CN108046407B - Adopts nano-CeO2/H2O2/O3Method for treating acidic degradation-resistant wastewater by system - Google Patents
Adopts nano-CeO2/H2O2/O3Method for treating acidic degradation-resistant wastewater by system Download PDFInfo
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- CN108046407B CN108046407B CN201711110906.9A CN201711110906A CN108046407B CN 108046407 B CN108046407 B CN 108046407B CN 201711110906 A CN201711110906 A CN 201711110906A CN 108046407 B CN108046407 B CN 108046407B
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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
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F1/722—Oxidation by peroxides
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
Abstract
The invention discloses a method for treating acidic wastewater by heterogeneous catalysis of ozone and hydrogen peroxide. The catalyst is synthesized by adopting a high-temperature nitrate decomposition method. The solid catalyst used in X-ray diffraction analysis (XRD) contains cerium dioxide, and X-ray photoelectron spectroscopy (XPS) analysis proves that Ce is simultaneously present in the catalyst3+And Ce4+. The catalyst is a nanosphere agglomerate when the shape of the catalyst is observed by a Scanning Electron Microscope (SEM). The catalyst synthesized by the method is used for heterogeneous catalysis of ozone hydrogen peroxide to oxidize refractory organic matters (such as acetic acid) in acidic water, and shows good activity. Compared with the prior art, the solid catalyst prepared by the invention has the advantages of simple preparation, low production cost, high catalytic activity and higher application value.
Description
(I) technical field
The invention relates to the field of wastewater treatment, in particular to a method for preparing nano-CeO2/H2O2/O3A method for treating acidic degradation-resistant wastewater by a system.
With nano-CeO2/H2O2/O3The system efficiently treats the pollutants which are difficult to degrade in the acidic wastewater, and particularly, the pollutants which are difficult to degrade in the acidic wastewater are treated by catalytic ozonization by using nano cerium oxide as a catalyst.
(II) background of the invention
Since the 21 st century, with the development of industrialization and urbanization, the environment pollution situation is more and more severe, and the problems of industrial waste water, urban domestic sewage, river and lake pollution and the like have great influence on national economic development, ecological environment and human health. Most of the wastewater contains difficultly-degraded biological pollutants such as polycyclic aromatic hydrocarbon, halogenated hydrocarbon, heterocyclic compounds, organic pesticides and the like, and the traditional biochemical method is very difficultAnd (6) processing. Advanced Oxidation Processes (AOPs) are one of the most promising methods for treating organic refractory wastewater today. Including Fenton (H)2O2/Fe2+) Fenton-like, ozone advanced oxidation process (hereinafter referred to as AOP-O)3) Persulfate advanced oxidation technology and the like.
The ozone advanced oxidation technology has the advantages of greenness, high efficiency, no secondary pollution and the like, and has good application prospect in the aspect of sewage treatment. Most unsaturated and macromolecular aromatic organic substances can directly react with ozone, but are accompanied by the generation of a large amount of by-products such as organic small molecular acid and the like, and the by-products are difficult to be directly oxidized by ozone. Selecting appropriate catalyst such as transition metal oxide CuO, MnO2、TiO2、Fe2O3Catalyzing ozone to generate hydroxyl radical (. OH) with higher oxidation is the core content of the current research on ozone advanced oxidation. Ozone is relatively prone to generate hydroxyl radicals under alkaline conditions, however, due to the generation of organic acids, the solution tends to become acidic as the reaction proceeds such that the rate of degradation decreases and even terminates. The ozone and hydrogen peroxide coupling technology makes it possible for ozone to decompose and produce hydroxyl radical under acid condition. But the efficiency is still low.
Heterogeneous catalysis of H in recent years2O2/O3The system is one of the hot spots in research. Titanium lewis acids, titanium silicalite (TS-1) and solid super acids (SZF) are several catalysts that we have discovered in the past year that are highly efficient. No studies on cerium oxide in this regard have been reported. This work prepared nano-cerium oxide and found it to catalyze H2O2/O3The system has good removal effect on the small molecular acid which is difficult to degrade under the acidic condition.
Disclosure of the invention
The invention aims to overcome the defect that the existing ozone is difficult to degrade acidic wastewater, and provides a wastewater treatment method which can efficiently catalyze ozone to generate hydroxyl radicals under an acidic condition (pH is less than or equal to 5) and degrade difficult-to-degrade organic small molecular acid. The method is expected to solve the problem that the acid wastewater is difficult to treat in the field of environmental water treatment.
