur-containing heterocycle, polycyclic aromatic hydrocarbon, or humic acid.
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| CN116020462A (en) * | 2021-10-26 | 2023-04-28 | 中国石油化工股份有限公司 | Ozone catalytic oxidation catalyst and its preparation method and wastewater treatment method |
| CN118847116B (en) * | 2024-09-25 | 2024-12-24 | 苏州大学 | A composite active aluminum-based ozone oxidation catalyst and its preparation method and application |
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