CN114749190A - Preparation and application of Fenton cocatalyst for continuous flow drug wastewater treatment - Google Patents
Preparation and application of Fenton cocatalyst for continuous flow drug wastewater treatment Download PDFInfo
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- CN114749190A CN114749190A CN202210185548.2A CN202210185548A CN114749190A CN 114749190 A CN114749190 A CN 114749190A CN 202210185548 A CN202210185548 A CN 202210185548A CN 114749190 A CN114749190 A CN 114749190A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- C02F2101/306—Pesticides
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention provides a preparation method and application of a Fenton cocatalyst for continuous flow organic wastewater treatmentxand/CM. The molybdenum sulfide prepared by the invention has the function of modifyingThe sex ceramic membrane has rich pore structure and excellent mechanical strength, contains a large number of reductive active sites, can efficiently promote the iron ion circulation in the Fenton reaction, and improves the utilization rate of the oxidant; the nano-catalyst is used in a continuous flow wastewater treatment reactor, can simultaneously realize the removal of suspended matters and the synchronous degradation of organic pollutants in actual wastewater, and solves the key technical problems that the nano-catalyst is difficult to be used in the continuous flow wastewater treatment reactor and the wastewater treatment efficiency of the traditional Fenton system is low.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to preparation and application of a Fenton cocatalyst for continuous flow drug wastewater treatment, and is suitable for rapid treatment of drug overproof water and other organic wastewater.
Background
Neonicotinoid pesticides are widely used in agricultural production as pesticides with the largest global dosage and scale, and insect pests are prevented and treated through seed soaking, foliage spraying and other ways. In recent years, water quality research finds that a large amount of neonicotinoid medicaments are detected in lakes and drinking water due to the use of the neonicotinoid medicaments. Researches show that the synergistic effect of various neonicotinoid drugs can lead the neonicotinoid drugs to show stronger toxicity under the condition of low concentration, and the residue of the drugs causes serious potential harm to the safety of human beings.
The Fenton technology is a water treatment technology with simple operation, quick reaction and high treatment efficiency. In the Fenton reaction, iron ion (Fe) is used2+) Activated hydrogen peroxide (H)2O2) The method generates oxidizing substances (hydroxyl radicals, singlet oxygen, high-valence metals and the like) with high reactivity, realizes the oxidative decomposition and deep removal of organic pollutant molecules, and therefore, the method is widely concerned in the deep treatment of organic wastewater. Iron ion cycle (Fe)3+/Fe2+) Is the key to limiting the efficiency of the traditional fenton reaction. However due to Fe3+The reduction rate of (A) is low, so that the traditional Fenton reaction needs continuous addition of Fe2+To maintain the reaction progress. Prior art iron ion cycle (Fe)3+/Fe2+) The rate is low, limiting the efficiency of the traditional fenton reaction.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides preparation and application of a Fenton cocatalyst for continuous flow drug wastewater treatment. The molybdenum sulfide modified functional ceramic membrane prepared by the method has rich pore structures and excellent mechanical strength, contains a large number of reductive active sites, can efficiently promote the iron ion circulation in the Fenton reaction, and improves the utilization rate of an oxidant; the nano catalyst is used in a continuous flow wastewater treatment reactor, can simultaneously realize removal of suspended matters and synchronous degradation of organic pollutants in actual wastewater, and solves the key technical problems that the nano catalyst is difficult to use in the continuous flow wastewater treatment reactor and the wastewater treatment efficiency of the traditional Fenton system is low.
The technical scheme of the invention is as follows:
a preparation method of a Fenton cocatalyst for continuous flow organic wastewater treatment is to prepare and obtain molybdenum sulfide MoS by a one-step hydrothermal methodxA modified functional ceramic membrane;
the specific method comprises the following steps: thiourea and ammonium molybdate are taken as reactants to prepare a reaction solution, a tubular ceramic membrane is taken as a supporting material, the reaction solution and the tubular ceramic membrane are transferred into a polytetrafluoroethylene reaction kettle together, and a molybdenum sulfide modified functional ceramic membrane MoS can be obtained through a hydrothermal reactionx/CM。
Preferably, x is 1 to 3.