Adopts nano-CeO2/H2O2/O3The method for treating the acidic degradation-resistant wastewater by the system comprises the following steps:
(1) adding nano-CeO into acidic wastewater containing organic pollutants and having pH of 1-52Solid catalyst and H2O2Stirring uniformly to obtain a mixed solution; the organic pollutants are one or a mixture of more of monocyclic and polycyclic aromatic compounds, heterocyclic compounds, aliphatic hydrocarbons and derivatives thereof; the organic contaminant H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 0.5-4: 0.2-3;
(2) and (3) introducing ozone into the mixed solution for degradation reaction to obtain degraded wastewater.
H2O2/O3The system has low degradation rate of organic pollutants under acidic condition, nano-CeO2Is added to greatly improve H2O2/O3The system has degradation rate to organic pollutants under acidic condition.
Nano-CeO of the invention2/H2O2/O3The system has higher degradation activity on acidic degradation-resistant wastewater; the acidic degradation-resistant wastewater contains organic pollutants which are difficult to treat by other ozone advanced oxidation technologies, and is preferably micromolecular organic acid wastewater in aliphatic hydrocarbon derivatives; the small-molecule organic acid is preferably acetic acid.
In the embodiment of the invention, the small molecular organic acid-acetic acid which is difficult to treat is adopted as the organic pollutant, and when the acetic acid is degraded by adopting the method, the action mechanism is that the acetic acid is usually taken as a byproduct in the degradation process of the large molecular organic pollutant, the property is stable, and generally, only the hydroxyl radical with super-strong oxidizability can oxidize and decompose the acetic acid. In general, if acetic acid can be effectively degraded, it is considered that other organic pollutants, such as macromolecular organic substances of aliphatic, aromatic, etc., can also be effectively and highly degraded.
For degrading waste water containing organic pollutants of unknown concentration, the waste water is first measuredThe COD value can be used for estimating the quality of the organic wastewater contained in the wastewater according to the COD value of the wastewater, thereby determining the H required to be added2O2And nano-CeO2And (4) adding the solid catalyst.
Preferably, the nano-CeO2The solid catalyst is nano cerium oxide synthesized by taking cerous nitrate hexahydrate as a precursor and adopting a high-temperature thermal decomposition method.
Further preferably, the nano-CeO2The preparation method of the solid catalyst comprises the following steps:
(a) weighing cerous nitrate hexahydrate, putting the cerous nitrate hexahydrate in a ceramic boat, putting the ceramic boat in a muffle furnace, and heating the ceramic boat at the temperature of 10 ℃ for min in the air atmosphere-1The temperature rising rate is increased to 550 ℃ and calcined for 4 hours to obtain a light yellow solid;
(b) fully grinding the light yellow solid in the step (a) to obtain nano-CeO2A solid catalyst.
Preferably, in the mixed solution of step (1), organic contaminants, H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 0.5-4: 0.2-3; further preferably, the organic contaminant H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 1-4: 0.8-1.6; most preferably, organic contaminant, H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 2-4: 0.8.
Preferably, in step (2), the ozone is O2/O3Introducing mixed gas in a form of flow rate of 0.1-0.6 L.min-1Wherein the concentration of ozone is 1.4-39.2 mg.L-1。
Compared with the prior art, the wastewater treatment method has the following advantages:
(1) the acidic degradation-resistant wastewater can be efficiently degraded under an acidic condition (pH is less than or equal to 5), the utilization rate of ozone can be increased, organic pollutants in the acidic wastewater can be completely removed, and secondary pollution of byproducts is avoided;
(2)nano-CeO2the solid catalyst has simple preparation, low synthesis cost, high catalytic efficiency, high ozone utilization rate and less ozoneThe addition amount can realize good degradation effect, and the catalytic application prospect is excellent.
(IV) description of the drawings
FIG. 1 is a diagram of an experimental apparatus for degrading acetic acid in water by catalytic ozonation in the example; in the figure, 1-oxygen cylinder, 2-ozone generator, 3-flowmeter, 4-ozone reactor, 5-recirculated cooling water outlet, 6-feed inlet, 7-sampling port, 8-recirculated cooling water inlet, 71-ozone absorber, 72-ozone absorber, 9-discharge outlet, 10.1, 10.2-ozone absorber.
