CN114538594A - Preparation method of multi-transition metal composite environment restoration material - Google Patents
Preparation method of multi-transition metal composite environment restoration material Download PDFInfo
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- CN114538594A CN114538594A CN202210191287.5A CN202210191287A CN114538594A CN 114538594 A CN114538594 A CN 114538594A CN 202210191287 A CN202210191287 A CN 202210191287A CN 114538594 A CN114538594 A CN 114538594A
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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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- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
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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
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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
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a preparation method of a multi-element transition metal composite environment restoration material, which comprises the following steps: mixing CuSO4·5H2O and FeCl3·6H2Stirring O according to the proportion to completely dissolve the O in the deionized water; dropwise adding NaOH solution and Na2CO3Carrying out coprecipitation reaction on the solution, keeping the temperature at 60 ℃ for 4h, then carrying out suction filtration, washing and vacuum drying to obtain a blue-gray solid; putting the blue gray solid into a muffle furnace for calcining to obtain CuFe2O4Nanoparticles of CuFe2O4Adding the nano particles into a mixed solution of water, ethanol, hexadecyl trimethyl ammonium bromide and tetraethyl silicate, dropwise adding ammonia water, further stirring the reaction mixture, and then filtering, washing and vacuum drying; calcining to obtain CuFe2O4/SiO2The environment restoration material prepared by the invention can efficiently degrade various organic pollutants in water in a wider pH range, can be applied to various water treatment processes and water environment restoration engineering practices in various ways, and has high activity and stability after repeated use.
Description
Technical Field
The invention relates to the technical field of environment restoration materials, in particular to a preparation method of a multi-element transition metal composite environment restoration material.
Background
At present, the traditional Fenton reaction has the problems of easy generation of iron mud, low pH condition and the like, and materials related to transition metals are adopted as Fenton-like reagents to react in a wide pH range to generate hydroxyl radicals so as to efficiently degrade and even completely mineralize organic pollutants in water, so that the Fenton-like reagents are hot spots of current scientific research and technical development. The compounding of the multi-element transition metal is beneficial to realizing the cooperative catalysis, and the reaction efficiency and the activity stability can be improved by loading the multi-element transition metal on the porous material. Various processes can be adopted to achieve the degradation goal in the application process. Therefore, it is urgently needed to develop a preparation method of the multi-element transition metal composite environment-repairing material to solve the above technical problems.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of a multi-transition metal composite environment restoration material, the prepared environment restoration material can efficiently degrade various organic pollutants including macromolecules such as humic acid in water in a wider pH range, can be applied to various water treatment processes and water environment restoration engineering practices in a manner of batch type, fluidized bed, permeable reactive barrier and the like, has high activity and stability after repeated use, has wide application prospect, and is beneficial to popularization and application.
In order to achieve the purpose, the preparation method of the multi-transition metal composite environment repair material provided by the invention comprises the following steps:
s1: mixing CuSO4·5H2O and FeCl3·6H2Stirring O according to the proportion to completely dissolve the O in the deionized water;
s2: NaOH solution and Na are slowly added dropwise2CO3Carrying out coprecipitation reaction on the solution, keeping the temperature at 60 ℃ for 4h after complete precipitation, then carrying out suction filtration, pulping and washing by using deionized water and absolute ethyl alcohol in sequence, and drying in vacuum at 70 ℃ for 4h after washing is finished to obtain a blue-gray solid;
S3: putting the blue gray solid obtained in the S2 into a muffle furnace for calcining to obtain CuFe2O4Nanoparticles of CuFe2O4Adding the nano particles into a mixed solution of water, ethanol, hexadecyl trimethyl ammonium bromide and tetraethyl silicate, dropwise adding ammonia water at 45 ℃, further stirring the reaction mixture for 6 hours, and then filtering, washing and vacuum drying;
s4: calcining the solid obtained after the S3 vacuum drying in a muffle furnace to obtain CuFe2O4/SiO2Composite environmental repair materials.
Preferably, in S1, CuSO4·5H2O and FeCl3·6H2The ratio of O is 2: 1.
Preferably, in S3, washing is performed with water.