Preferably, the tubular ceramic membrane material is Al2O3The aperture is 0.2-50 μm, and the porosity is 20-50%.
Preferably, the concentration of thiourea is 0.05-1.0M, the concentration of ammonium molybdate is 0.01-0.5M, and the molar ratio of thiourea to ammonium molybdate is 1: 1 to 4.
Preferably, the volume ratio of the reaction solution to the ceramic membrane is 1: 2-10 ℃, the hydrothermal reaction temperature is 120-200 ℃, and the reaction time is 6-24 h.
The invention also provides an application method of the Fenton cocatalyst in treatment of continuous flow organic wastewater, which comprises the following steps:
firstly, preparing an integrated wastewater treatment reactor, which comprises a feeder, a water inlet pipe, a wastewater treatment reactor and a water outlet pipe;
then, the functional ceramic membrane MoS prepared by the method is usedxThe bottom of the/CM is sealed and arranged in a reaction chamber of the reactor, and the organic wastewater flows through the MoS under the action of gravity or an external peristaltic pumpxCM, namely organic pollutants in single flow-through processAnd (4) removing with high efficiency.
Furthermore, the integrated wastewater treatment reactor is of a sealing structure, the interior of the integrated wastewater treatment reactor is a reaction chamber, and a plurality of functional ceramic membranes MoS with sealed bottoms are vertically arranged in parallelx/CM；
The water inlet pipe is filled with various functional ceramic membranes MoS from the top of the sealing structurexinside/CM, organic wastewater is treated and then flows from each functional ceramic membrane MoSxthe/CM side wall pore flows out and is discharged through a water outlet pipe positioned at the bottom of the sealing structure;
the feeder is connected to a water inlet pipe through a pump, and the hydrogen peroxide solution is mixed with the organic wastewater.
Furthermore, the integrated wastewater treatment reactor takes organic glass or stainless steel as a manufacturing material.
Further, iron ions contained in the organic wastewater are used as a catalyst, hydrogen peroxide added into the organic wastewater is used as an oxidant, the functional ceramic membrane is used as a cocatalyst, and oxidizing substances are generated through a Fenton-like reaction to remove organic pollutants;
the concentration range of the iron ions is 0.01-0.1 mM;
the hydrogen peroxide H2O2The concentration range is 0.1 to 1.0 mM.
Further, the organic wastewater is in MoSxThe residence time in the CM pore channel is 2-30 min.
Further, the organic wastewater comprises clothianidin, thiamethoxam and dinotefuran wastewater, and the concentration range of the organic matters is 0.1-100 mg/L.
The beneficial technical effects of the invention are as follows:
1. the tubular ceramic membrane is used as a support material, the molybdenum sulfide modified functional ceramic membrane prepared by a hydrothermal method has rich pore structures and excellent structural strength, and meanwhile, the molybdenum sulfide cocatalyst loaded in the pore channel can promote the circulation of iron ions (Fe) in Fenton reaction3+/Fe2+) The activation efficiency and the utilization rate of the Fenton reaction oxidant are improved, and the functional ceramic membrane co-catalysis Fenton system is beneficial to realizing suspended matters and difficult substances in wastewaterThe organic pollutants are synchronously and efficiently removed.
2. The specific three-dimensional pore channel structure of the molybdenum sulfide modified functional ceramic membrane prepared by the invention provides support for molybdenum sulfide, so that the molybdenum sulfide modified functional ceramic membrane has excellent mechanical strength; meanwhile, the rich reductive active sites on the surface of the molybdenum sulfide can effectively promote the iron ion circulation; the stable iron ion concentration can realize the high-efficiency activation of the oxidant, and further realize the oxidative degradation of organic pollutants. The functional ceramic membrane has efficient Fenton catalytic performance, has obvious effect of oxidizing and degrading organic pollutants in wastewater, and is suitable for quickly treating anabasine drug overproof water and other organic wastewater.