FIG. 2 is nano-CeO2XRD characterization pattern of the solid catalyst;
FIG. 3 is nano-CeO2SEM characterization of solid catalyst;
FIG. 4 is nano-CeO2XPS profile of solid catalyst;
FIG. 5 is a graph showing comparative results of different catalysts under the same conditions.
FIG. 6 is CeO2The effect of catalyzing different systems to degrade acetic acid is shown.
FIG. 7 is a graph comparing the amount of hydroxyl radicals generated in different systems.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
The following examples all used the apparatus shown in FIG. 1 for wastewater treatment, which includes an oxygen cylinder 1, an ozone generator 2, a flow meter 3, an ozone reactor 4, ozone absorbing devices 10.1, 10.2, and an ozone destructor 11. Oxygen steel bottle 1, ozone generator 2, flowmeter 3, ozone reactor 4, ozone absorbing device 10.2, ozone destructor 11 pass through the pipeline and connect gradually series connection, the connecting line between flowmeter 3 and the ozone reactor 4 is equipped with the two-way valve, another route of two-way valve is connected with another ozone absorbing device 10.1. The ozone reactor 4 is provided with a circulating cooling water inlet 8 and a cooling water outlet 5 which are communicated with circulating cooling water, and the ozone reactor 4 is also provided with a feeding hole 6 at the upper part and a sampling hole 7 and a discharging hole 9 at the lower part. The ozone absorbing means 10.1, 10.2 take the most common form of two or more connected test tubes or other containers filled with a 2% KI solution. The ozone generator is CFS-1A, the destructor is ODF-003, the contact material is 316L stainless steel, the ozone reactor is made of common glass, the inner diameter is 5cm, the height is 75cm, a sand core at the bottom of the ozone reactor is a gas stepping device, and silica gel tubes are adopted as connecting pipelines.
Before reaction, the ozone reactor is cleaned by secondary deionized water, pretreated by ozone for 5min, and after emptying, the reactor is flushed twice by secondary deionized water. The wastewater solution to be treated is prepared by deionized water and is placed in an ozone reactor 4, and a proper amount of catalyst is added into the ozone reactor 4. During the reaction, oxygen flowing out of the oxygen cylinder 1 is used as raw material gas, ozone is generated by an ozone generator, and O is obtained2/O3Mixing gas, controlling ozone concentration by regulating discharge power and gas flow of ozone generator, opening two-way valve connected with ozone reactor, and opening O2/O3The mixed gas enters a reactor to react with the wastewater, the wastewater is degraded, and O passes through an ozone reactor2/O3The mixed gas leaves from the top of the reactor, passes through an ozone absorption device 10.2 and an ozone destructor 11 and is discharged into the air. During the reaction period, samples were taken from the sampling port at regular intervals for analysis, and the water sample was bubbled with nitrogen for 3min to terminate the oxidation reaction of ozone.
After the reaction is finished, a two-way valve connected with an ozone absorption device 10.1 is opened, and 2% KI solution is used for absorbing ozone tail gas.
nano-CeO2Preparation of solid catalyst:
(1) weighing 5g of cerous nitrate hexahydrate and putting the cerous nitrate hexahydrate in a ceramic boat;
(2) putting the sample weighed in the step (1) into a muffle furnace, and heating at 10 ℃ for min in an air atmosphere-1The temperature rising rate is increased to 550 ℃ and calcined for 4 hours to obtain a light yellow solid;
(3) the light yellow solid in the step (2) is transferred into an agate mortar for full grinding and then stored to prepare nano-CeO2The XRD characterization chart, the SEM characterization chart and the XPS characterization chart of the solid catalyst are shown in figures 2-4. In XRD pattern, by comparing standard CeO2Catalyst composition prepared by card description is CeO2And SEM shows that the catalyst is nanosphere agglomerates of 10-50nm and has higher specific surface area. X-ray photoelectron spectroscopy (XPS) showed that the prepared CeO2The catalyst has more Ce3+The existence of (2) means that the catalyst has a plurality of oxygen vacancies and has higher catalytic activity.