Preferably, in the S3, the calcining temperature is 500 ℃ and the calcining time is 6 h.
Preferably, in the S3, the temperature of vacuum drying is 70 ℃.
Preferably, in the S4, the calcining temperature is 500 ℃ and the calcining time is 5 h.
The preparation method of the multi-element transition metal composite environment restoration material provided by the invention has the following beneficial effects.
1. The multi-element transition metal composite environment restoration material prepared by the invention can efficiently degrade various organic pollutants including macromolecules such as humic acid and the like in water within a wider pH range, and the degradation rate reaches 80-100%.
2. The multi-element transition metal composite environment restoration material prepared by the invention can be applied to various water treatment processes and water environment restoration engineering practices in a manner of batch type, fluidized bed, permeable reactive barrier and the like, and can still maintain the activity stability of more than 92% after being repeatedly used for more than ten times.
Drawings
FIG. 1 is an analysis diagram of X-ray diffraction, aperture and specific surface area of the multi-element transition metal composite environment repairing material prepared by the invention;
FIG. 2 is a diagram showing the effect of humic acid degradation by six-time reuse of the multi-element transition metal composite environment restoration material prepared by the invention.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and accompanying drawings to assist in understanding the contents of the invention.
The invention provides a preparation method of a multi-transition metal composite environment restoration material, which comprises the following steps:
s1: mixing CuSO4·5H2O and FeCl3·6H2Stirring O according to the ratio of 2:1 to completely dissolve the O in the deionized water;
s2: NaOH solution and Na are slowly added dropwise2CO3Carrying out coprecipitation reaction on the solution, keeping the temperature at 60 ℃ for 4h after complete precipitation, then carrying out suction filtration, pulping and washing by using deionized water and absolute ethyl alcohol in sequence, and drying in vacuum at 70 ℃ for 4h after washing is finished to obtain a blue-gray solid;
s3: calcining the blue gray solid obtained from S2 in a muffle furnace at 500 ℃ for 6h to obtain CuFe2O4Nanoparticles of CuFe2O4Adding the nanoparticles into a mixed solution of water, ethanol, hexadecyl trimethyl ammonium bromide and tetraethyl silicate, dropwise adding ammonia water at 45 ℃, further stirring the reaction mixture for 6 hours, then filtering, washing with water, and drying in vacuum at the temperature of 70 ℃;
s4: calcining the solid obtained after the vacuum drying of S3 in a muffle furnace at the calcining temperature of 500 ℃ for 5h to obtain CuFe2O4/SiO2Composite environmental repair materials.
As shown in fig. 1, it is an analysis diagram of X-ray diffraction, aperture and specific surface area of the multi-element transition metal composite environment repairing material prepared by the present invention. The X-ray diffraction result shows that the prepared multi-element transition metal composite environment restoration material has a good crystal structure and a porous structure, and the specific surface area is obviously improved by loading. X photoelectron spectrum shows that the surface of the prepared multi-transition metal composite environment repairing material has multi-transition metal active centers.
As shown in FIG. 2, the effect diagram of the multi-element transition metal composite environment restoration material prepared by the invention for degrading humic acid after being reused for six times is shown. The results show that: the degradation rate of humic acid reaches 100 percent under the condition of 80 ℃. The prepared multi-element transition metal composite environment restoration material has high activity stability, the degradation rate of humic acid is more than 98.5% after the multi-element transition metal composite environment restoration material is repeatedly used for six times, and the multi-element transition metal composite environment restoration material can be used as a Fenton-like reagent and can generate active oxygen species through reaction in a wider pH range to degrade organic pollutants in water.
The inventive concept is explained in detail herein using specific examples, which are given only to aid in understanding the core concepts of the invention. It should be understood that any obvious modifications, equivalents and other improvements made by those skilled in the art without departing from the spirit of the present invention are included in the scope of the present invention.