3. Based on the excellent co-catalysis performance of molybdenum sulfide in the Fenton reaction and the excellent structural performance of the ceramic membrane, the invention solves the key technical problems that the nano material is difficult to be used in a continuous flow wastewater treatment reactor, the iron ion circulation efficiency in the Fenton reaction is low, iron mud is easy to generate, the utilization rate of an oxidant is low, and suspended matters in actual wastewater and organic pollutants are synchronously degraded. Meanwhile, the invention adopts the supported cocatalyst, thereby avoiding the problem of easy loss when the cocatalyst is directly added into the reactor, and further improving the treatment efficiency of the Fenton technology in the actual wastewater treatment.
4. The invention improves the circulation efficiency of iron ions in Fenton reaction under the condition of not providing additional energy, and simultaneously realizes the continuous treatment of wastewater. Compared with the electro-fenton technology, the main progressions are as follows: 1) the work does not need to provide energy; 2) the connection between the ceramic membrane and components such as a peristaltic pump can be realized by utilizing the three-dimensional structure of the ceramic membrane, and the system is simpler and easier to operate; 3) electro-Fenton is to utilize the electrocatalysis process to produce the oxidizing agent to realize the waste water treatment, but the invention utilizes the catalysis-assisted Fenton performance of the molybdenum disulfide to realize the high-efficient circulation of the catalyst, thus improve the waste water treatment efficiency.
5. Compared with the traditional molybdenum disulfide existing in the organic functional membrane, the molybdenum disulfide grows on the surface of the pore channel of the ceramic membrane. The traditional molybdenum sulfide is used as a modified material of an organic functional film layer in a composite film material, and the molybdenum disulfide is used as a catalyst promoter of Fenton reaction, so that the high-efficiency circulation of the catalyst is realized, and the wastewater treatment efficiency of the catalyst is improved.
6. Aiming at the speed-limiting step of iron ion circulation in Fenton reaction, the invention utilizes the functional ceramic membrane as the cocatalyst to improve the circulation rate, thereby improving the wastewater treatment efficiency of the system. Therefore, compared with the traditional Fenton reaction, the method is based on the Fenton reaction, and improves and expands the wastewater treatment efficiency to a certain extent. The functional ceramic membrane not only plays a role in physically filtering wastewater, but also serves as a cocatalyst, and iron ion circulation is promoted by using reduced molybdenum ions of the functional ceramic membrane, so that hydrogen peroxide H is increased2O2The activation efficiency of (2) promotes the oxidative degradation of organic pollutants.
Drawings
FIG. 1 is a diagram of a functional ceramic membrane prepared by the preparation method provided in example 1 of the present invention;
FIG. 2 is a micro-topography of a functional ceramic film prepared by the preparation method provided in example 1 of the present invention;
FIG. 3 is a diagram of a functional ceramic membrane prepared by the preparation method of example 2 of the present invention;
FIG. 4 is a schematic diagram and a schematic structural view of a wastewater treatment reactor in which the method of the present invention is applied in example 3;
FIG. 5 is a graph showing the effect of the application method provided in example 3 of the present invention on the treatment of organic wastewater.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
preparing 25mL (0.05M) of ammonium molybdate solution and 25mL (0.1M) of thiourea solution, ultrasonically dispersing for 20min, mixing, and transferring into a 100mL polytetrafluoroethylene reaction kettle; using 100mL of deionizationWashing the waste tubular ceramic membrane with seed water, placing the washed tubular ceramic membrane in a 60 ℃ oven for drying, wherein the size of the tubular ceramic membrane is phi 3.0cm multiplied by 2.0cm multiplied by 5.0cm (outer diameter multiplied by inner diameter multiplied by height, hollow structure, membrane volume is 20mL), the pore diameter is 30 mu m, the porosity is 43%, and then transferring the dried tubular ceramic membrane to the mixed reaction solution; finally, sealing the polytetrafluoroethylene reaction kettle, and placing the reaction kettle in a drying oven at 200 ℃ for hydrothermal reaction for 8 hours to obtain the molybdenum sulfide modified functional ceramic membrane (MoS)x/CM) (as shown in fig. 1 and 2).