In the following examples, the method of measuring the acetic acid concentration was as follows: measuring the pH value by using a pH precision acidimeter; the concentration of acetate ions in the solution was determined using high performance liquid chromatography UltiMate3000 (ThermoFisher Dionex UltiMate3000, USA) with column type: c18 column (250X 4.6mm, particle size 5mm), eluent 0.0134mol phosphate buffer (pH 3) mixture and methanol (950:50, V: V), flow rate of 1.20mL min-1And the ultraviolet detection wavelength is 210 nm.
Example 1
The prepared catalyst finished product is used for catalyzing, ozonizing and degrading acetic acid wastewater (the concentration of acetic acid is 100mg/L, the volume of reaction liquid is 250ml, and the rest is water). The amount of catalyst added was 0.08g/L and the amount of hydrogen peroxide added was 100mg/L, and the pH of the solution was adjusted to 3.0 with sulfuric acid. The experiment was carried out in a semi-batch process at O2/O3The flow rate of the mixed gas is 0.1L/min, the ozone output is 9.9mg/min, and the sampling detection is carried out when the experimental reaction is 30 min.
Comparative examples 1 to 4
For comparison, the following 4 sets of comparative tests, each H, were carried out under the same experimental conditions2O2/O3、CeO2/O3、CeO2/H2O2/O2、CeO2/O2The system degrades the acetic acid solution with the same concentration.
The concentration of acetic acid (initial concentration 100mg/L) at 30min of the water sample treatment is shown in Table 1.
TABLE 1
Examples 2 to 4
The prepared catalyst finished product is used for catalyzing H2O2/O3Degrading acetic acid wastewater (acetic acid concentration is 100mg/L, H)2O2The dosage is 100mg/L, the volume of the reaction solution is 250ml, and the rest is water). The addition of the catalyst is 0.08g/L, the experiment adopts a semi-batch processing mode, and the catalyst is added in O2/O3The flow rate of the mixed gas is 0.1L/min, the ozone output is 9.9mg/min, and the sampling detection is carried out when the experimental reaction is 30 min.
Examples 2 to 4 the pH of the solution was adjusted to 1.0, 5.0 and 7.0 with sulfuric acid, respectively, and the other conditions were the same as in example 1.
The concentration of acetic acid (initial concentration 100mg/L) at 30min of the water sample treatment is shown in Table 2.
TABLE 2
Examples 5 to 8
The prepared catalyst finished product is used for catalyzing, ozonizing and degrading acetic acid wastewater (the concentration of acetic acid is 100mg/L, H is2O2The dosage is 100mg/L, the volume of the reaction solution is 250ml, and the rest is water). Then the pH value is adjusted to 3.0 by using sulfuric acid respectively. The experiment was carried out in a semi-batch process at O2/O3The flow rate of the mixed gas is 0.1L/min, the ozone output is 9.9mg/min, and the sampling detection is carried out when the experimental reaction is 30 min.
The catalysts of examples 5 to 8 were added in amounts of 0.02g/L, 0.04g/L, 0.16g/L and 0.32g/L, respectively, under the same conditions as in example 1.
The acetic acid concentration (initial concentration 100mg/L) at 30min of the water sample treatment is shown in Table 3.
TABLE 3
Examples 9 to 12
The prepared catalyst finished product is used for catalyzing, ozonizing and degrading acetic acid wastewater (the concentration of acetic acid is 100mg/L, H is2O2The dosage is 100mg/L, the volume of the reaction solution is 250ml, and the rest is water). The addition of the catalyst was 0.08g/L, and the pH was adjusted to 3.0 with sulfuric acid. The experiment was carried out in a semi-batch process at O2/O3The flow rate of the mixed gas is 0.1L/min, and the sampling detection is carried out when the experimental reaction is carried out for 30 min.
Examples 9 to 12 had ozone production amounts of 1.4mg/min, 4.5mg/min, 20.2mg/min and 39.2mg/min, and the other conditions were the same as in example 1.
The acetic acid concentration (initial concentration 100mg/L) at 30min of the water sample treatment is shown in Table 4.
