CN103831107A - Preparation method of catalyst with ferric oxide nanosheet-coated nanometer carbon fibers - Google Patents
Preparation method of catalyst with ferric oxide nanosheet-coated nanometer carbon fibers Download PDFInfo
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- CN103831107A CN103831107A CN201410016007.2A CN201410016007A CN103831107A CN 103831107 A CN103831107 A CN 103831107A CN 201410016007 A CN201410016007 A CN 201410016007A CN 103831107 A CN103831107 A CN 103831107A
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Abstract
The invention discloses a composite catalyst with ferric oxide nanosheet-coated nanometer carbon fibers, and a preparation method thereof. The preparation method comprises the following steps: preparing ferric nitrate-containing nanometer polyacrylonitrile fibers by electrostatic spinning, drying, pre-oxidizing and carbonizing the fibers to prepare polyacrylonitrile-based carbon fibers with iron oxide seeds, putting the carbon fibers in an iron-containing salt solution, treating the solution at 140 DEG C for a certain time by a hydrothermal method, then washing and drying to obtain the composite catalyst with scaly ferric oxide nanosheet-coated nanometer carbon fibers. According to the invention, iron oxide-containing nanometer carbon fibers are used as carriers of scaly ferric oxide, and the prepared composite catalyst has better catalytic activity than traditional ferric oxide, has good stability, and has wide application prospects in aspects of photocatalytic degradation of organic pollutants in visible light or natural sun light, hydrogen production by photocatalytic cracking of water, photocatalytic synthetic reactions, and the like.
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 new forms of energy solution environmentally friendly or to environmental impact minimization, by keeping economic sustainable development and maintaining that to be applicable to the environment of human living most important.In this respect, take the renewable material such as water, living beings as raw material, utilizing solar energy photocatalytic decomposition water, carbon dioxide reduction, degradation of contaminant technology is one of desirable approach 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 that solar spectral distributes, the energy conversion efficiency that improves solar energy photocatalytic need to be from comprehensive considerations in aspect such as band gap, band edge coupling, electric charge transmission.At present, developed TiO
2, ZnO, Bi
2o
3, Fe
2o
3deng thering is the corresponding nanometer semiconductor oxidation of visible ray, wherein, the Fe of narrow band gap
2o
3(band gap is 2.2eV), due to features such as its low cost, simple production, environment friendly and excellent chemical stabilities, has been considered to a kind of promising catalysis material.But, Fe
2o
3in photic electronics--hole separates being difficult to, and improves like this its photocatalysis efficiency and meets practical application and remain a challenge.
Recently, the coupling of catalyst and inertia supporter being prepared to composite catalyst is one of a kind of method of research that improves separation of charge.The people such as Mu have reported that nano zine oxide carbon fiber composite catalyst can significantly improve the efficiency of photocatalytic degradation rhodamine B (RB).Also have some reports to show the photic electronics that carbon nano-fiber can effectively catch and transport.
But at present, above-mentioned technology is also in the developmental research stage, how maturation is efficiently by Fe
2o
3composite catalyst is prepared in the coupling of catalyst and carbon nano-fiber, thereby obtains the catalyst that meets of efficient stable, and this is still the Focal point and difficult point in industrial production now.
Summary of the invention
Object of the present invention is the preparation method of the di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst that a kind of efficient stable is provided, and it is applied 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, step 1 is the preparation that has the nano polypropylene itrile group carbon fiber of iron oxide seed; Step 2 is the preparation of the ferric oxide particles of carried by nano carbon fiber.
Preferably, in step 1, 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, carry out electrostatic spinning, make the nano polypropylene nitrile fiber that contains ferric nitrate; The nano polypropylene nitrile fiber vacuum drying at a certain temperature that contains ferric nitrate that electrostatic spinning is made, carries out pre-oxidation subsequently, then under the protection of inert gas gas, carries out carbonization, thereby makes the nanometer acrylonitrile base carbon fiber that contains 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 that contains iron oxide seed making in step 1 and appropriate solution containing iron salts are together put into water heating kettle liner, ultrasonic processing a period of time, make solution and acrylonitrile base carbon fiber fully disperse to contact; 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, with deionized water washing, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
The carbon fiber loaded iron oxide sample finally obtaining is dry in baking oven, finally can make described flakey di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst.
The di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst obtaining by enforcement of the present invention, its catalytic activity is better than traditional Fe
2o
3, and good stability, has wide practical use at aspects such as visible ray or natural solar radiation photocatalytic degradation organic pollution, the hydrogen manufacturing of photocatalytic cleavage water, the synthetic reactions of photocatalysis.
Accompanying drawing explanation
Fig. 1 utilizes the effect schematic diagram that in the present invention, composite catalyst carries out methyl orange degradation reaction.
The specific embodiment
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 that contains iron oxide seed; The preparation of the ferric oxide particles of carried by nano carbon fiber.
In step 1, first take Fe (NO
3)
39H
2o is dissolved in DMF (DMF), magnetic agitation 2 hours, then take polyacrylonitrile (PAN), and be dispersed to above-mentioned solution, be stirred to solution transparent and homogeneous.Then, solution is moved in glass syringe, carry out electrostatic spinning, make the nano polypropylene nitrile fiber that contains ferric nitrate.The nano polypropylene nitrile fiber vacuum drying at 60 ℃ that contains ferric nitrate that electrostatic spinning is made; move into subsequently in baking oven; in air, carry out pre-oxidation, under the protection of inert gas, in carbide furnace, carry out subsequently carbonization, make the nanometer acrylonitrile base carbon fiber that contains iron oxide seed.