Example 2:
preparing 12mL (0.2M) of ammonium molybdate solution and 12mL (1.0M) of thiourea solution, ultrasonically dispersing for 20min, mixing, and transferring into a 50mL polytetrafluoroethylene reaction kettle; washing the waste tubular ceramic membrane by using 100mL of deionized water, placing the washed tubular ceramic membrane in a 60 ℃ drying oven for drying, wherein the size of the tubular ceramic membrane is phi 1.2cm multiplied by 0.8cm multiplied by 3.0cm, the aperture is 0.5 mu m, the porosity is 28%, and then transferring the dried tubular ceramic membrane to the mixed reaction solution; finally, sealing the polytetrafluoroethylene reaction kettle, and placing the reaction kettle in a drying oven at 150 ℃ for hydrothermal reaction for 20 hours to obtain the molybdenum sulfide modified functional ceramic membrane (MoS)x/CM) (as shown in FIG. 3).
Example 3:
(1) one end of the functional ceramic membrane prepared in the example 1 is sealed to be used as a bottom; then, it was used as a Fenton co-catalyst and placed in a reaction chamber of a continuous flow wastewater treatment reactor, the diameter of the reaction chamber was 11.0cm, the height was 5.0cm, and the organic glass on the upper layer of the reaction chamber was provided with uniformly distributed pores having a diameter of 3.0cm, which was consistent with the size of the functional ceramic membrane of example 1 (see FIG. 4);
(2) taking 10mg/L clothianidin wastewater (simulated drug wastewater) as a treatment object, wherein the concentration of iron ions contained in the wastewater is 0.04mM, and the concentration of hydrogen peroxide is 0.4mM, and adjusting the concentration of the wastewater in MoS through a valve arranged in a continuous flow wastewater treatment reactorxThe residence time in the CM channels was set at 8 min. After the reactor is operated for 60 hours, the removal rate of the clothianidin by the reaction system can still be kept above 70% (as shown in figure 5).
While the embodiments of the present invention have been disclosed above, it is not limited to the applications listed in the description and embodiments, but is fully applicable to various fields suitable for the present invention, and it will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in the embodiments without departing from the principle and spirit of the present invention, and therefore the present invention is not limited to the specific details without departing from the general concept defined in the claims and the scope of equivalents thereof.
Claims (10)
1. The preparation method of the Fenton cocatalyst for continuous flow organic wastewater treatment is characterized in that the molybdenum sulfide MoS is prepared and obtained by a one-step hydrothermal methodxA modified functional ceramic membrane;
the specific method comprises the following steps: thiourea and ammonium molybdate are taken as reactants to prepare reaction liquid, a tubular ceramic membrane is taken as a supporting material, the reaction liquid and the tubular ceramic membrane are transferred into a polytetrafluoroethylene reaction kettle together, and the functional ceramic membrane MoS modified by molybdenum sulfide can be obtained through hydrothermal reactionx/CM。
2. The method according to claim 1, wherein the tubular ceramic membrane material is Al2O3The aperture is 0.2-50 μm, and the porosity is 20-50%.
3. The preparation method according to claim 1, wherein the thiourea concentration is 0.05M to 1.0M, the ammonium molybdate concentration is 0.01M to 0.5M, and the molar ratio of thiourea to ammonium molybdate is 1: 1 to 4.
4. The method according to claim 1, wherein the volume ratio of the reaction solution to the ceramic membrane is 1: 2-10 ℃, the hydrothermal reaction temperature is 120-200 ℃, and the reaction time is 6-24 h.