TABLE 4
Examples 13 to 15
The prepared catalyst finished product is used for catalyzing, ozonizing and degrading acetic acid wastewater (the concentration of acetic acid is 100mg/L, the volume of reaction liquid is 250ml, and the rest is water). The addition of the catalyst was 0.08g/L, and the pH was adjusted to 3.0 with sulfuric acid, respectively. The experiment was carried out in a semi-batch process at O2/O3The flow rate of the mixed gas is 0.1L/min, the ozone output is 9.9mg/min, and the sampling detection is carried out when the experimental reaction is 30 min.
Examples 13 to 15H2O2The amounts of the reagents added were 50mg/L, 200mg/L and 400mg/L, respectively, and the other conditions were the same as in example 1.
The acetic acid concentration (initial concentration 100mg/L) at 30min of the water sample treatment is shown in Table 5.
TABLE 5
Example 16
The prepared catalyst finished product is used for catalyzing, ozonizing and degrading nitrobenzene wastewater (the concentration of nitrobenzene is 100mg/L, the volume of reaction liquid is 500ml, and the rest is water). The addition of the catalyst was 0.08g/L, and the pH was adjusted to 3.0 with sulfuric acid, respectively. The experiment was carried out in a semi-batch process at O2/O3The mixed gas flow rate is 0.1L/min, the ozone output is 9.9mg/min, the experimental reaction is carried out for 5min, 10min, 20min, 30min and 40min, samples are taken to detect the nitrobenzene concentration, and the COD is measured.
| Example 16 | 0min | 5min | 10min | 20min | 30min | 40min |
| Nitrobenzene concentration (mg/L) | 100 | 50.92 | 25.25 | 0.4572 | 0 | 0 |
| COD(mg/L) | 190.1 | 151.6 | 84 | 54 | 48 | 32 |
Claims (5)
1. Adopts nano-CeO2/H2O2/O3The method for treating the acidic degradation-resistant wastewater by the system is characterized by comprising the following steps of:
(1) adding nano-CeO into acidic wastewater containing organic pollutants and having pH of 1-52Solid catalyst and H2O2Stirring uniformly to obtain a mixed solution; the organic contaminant H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 0.5-4: 0.2-3; the organic pollutant is acetic acid;
(2) and (3) introducing ozone into the mixed solution for degradation reaction to obtain degraded wastewater.
2. The method of claim 1 using nano-CeO2/H2O2/O3The method for treating the acidic degradation-resistant wastewater by the system is characterized by comprising the following steps: the nano-CeO2The solid catalyst is nano cerium oxide synthesized by taking cerous nitrate hexahydrate as a precursor and adopting a high-temperature thermal decomposition method.
3. The method of claim 2 wherein nano-CeO is adopted2/H2O2/O3The method for treating acidic degradation-resistant wastewater by using the system is characterized in that the nano-CeO2The preparation method of the solid catalyst comprises the following steps: (a) weighing cerous nitrate hexahydrate, putting the cerous nitrate hexahydrate in a ceramic boat, putting the ceramic boat in a muffle furnace, and heating the ceramic boat at the temperature of 10 ℃ for min in the air atmosphere-1The temperature rising rate is increased to 550 ℃ and calcined for 4 hours to obtain a light yellow solid;
(b) fully grinding the light yellow solid in the step (a) to obtain nano-CeO2A solid catalyst.
4. The method of claim 1 wherein nano-CeO is used2/H2O2/O3The method for treating the acidic degradation-resistant wastewater is characterized in that in the mixed solution in the step (1), the organic pollutants and H2O2And nano-CeO2The mass ratio of the solid catalyst is 1: 1-4: 0.8-1.6.
5. The method of claim 1 wherein nano-CeO is used2/H2O2/O3The method for treating the acidic degradation-resistant wastewater is characterized in that in the step (2), the ozone is O2/O3Introducing mixed gas in a form of flow rate of 0.1-0.6 L.min-1Wherein the concentration of ozone is 1.4-39.2 mg.L-1。
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| CeO2纳米材料催化H2O2降解酸性二号橙的研究;沈星星;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;中国学术期刊（光盘版）电子杂志社;20120615(第6期);B020-173 * |
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Application publication date: 20180518 Assignee: ZHEJIANG DOWAY ADVANCED TECHNOLOGY Co.,Ltd. Assignor: JIANG University OF TECHNOLOGY Contract record no.: X2023980037737 Denomination of invention: A method for treating acid refractory wastewater using the nano CeO2/H2O2/O3system Granted publication date: 20210202 License type: Common License Record date: 20230707 |