CN106517341A - Method for preparing manganese dioxide nano-catalyst and application thereof - Google Patents

Method for preparing manganese dioxide nano-catalyst and application thereof Download PDF

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CN106517341A
CN106517341A CN201610902999.8A CN201610902999A CN106517341A CN 106517341 A CN106517341 A CN 106517341A CN 201610902999 A CN201610902999 A CN 201610902999A CN 106517341 A CN106517341 A CN 106517341A
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mno
catalyst
mno2
solution
nano
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CN106517341B (en
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杜红梅
江训恒
严慧敏
邹建平
朱建军
邢秋菊
曾文龙
孙雨欣
鄢光雨
张军
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Nanchang Hangkong University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/02—Oxides; Hydroxides
    • 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
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • 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
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C02F2101/38—Organic compounds containing nitrogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a method for preparing an alpha-MnO2 nano-catalyst and application thereof. Through two-step synthesis, a MnO2 nano-material is obtained. The method comprises the following steps: firstly carrying out self-decomposition on potassium permanganate under the alkaline condition to obtain a precursor delta-MnO2; and carrying out ultrasonic treatment by adding GO into the delta-MnO2 obtained after ultrasonic treatment, and carrying out hydro-thermal treatment in a muffle furnace for 24 h so as to finally obtain the alpha-MnO2 nano-material. The invention has the following advantages: 1, the nanofibrous MnO2 catalyst is synthesized for the first time; 2, the catalyst has good capability of degrading organic pollutants, can catalyze self-decomposition of PMS to generate lots of .OH and SO4.<-> free radicals so as to enhance p-nitrophenol degradation efficiency; and 3, the preparation method of the catalyst is simple and feasible; production cost is low; yield and purity are both high; and the thermal-synthesized MnO2 nano-fiber is a catalyst with strong morphology homogeneity, high specific surface area and good heat stability.

