CN103831107B - A kind of preparation method of di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst - Google Patents
A kind of preparation method of di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst Download PDFInfo
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- CN103831107B CN103831107B CN201410016007.2A CN201410016007A CN103831107B CN 103831107 B CN103831107 B CN 103831107B CN 201410016007 A CN201410016007 A CN 201410016007A CN 103831107 B CN103831107 B CN 103831107B
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Abstract
The invention discloses composite catalyst of a kind of di-iron trioxide nanometer sheet parcel carbon nano-fiber and preparation method thereof, the nano polypropylene nitrile fiber containing ferric nitrate is obtained by electrostatic spinning, this fiber obtains the polyacrylonitrile-based carbon fibre containing iron oxide seed through super-dry, pre-oxidation and carbonization, then this kind of carbon fiber is placed in the salting liquid of iron content, adopt hydro-thermal method at 140 degree of process certain hours, through washing, drying, namely obtain the composite catalyst of flakey di-iron trioxide nanometer sheet parcel carbon nano-fiber.The present invention adopts containing the carrier of ferric oxide nano carbon fiber as flakey di-iron trioxide, obtained catalytic activity is better than traditional di-iron trioxide, and good stability, have wide practical use in visible ray or natural solar radiation photocatalytic degradation organic pollution, the hydrogen manufacturing of photocatalytic cleavage water, photocatalysis synthetic reaction etc.
Description
Technical field
The invention belongs to the photocatalysis field in applied chemistry, be specifically related to a kind of di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst and preparation method thereof.
Background technology
Energy crisis and environmental pollution have become the global significant problem of 21 century, develop environmentally friendly or to environmental impact minimization new forms of energy solution, by most important to keeping the environment of economic sustainable development and the applicable human living of maintenance.In this respect, with the renewable material such as water, living beings for raw material, solar energy photocatalytic decomposition water, carbon dioxide reduction, degradation of contaminant technology is utilized to be then one of desirable route fundamentally solving the energy and problem of environmental pollution, there is huge economic and social benefit, also meet the active demand of Chinese energy safety strategy and the strategy of sustainable development simultaneously.
Consider the feature of solar energy Spectral structure, the energy conversion efficiency improving solar energy photocatalytic needs the consideration comprehensive from aspects such as band gap, band edge coupling, transferring charge.At present, TiO is developed
2, ZnO, Bi
2o
3, Fe
2o
3etc. having the corresponding nanometer semiconductor oxidation of visible ray, wherein, the Fe of narrow band gap
2o
3(band gap is 2.2eV) due to its low cost, simple to produce, the feature such as the chemical stability of environment friendly and excellence, be considered to a kind of promising catalysis material.But, Fe
2o
3in photoinduced electron--hole, to very difficult separation, is improved its photocatalysis efficiency like this and is met practical application and remain a challenge.
Recently, catalyst is coupled with inert support body to prepare composite catalyst be a kind ofly improve one of method of the research of separation of charge.The people such as Mu report the efficiency that nano zine oxide carbon fiber composite catalyst can significantly improve photocatalytic degradation rhodamine B (RB).Also has the photoinduced electron that some report display carbon nano-fibers can effectively catch and transport.
But at present, above-mentioned technology is also in the developmental research stage, how ripe efficiently by Fe
2o
3catalyst is coupled with carbon nano-fiber and prepares composite catalyst, thus obtain efficient stable meet catalyst, this be still present industrial produce in Focal point and difficult point.
Summary of the invention
Namely object of the present invention is to provide a kind of preparation method of di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst of efficient stable, makes it apply in the reaction of visible ray and natural sunlight catalytic.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst, it mainly comprises two steps, and step one is the preparation of the nano polypropylene itrile group carbon fiber having iron oxide seed; Step 2 is the preparation of the ferric oxide particles of carried by nano carbon fiber.