Claims (6)
1. The preparation method of the multi-transition metal composite environment restoration material is characterized by comprising the following steps:
s1: mixing CuSO4·5H2O and FeCl3·6H2Stirring O according to the proportion to completely dissolve the O in the deionized water;
s2: NaOH solution and Na are slowly added dropwise2CO3Carrying out coprecipitation reaction on the solution, keeping the temperature at 60 ℃ for 4h after complete precipitation, then carrying out suction filtration, pulping and washing by using deionized water and absolute ethyl alcohol in sequence, and drying in vacuum at 70 ℃ for 4h after washing is finished to obtain a blue-gray solid;
s3: putting the blue gray solid obtained in the S2 into a muffle furnace for calcining to obtain CuFe2O4Nanoparticles of CuFe2O4Adding the nano particles into a mixed solution of water, ethanol, hexadecyl trimethyl ammonium bromide and tetraethyl silicate, dropwise adding ammonia water at 45 ℃, further stirring the reaction mixture for 6 hours, and then filtering, washing and vacuum drying;
s4: calcining the solid obtained after S3 vacuum drying in a muffle furnaceFiring to obtain CuFe2O4/SiO2Composite environmental repair materials.
2. The method for preparing the environment-repairing material as claimed in claim 1, wherein in S1, CuSO4·5H2O and FeCl3·6H2The ratio of O is 2: 1.
3. The method for preparing the environment-repairing material as claimed in claim 1, wherein in S3, water is used for washing.
4. The method for preparing the environment-repairing material as claimed in claim 1, wherein the calcining temperature in S3 is 500 ℃ and the calcining time is 6 hours.
5. The method for preparing the environment-repairing material as claimed in claim 1, wherein the temperature of vacuum drying in S3 is 70 ℃.
6. The method for preparing the environment-repairing material as claimed in claim 1, wherein the calcining temperature in S4 is 500 ℃ and the calcining time is 5 h.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0891917A (en) * | 1994-09-19 | 1996-04-09 | Matsushita Electric Ind Co Ltd | Ferrite material and its production |
| CN110423256A (en) * | 2019-07-30 | 2019-11-08 | 陈国岸 | A method of fulvic acid is produced using transition metal ion catalyst hydrogen peroxide degradation low-order coal |
| CN110961108A (en) * | 2019-12-18 | 2020-04-07 | 泉州师范学院 | Copper ferrite nanocomposite and preparation method and application thereof |
| CN111286324A (en) * | 2020-03-27 | 2020-06-16 | 上海应用技术大学 | Fluorescent probe for detecting hypochlorite in water environment and preparation method and application thereof |
| CN111974394A (en) * | 2020-09-22 | 2020-11-24 | 广东石油化工学院 | Copper ferrite composite material with high catalytic activity and application thereof |
| CN113101930A (en) * | 2021-03-12 | 2021-07-13 | 中南大学 | Preparation of copper ferrite Fenton catalyst with coralline morphology and application of copper ferrite Fenton catalyst in Fenton catalytic oxidation of landfill leachate |
-
2022
- 2022-02-28 CN CN202210191287.5A patent/CN114538594A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0891917A (en) * | 1994-09-19 | 1996-04-09 | Matsushita Electric Ind Co Ltd | Ferrite material and its production |
| CN110423256A (en) * | 2019-07-30 | 2019-11-08 | 陈国岸 | A method of fulvic acid is produced using transition metal ion catalyst hydrogen peroxide degradation low-order coal |
| CN110961108A (en) * | 2019-12-18 | 2020-04-07 | 泉州师范学院 | Copper ferrite nanocomposite and preparation method and application thereof |
| CN111286324A (en) * | 2020-03-27 | 2020-06-16 | 上海应用技术大学 | Fluorescent probe for detecting hypochlorite in water environment and preparation method and application thereof |
| CN111974394A (en) * | 2020-09-22 | 2020-11-24 | 广东石油化工学院 | Copper ferrite composite material with high catalytic activity and application thereof |
| CN113101930A (en) * | 2021-03-12 | 2021-07-13 | 中南大学 | Preparation of copper ferrite Fenton catalyst with coralline morphology and application of copper ferrite Fenton catalyst in Fenton catalytic oxidation of landfill leachate |
Non-Patent Citations (1)
| Title |
|---|
| 王洪朝: "3-甲氧基-4-羟基扁桃酸高效氧化催化剂研制与应用" * |
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