Description

A kind of method for preparing manganese dioxide nano catalyst and its application
Technical field
The present invention relates to a kind of method for preparing manganese dioxide nano catalyst and its application.
Background technology
In recent years, it is industrial to develop the growth for not only having driven national economy rapidly, also result in water pollution disaster thing The frequent generation of part.And the pollution of water resource is especially prominent in environmental problem one, and the universal face in countries in the world at present Face and one of problem demanding prompt solution.After different types of many clock organic pollutions enter water body, it is not easily decomposed, can be steady for a long time Fixed is present in water body, and there is major part itself intermediate product of toxicity, many organic matters or its degraded to have " carcinogenic, cause " three cause " effect of abnormal, mutagenesis ", constitutes huge threat to the health of the mankind.For the organic pollution of these difficult degradations, Especially persistence organic pollutant（POPs）, it is difficult to remove using traditional physics, chemistry, biological treatment.Therefore How to efficiently synthesize out the catalyst of function admirable, and efficiently to remove a large amount of POPs present in environment be current research weight Point.Water pollution problems in the environment problem that not just China is present, it is in other countries, or even is all difficult in world wide The major issue of solution.
Manganese dioxide is the Mn oxide that a class has various excellent chemical performances.It has abundant crystal structure and variable Valence state, α-MnO2It is with MnO6The black floc being made up of construction unit, which has one-dimensional octahedra tunnel knot Structure.α-MnO2Nanofiber form has greatly help for the raising of organic matter degradation rate.
Hydrothermal synthesis method is that, under subcritical and supercritical water heat condition, as reaction is in molecular level, reactivity is carried Height, thus hydro-thermal reaction can substitute some high temperature solid state reactions.Again due to homogeneous nucleation and the nonhomogen-ous nucleation of hydro-thermal reaction Mechanism is different from the flooding mechanism of solid phase reaction, thus can create noval chemical compound and the green wood that other methods cannot be prepared Material.Hydrothermal synthesis method advantage is that products therefrom purity is high, and good dispersion, granularity are easy to control.And the present invention make use of water well The advantage of thermal synthesis method, and successfully synthesize that homogeneity is strong, the catalyst α-MnO of good stability2。
The content of the invention
It is an object of the invention to provide a kind of method for preparing manganese dioxide nano catalyst and its application, are that degraded is held Long property organic pollution（POPs）There is provided a kind of more efficient material, and improve conscientiously the degradation efficiency and POPs of POPs Mineralization degree.
The present invention is achieved like this, a kind of method for preparing manganese dioxide nano catalyst, prepares α-MnO2Nanometer Catalyst, the catalyst are synthesized into by simple two-step method, obtain δ-MnO by precipitation method synthesis first2, then lead to Hydro-thermal reaction is crossed, by δ-MnO2It is changed into α-MnO2, and α-MnO2It is bigger with more preferable crystallinity, specific surface area, and have more The ability of good degraded persistence organic pollutant；It is characterized in that method and step is as follows：
（1）δ-MnO2Preparation：Weigh 15-18 gram of KOH to be dissolved in the mixed solution of second alcohol and water of 50-100 milliliters, second Alcohol is 1 with the volume ratio of water:1, it is uniformly mixing to obtain solution A.Weigh 4-8 gram of potassium permanganate and be dissolved in 20-40 milliliter deionizations In water, stir and obtain solution B.Solution A is slowly added dropwise in solution B, is sufficiently mixed and is uniformly reacted.Vacuum Suction filtration, is dried 6-12 hours in 80 degree of air dry ovens and obtains final product δ-MnO2。
（2）α-MnO2Preparation：Weigh（1）250 milligrams of the sample of middle drying is dissolved in 65-85 ml deionized waters, surpasses Sound 10-40 minutes；Add the graphene oxide of 2.3 g/l of 10-20 milliliters, ultrasonic 10-40 minutes；Resulting solution is loaded into poly- In tetrafluoroethene reactor, hydro-thermal reaction 24-40 hour in 150 ~ 200 DEG C of Muffle furnaces is put into.The material of Hydrothermal Synthesiss is carried out Vacuum filtration, after multiple deionized water washing, is dried in being put into vacuum drying chamber and obtains final product α-MnO2。
It is an advantage of the invention that：1st, catalyst of the invention is nanometer fibrous MnO2.2nd, catalyst of the invention tool There are preferable degradable organic pollutant effect, in advanced oxidation field, MnO2The selfdecomposition of PMS can be catalyzed, be produced substantial amounts of OH and SO4 •Free radical, so that effectively improve the degradation efficiency of p-nitrophenol.3rd, preparation method of the invention it is simple, Low production cost, yield and purity are higher, the MnO of synthesis2Nanofiber is that a kind of topography uniformity is strong, specific surface area compared with The good catalyst of high, heat endurance.
Description of the drawings
Fig. 1 is α-MnO of the present invention2Catalyst and presoma δ-MnO2X-ray powder diffraction comparison diagram.
Fig. 2 is α-MnO of the present invention2The scanning electron microscope (SEM) photograph of catalyst.
Fig. 3 is α-MnO of the present invention2Catalyst and presoma δ-MnO2Catalyst is degraded p-nitrophenol under numerous conditions Effect comparison diagram.
Fig. 4 is α-MnO of the present invention2During catalyst degradation p-nitrophenol, under different sample times, all band of filtrate is scanned Figure.
Specific embodiment
Embodiments of the invention are described in further detail below in conjunction with description of the drawings, but the present embodiment is not used to limit The system present invention, every analog structure and its similar change using the present invention, all should list protection scope of the present invention in.
The synthesis of the catalyst material of the present invention：
（1）δ-MnO2Preparation：Weigh 15-18 gram of KOH to be dissolved in the mixed solution of second alcohol and water of 50-100 milliliters, second Alcohol is 1 with the volume ratio of water:1, it is uniformly mixing to obtain solution A.Weigh 4-8 gram of potassium permanganate and be dissolved in 20-40 milliliter deionizations In water, stir and obtain solution B.Solution A is slowly added dropwise in solution B, is sufficiently mixed and is uniformly reacted.Vacuum Suction filtration, is dried 6-12 hours in 80 degree of air dry ovens and obtains final product δ-MnO2。
（2）α-MnO2Preparation：Weigh（1）250 milligrams of the sample of middle drying is dissolved in 65-85 ml deionized waters, surpasses Sound 10-40 minutes；Add the graphene oxide of 2.3 g/l of 10-20 milliliters, ultrasonic 10-40 minutes；Resulting solution is loaded into poly- In tetrafluoroethene reactor, hydro-thermal reaction 24-40 hour in 150 ~ 200 DEG C of Muffle furnaces is put into.The material of Hydrothermal Synthesiss is carried out Vacuum filtration, after multiple deionized water washing, is dried in being put into vacuum drying chamber and obtains final product α-MnO2。
As shown in figure 1, Jing X-ray powder diffraction test results show, the catalyst diffraction that the present invention is synthesized with hydro-thermal method Scheme basic and α-MnO2Standard card（JCPDS NO. 00-029-1020）Correspond, hydro-thermal method used by this explanation present invention Successfully synthesize pure α-MnO2Catalyst.
As shown in Fig. 2 understanding the α-MnO that the present invention synthesizes by Electronic Speculum test result2It is about 50-60 nanometers for diameter Nanofiber.
As shown in figure 3, the present invention compared for p-nitrophenol（4-NP）Auto-degradation, PMS to the degraded of 4-NP and The two kinds of suction-operateds of different crystal forms catalyst to 4-NP and the degradation effect to 4-NP.As pH=3.48, the 25 of 100 milliliters The basic degraded in 80 min of the p-nitrophenol of mg/litre is complete.And presoma δ-MnO2For comparing, degradation efficiency compared with It is secondary.
As shown in figure 4, the present invention is sampled to the degradation experiment of different time, takes filtrate and carry out all band scanning and can obtain All band scanning figure, it is seen that with the carrying out of reaction, the most strong absworption peak at p-nitrophenol 317nm is continuous Reduce, be converted into the absworption peak of other materials, it is final to disappear.
The catalyst of the present invention is nanometer fibrous MnO2；Catalyst synthesized by of the invention can be stronger promotion PMS Selfdecomposition, so that produce more OH and SO4 •Free radical, this degraded to POPs provide the foundation.The carried catalysis of the present invention Agent preparation method is simple, low production cost, yield and purity are higher.Its will environment functional material, sewage disposal, The fields such as heavy metal adsorption have potential application prospect.