Preferably, in step one, first take Fe (NO
3)
39H
2o is dissolved in DMF (DMF), carries out magnetic agitation, then takes polyacrylonitrile (PAN), is dispersed to above-mentioned solution, is stirred to solution transparent and homogeneous; Then, electrostatic spinning is carried out, the obtained nano polypropylene nitrile fiber containing ferric nitrate; The nano polypropylene nitrile fiber vacuum drying at a certain temperature containing ferric nitrate obtained by electrostatic spinning, carries out pre-oxidation subsequently, then under inert gas gas shielded, carries out carbonization, thus the obtained nanometer acrylonitrile base carbon fiber containing iron oxide seed.
Preferably, in step 2---in the preparation of the ferric oxide particles of carried by nano carbon fiber, first the nanometer acrylonitrile base carbon fiber containing iron oxide seed obtained in step one and appropriate solution containing iron salts are together put into water heating kettle liner, ultrasonic process a period of time, make solution and the abundant dispersing contact of acrylonitrile base carbon fiber; Build water heating kettle, tighten stainless steel outer cover, by water heating kettle hydro-thermal certain hour under certain high temperature; After having reacted, be cooled to room temperature, spend deionized water, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
By dry in an oven for the carbon fiber loaded iron oxide sample finally obtained, described flakey di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst finally can be obtained.
The di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst obtained by enforcement of the present invention, its catalytic activity is better than traditional Fe
2o
3, and good stability, have wide practical use in visible ray or natural solar radiation photocatalytic degradation organic pollution, the hydrogen manufacturing of photocatalytic cleavage water, photocatalysis synthetic reaction etc.
Accompanying drawing explanation
Fig. 1 is the effect schematic diagram utilizing composite catalyst in the present invention to carry out methyl orange degradation reaction.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
In the present invention, the preparation of composite catalyst mainly comprises two steps: the preparation of the polyacrylonitrile-based carbon fibre containing iron oxide seed; The preparation of the ferric oxide particles of carried by nano carbon fiber.
In step one, first take Fe (NO
3)
39H
2o is dissolved in DMF (DMF), magnetic agitation 2 hours, then takes polyacrylonitrile (PAN), is dispersed to above-mentioned solution, is stirred to solution transparent and homogeneous.Then, solution is moved in glass syringe, carry out electrostatic spinning, the obtained nano polypropylene nitrile fiber containing ferric nitrate.The nano polypropylene nitrile fiber vacuum drying at 60 DEG C containing ferric nitrate that electrostatic spinning is obtained; move into subsequently in baking oven; carry out pre-oxidation in atmosphere, under the protection of inert gas, in carbide furnace, carry out carbonization subsequently, the obtained nanometer acrylonitrile base carbon fiber containing iron oxide seed.
Then step 2 is carried out---the preparation of the ferric oxide particles of carried by nano carbon fiber, first the nanometer acrylonitrile base carbon fiber containing iron oxide seed obtained in step one and appropriate solution containing iron salts are together put into 100mL water heating kettle liner, ultrasonic process 30min, makes solution and the abundant dispersing contact of acrylonitrile base carbon fiber.Build water heating kettle, tighten stainless steel outer cover, water heating kettle is placed in baking oven, hydro-thermal certain hour at 140 DEG C.After having reacted, be cooled to room temperature, spend deionized water, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
By dry in an oven for the iron oxide sample of the carried by nano carbon fiber obtained by above-mentioned two steps, flakey di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst finally can be obtained.
Verified by the degradation experiment of methyl orange by the activity of the di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst prepared by said method, experimental procedure is as follows:
(1) compound concentration is the methyl orange solution of 20mg/L, is placed in volumetric flask, volumetric flask masking foil is wrapped to be placed in lucifuge place for subsequent use, measures 50mL at every turn and uses;
(2) by 0.05g catalyst ultrasonic disperse 15min in 50mL deionized water;
(3) joined by 50mL methyl orange solution in scattered 50mL catalyst suspension, now the concentration of methyl orange is 10mg/L, mixed liquor darkroom is stirred 15min to reach absorption-desorption balance;
(4) reactor that mixed liquor is housed is placed in xenon lamp front irradiation, light source is 300WXe lamp.Add optical filtering with elimination ultraviolet light (λ > 430nm), get primary first-order equation solution every 10min, at every turn about 5mL, centrifugal rear extraction supernatant liquor surveys its absorbance.