5. A method for applying the Fenton's cocatalyst according to any one of claims 1 to 4 to the treatment of continuous flow organic wastewater, characterized in that an integrated wastewater treatment reactor is firstly prepared, wherein the integrated wastewater treatment reactor comprises a feeder, a water inlet pipe, a wastewater treatment reactor and a water outlet pipe;
then, a functional ceramic membrane MoS prepared according to any one of claims 1 to 4xThe bottom of the/CM is sealed and arranged in a reaction chamber of the reactor, and the organic wastewater flows through the MoS under the action of gravity or an external peristaltic pumpxand/CM, namely the organic pollutants can be efficiently removed in a single flow-through process.
6. The application method of claim 5, wherein the integrated wastewater treatment reactor is a sealed structure, the inside of the integrated wastewater treatment reactor is a reaction chamber, and a plurality of functional ceramic membranes MoS with sealed bottoms are vertically arranged in parallelx/CM；
The water inlet pipe is filled with various functional ceramic membranes MoS from the top of the sealing structurexinside/CM, organic wastewater is treated and then flows from each functional ceramic membrane MoSxthe/CM side wall pore flows out and is discharged through a water outlet pipe positioned at the bottom of the sealing structure;
the feeder is connected to a water inlet pipe through a pump, and the hydrogen peroxide solution is mixed with the organic wastewater.
7. The method of use of claim 5, wherein the integrated wastewater treatment reactor is fabricated from plexiglas or stainless steel.
8. The application method of claim 5, wherein iron ions contained in the organic wastewater are used as a catalyst, hydrogen peroxide added in the organic wastewater is used as an oxidant, the functional ceramic membrane is used as a cocatalyst, and oxidizing substances are generated through Fenton-like reaction to remove organic pollutants;
the concentration range of the iron ions is 0.01-0.1 mM;
the hydrogen peroxide H2O2The concentration range is 0.1 to 1.0 mM.
9. The method of application according to claim 5,the organic wastewater is in MoSxThe residence time in the CM pore channel is 2-30 min.
10. The application method of claim 5, wherein the organic wastewater comprises clothianidin, thiamethoxam and dinotefuran wastewater, and the concentration of the organic matters is in the range of 0.1 mg/L-100 mg/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115869980A (en) * | 2022-11-01 | 2023-03-31 | 同济大学 | Monoatomic catalytic membrane for persulfate wastewater treatment system and preparation and application thereof |
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| CN113457691A (en) * | 2021-07-16 | 2021-10-01 | 南京工业大学 | Gold-silver alloy nano flower water treatment catalyst and preparation method and application thereof |
| CN113731448A (en) * | 2021-08-20 | 2021-12-03 | 华南理工大学 | Homogeneous Fenton cocatalyst, and preparation method and application thereof |
| CN113996316A (en) * | 2021-11-24 | 2022-02-01 | 南京泽佑环保科技有限公司 | Granulation method of heterogeneous Fenton catalyst |
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| CN109772370A (en) * | 2019-03-01 | 2019-05-21 | 华东理工大学 | A kind of water purification beaded catalyst and its preparation method and application |
| CN111018083A (en) * | 2019-12-19 | 2020-04-17 | 南京师范大学 | Ceramic membrane Fenton reactor and application method thereof |
| CN113457691A (en) * | 2021-07-16 | 2021-10-01 | 南京工业大学 | Gold-silver alloy nano flower water treatment catalyst and preparation method and application thereof |
| CN113731448A (en) * | 2021-08-20 | 2021-12-03 | 华南理工大学 | Homogeneous Fenton cocatalyst, and preparation method and application thereof |
| CN113996316A (en) * | 2021-11-24 | 2022-02-01 | 南京泽佑环保科技有限公司 | Granulation method of heterogeneous Fenton catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115869980A (en) * | 2022-11-01 | 2023-03-31 | 同济大学 | Monoatomic catalytic membrane for persulfate wastewater treatment system and preparation and application thereof |
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