Then carry out step 2---the preparation of the ferric oxide particles of carried by nano carbon fiber, first the nanometer acrylonitrile base carbon fiber that contains iron oxide seed making in step 1 and appropriate solution containing iron salts are together put into 100mL water heating kettle liner, ultrasonic processing 30min, makes solution and acrylonitrile base carbon fiber fully disperse to contact.Build water heating kettle, tighten stainless steel outer cover, water heating kettle is placed in to baking oven, hydro-thermal certain hour at 140 ℃.After having reacted, be cooled to room temperature, with deionized water washing, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
The iron oxide sample of the carried by nano carbon fiber obtaining by above-mentioned two steps is dry in baking oven, finally can make flakey di-iron trioxide nanometer sheet parcel nanocarbon fiber composite catalyst.
Wrapping up the activity of nanocarbon fiber composite catalyst can verify by the degradation experiment of methyl orange by the prepared di-iron trioxide nanometer sheet of said method, and experimental procedure is as follows:
(1) methyl orange solution that compound concentration is 20mg/L, is placed in volumetric flask, volumetric flask is wrapped with masking foil to be placed in lucifuge place for subsequent use, measures 50mL at every turn and uses;
(2) by ultrasonic 0.05g catalyst dispersion 15min in 50mL deionized water;
(3) 50mL methyl orange solution is joined in scattered 50mL catalyst suspension, now the concentration of methyl orange is 10mg/L, and 15min is stirred to reach absorption-desorption balance in mixed liquor darkroom;
(4) reactor that mixed liquor is housed is placed in to 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, each about 5mL, centrifugal rear extraction supernatant liquor is surveyed its absorbance.
The effect schematic diagram of accompanying drawing 1 for 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 measure obtained ultraviolet-visible spectrogram, the degradation rate that wherein the insertion figure in the upper left corner is methyl orange is schemed over time.From this accompanying drawing 1, methyl orange is degradable after illumination 100min, and the visible prepared composite catalyst of the present invention has extremely strong efficient stable.
The above; be only the detailed specific embodiment of the present invention, but protection scope of the present invention is not limited to this, any people who is familiar with this technology is in the disclosed technical scope of the present invention; the variation that can expect easily or replacement, within all should being encompassed in 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 (4)
1. a preparation method for di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst, is characterized in that: this preparation method mainly comprises two steps, and step 1 is the preparation of the nano polypropylene itrile group carbon fiber that contains iron oxide seed; Step 2 is, utilizes the nano polypropylene itrile group carbon fiber that has iron oxide seed making in step 1, carries out the preparation of the ferric oxide particles of carried by nano carbon fiber.
2. the preparation method of a kind of di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst according to claim 1, is characterized in that: preferred, in step 1, 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, carry out electrostatic spinning, make the nano polypropylene nitrile fiber that contains ferric nitrate; The nano polypropylene nitrile fiber vacuum drying at a certain temperature that contains ferric nitrate that electrostatic spinning is made, carries out pre-oxidation subsequently, then under the protection of inert gas, carries out carbonization, thereby makes the nanometer acrylonitrile base carbon fiber that contains iron oxide seed.
3. the preparation method of a kind of di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst according to claim 1 and 2, it is characterized in that: preferred, in step 2, first the nanometer acrylonitrile base carbon fiber that contains iron oxide seed making in step 1 and appropriate solution containing iron salts are together put into water heating kettle liner, ultrasonic processing a period of time, make solution and acrylonitrile base carbon fiber fully disperse to contact; 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, with deionized water washing, centrifugal several times, obtain the iron oxide sample of carried by nano carbon fiber.
4. a di-iron trioxide nanometer sheet parcel carbon nano-fiber catalyst, is characterized in that: its preparation method by any one in claim 13 obtains.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104986804A (en) * | 2015-08-12 | 2015-10-21 | 兰州大学 | Method for preparing gamma-Fe2O3 magnetic nano-particles |
| CN107531489A (en) * | 2015-03-27 | 2018-01-02 | 富士化学工业株式会社 | The complex of new iron compound and graphene oxide |
| CN108630921A (en) * | 2018-04-24 | 2018-10-09 | 西安科技大学 | The preparation method of ferriferous 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 |
| CN113260244A (en) * | 2021-05-14 | 2021-08-13 | 同济大学 | Composite material and preparation method and application thereof |
| CN113337900A (en) * | 2021-06-02 | 2021-09-03 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107531489A (en) * | 2015-03-27 | 2018-01-02 | 富士化学工业株式会社 | The complex of new iron compound and graphene oxide |
| CN104986804A (en) * | 2015-08-12 | 2015-10-21 | 兰州大学 | Method for preparing gamma-Fe2O3 magnetic nano-particles |
| CN108630921A (en) * | 2018-04-24 | 2018-10-09 | 西安科技大学 | The preparation method of ferriferous 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 |
| CN113260244A (en) * | 2021-05-14 | 2021-08-13 | 同济大学 | Composite material and preparation method and application thereof |
| CN113337900A (en) * | 2021-06-02 | 2021-09-03 | 西安交通大学 | Photocatalytic fabric and preparation method and application thereof |
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| CN103831107B (en) | 2016-01-06 |
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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 |