Accompanying drawing 1 is the effect schematic diagram utilizing the composite catalyst of final preparation to carry out methyl orange degradation reaction, main body in methyl orange degradation process at regular intervals interval carry out measuring obtained ultraviolet-visible spectrogram, wherein the insertion figure in the upper left corner is that the degradation rate of methyl orange is schemed over time.From this accompanying drawing 1, methyl orange is degradable after illumination 100min, and the composite catalyst prepared by visible the present invention has extremely strong efficient stable.
The above; be only the detailed description of the invention that the present invention is detailed, but protection scope of the present invention is not limited thereto, any people being familiar with this technology is in the technical scope disclosed by the present invention; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (2)
1. a preparation method for di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst, it is characterized in that: this preparation method mainly comprises two steps, step one is the preparation of the nano polypropylene itrile group carbon fiber containing iron oxide seed; Step 2 is, utilizes the nano polypropylene itrile group carbon fiber having iron oxide seed obtained in step one, carries out the preparation of the ferric oxide particles of carried by nano carbon fiber; Finally, the ferric oxide particles of the described carried by nano carbon fiber obtained in step 2 is carried out drying and can obtain di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst; In step one, first take Fe (NO
3)
39H
2o is dissolved in DMF (DMF), carries out magnetic agitation 2 hours, then takes polyacrylonitrile (PAN), is dispersed to above-mentioned solution, is stirred to solution transparent and homogeneous; Then, electrostatic spinning is carried out, the obtained nano polypropylene nitrile fiber containing ferric nitrate; The nano polypropylene nitrile fiber containing ferric nitrate obtained by electrostatic spinning vacuum drying at 60 DEG C of degree temperature, carries out pre-oxidation subsequently, then under the protection of inert gas, carries out carbonization, thus the obtained nanometer acrylonitrile base carbon fiber containing iron oxide seed; In step 2, first the nanometer acrylonitrile base carbon fiber containing iron oxide seed obtained in step one and appropriate solution containing iron salts are together put into 100mL water heating kettle liner, the ultrasonic process 30min time, make solution and the abundant dispersing contact of acrylonitrile base carbon fiber; Build water heating kettle, tighten stainless steel outer cover, by water heating kettle hydro-thermal certain hour under 140 DEG C of degree high temperature; After having reacted, be cooled to room temperature, spend deionized water, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
2. a di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst, is characterized in that: it obtained by the preparation method in claim 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3275836A4 (en) * | 2015-03-27 | 2018-11-14 | Fuji Chemical Industry Co., Ltd. | Novel composite of iron compound and graphene oxide |
| CN104986804B (en) * | 2015-08-12 | 2016-09-07 | 兰州大学 | Preparation γ-Fe2o3the method of magnetic nanoparticle |
| CN108630921B (en) * | 2018-04-24 | 2020-04-21 | 西安科技大学 | Preparation method of iron oxide/carbon fiber composite lithium ion battery cathode material |
| CN110075825A (en) * | 2019-05-08 | 2019-08-02 | 陕西科技大学 | A kind of fiber-loaded bismuth oxide nanometer sheet of large-size carbon and preparation method thereof |
| CN112695452A (en) * | 2020-12-16 | 2021-04-23 | 吉林农业大学 | Flexible three-dimensional magnetic nanofiber material and preparation method and application thereof |
| CN113260244B (en) * | 2021-05-14 | 2022-10-04 | 同济大学 | Composite material and preparation method and application thereof |
| CN113337900B (en) * | 2021-06-02 | 2023-05-26 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
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| WO2005045115A1 (en) * | 2003-11-10 | 2005-05-19 | Teijin Limited | Carbon fiber nonwoven fabric, and production method and use thereof |
| CN101455975A (en) * | 2007-12-14 | 2009-06-17 | 北京化工大学 | Porous carbon nanometer fiber-supported nanocrystal catalyst and preparation method thereof |
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Effective date of registration: 20170602 Address after: 523085 Guangdong city of Dongguan province water Road No. 96 branch of the international information industry park 20 Patentee after: Guangdong Vojssen environmental protection Polytron Technologies Inc Address before: 710049 Xianning West Road, Shaanxi, China, No. 28, No. Patentee before: Xi'an Jiaotong University |