Claims (1)

1. a kind of method for preparing manganese dioxide nano catalyst, prepares α-MnO2Nanocatalyst, the catalyst are by two-step method It is synthesized into, δ-MnO is obtained by precipitation method synthesis first2, then by hydro-thermal reaction, by δ-MnO2It is changed into α-MnO2；Which is special Levy is that method and step is as follows：
（1）δ-MnO2Preparation：Weigh 15-18 gram of KOH to be dissolved in the mixed solution of second alcohol and water of 50-100 milliliters, ethanol Volume ratio with water is 1:1, it is uniformly mixing to obtain solution A；
Weigh 4-8 gram of potassium permanganate to be dissolved in 20-40 ml deionized waters, stir and obtain solution B；
Solution A is slowly added dropwise in solution B, is sufficiently mixed and is uniformly reacted；
Vacuum filtration, is dried 6-12 hours in 80 degree of air dry ovens and obtains final product δ-MnO2；
（2）α-MnO2Preparation：Weigh（1）250 milligrams of the sample of middle drying is dissolved in 65-85 ml deionized waters, ultrasonic 10- 40 minutes；
Add the graphene oxide of 2.3 g/l of 10-20 milliliters, ultrasonic 10-40 minutes；
Resulting solution is loaded in ptfe autoclave, hydro-thermal reaction 24-40 hour in 150 ~ 200 DEG C of Muffle furnaces is put into；
The material of Hydrothermal Synthesiss is carried out into vacuum filtration, after multiple deionized water washing, is dried in being put into vacuum drying chamber Obtain final product α-MnO2。
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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN108002443A (en) * 2017-12-04 2018-05-08 清华大学 MnO for normal-temperature deep mineralising phenolic waste water2The preparation method of catalyst and application
CN109012655A (en) * 2018-07-11 2018-12-18 无锡市惠诚石墨烯技术应用有限公司 A kind of preparation method of graphene-sheet manganese dioxide
CN113634261A (en) * 2021-09-14 2021-11-12 莱西市两山环境生态科技中心 Waste water purification material
CN113648998A (en) * 2021-08-11 2021-11-16 北京工业大学 δ-MnO2Method and application of loaded graphene oxide and Ag-Gd composite catalyst
CN114212826A (en) * 2021-11-23 2022-03-22 湖北大学 MnO doped with Mo metal2Electrode material and preparation method and application thereof
CN114832832A (en) * 2022-06-06 2022-08-02 武汉理工大学 Copper doped alpha-MnO 2 -110 catalyst, preparation method and application thereof
CN115092966A (en) * 2022-07-04 2022-09-23 嘉应学院 Mixed-phase MnO of three-dimensional lamellar structure for toluene catalytic combustion 2 Preparation method of (1)
CN115739107A (en) * 2022-11-22 2023-03-07 安徽工业大学 Manganese dioxide nano composite material and preparation method thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108002443A (en) * 2017-12-04 2018-05-08 清华大学 MnO for normal-temperature deep mineralising phenolic waste water2The preparation method of catalyst and application
CN109012655A (en) * 2018-07-11 2018-12-18 无锡市惠诚石墨烯技术应用有限公司 A kind of preparation method of graphene-sheet manganese dioxide
CN113648998A (en) * 2021-08-11 2021-11-16 北京工业大学 δ-MnO2Method and application of loaded graphene oxide and Ag-Gd composite catalyst
CN113648998B (en) * 2021-08-11 2023-10-20 北京工业大学 δ-MnO 2 Method for loading graphene oxide and Ag-Gd composite catalyst and application
CN113634261A (en) * 2021-09-14 2021-11-12 莱西市两山环境生态科技中心 Waste water purification material
CN113634261B (en) * 2021-09-14 2022-05-06 山东环投环境工程有限公司 Waste water purification material
CN114212826A (en) * 2021-11-23 2022-03-22 湖北大学 MnO doped with Mo metal2Electrode material and preparation method and application thereof
CN114212826B (en) * 2021-11-23 2023-08-15 湖北大学 Mo metal doped MnO 2 Electrode material, preparation method and application thereof
CN114832832A (en) * 2022-06-06 2022-08-02 武汉理工大学 Copper doped alpha-MnO 2 -110 catalyst, preparation method and application thereof
CN115092966A (en) * 2022-07-04 2022-09-23 嘉应学院 Mixed-phase MnO of three-dimensional lamellar structure for toluene catalytic combustion 2 Preparation method of (1)
CN115739107A (en) * 2022-11-22 2023-03-07 安徽工业大学 Manganese dioxide nano composite material and preparation method thereof
CN115739107B (en) * 2022-11-22 2024-01-26 安徽工业大学 Manganese dioxide nanocomposite and preparation method thereof

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