CN104550994A - Method for visible light reducing ferric salt to iron nanoparticles in water solution - Google Patents
Method for visible light reducing ferric salt to iron nanoparticles in water solution Download PDFInfo
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- CN104550994A CN104550994A CN201310495758.2A CN201310495758A CN104550994A CN 104550994 A CN104550994 A CN 104550994A CN 201310495758 A CN201310495758 A CN 201310495758A CN 104550994 A CN104550994 A CN 104550994A
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Abstract
The invention relates to a method for visible light reducing ferric salt to iron nanoparticles in water solution and belongs to the field of photocatalytic technology and environmental science. The reduced iron nanoparticles can serve as a catalyst for photocatalytic water splitting for hydrogen production. The method includes adopting an LED lamp as the light source approximate to the sunlight, and performing reduction in the water solution containing organic dye photosensitizer and electron donor triethylamine. The method has the advantages that the iron nanoparticles obtained through photoreduction have small particle diameter and high activity, the iron nanoparticles can serve as the catalyst for photocatalytic water splitting, and the catalyst can be separated from the system easily to reuse; the method is easy and simple to implement and low in cost, and the environment protecting and energy saving requirements are met.
Description
Technical field
The present invention relates to a kind of in water visible ray reduction molysite produce Fe nanometer particles and the Fe nanometer particles that obtains can be used as catalyst application in photolysis water hydrogen, belong to photocatalysis technology and environmental science.
Background technology
Fe nanometer particles has a wide range of applications in materialogy fields such as high density magnetic pipe recording material, magnetic liquid, electric conductor, electromagnetically absorbing material, biomedical carrier and corrosion resistant coatings.Due to chemistry and the physical characteristic of its uniqueness, its application is made to obtain further expansion, as: as a kind of important combustion adjuvant and effective catalyst etc.Since German Gleiter H prepared the Fe nanometer particles of 6nm first in 1984, flourish to the research of nano metal in the world, and make great progress.At present, the common method of synthesis of nano iron granules has: physical method (comprises physical vaporous deposition, high-energy ball milling method, degree of depth modification method etc.) and chemical method (comprise solid state chemistry reducing process, solution phase chemical reduction, pyrolysis carbonyl iron is sent out, microemulsion method, electrodeposition process etc.).There is the features such as the not good and productive rate of non-oxidizability is low in the nano-iron particle of these methods synthesis, is unfavorable for the later stage application of product.At present, the method generally adopted adds various stabilizing agent exactly and is formed on surface coated, is conducive to improving its non-oxidizability.
Photolysis water hydrogen is the approach solving global energy crisis, and in photolysis water hydrogen, most critical is exactly find efficient and cheap catalyst, and iron is rich reserves on earth, and Fe nanometer particles is the candidate of an outstanding catalyst.Fe nanometer particles has been reported as the catalyst of photolysis water hydrogen, does not just also search out the way improving its efficiency.
Summary of the invention
The method that the object of the invention is to use up reduction molysite obtains Fe nanometer particles, and is applied in photolysis water hydrogen system by the Fe nanometer particles obtained.
Method of the present invention adds sensitising agent organic dyestuff (as fluorescein) in aqueous, metal molysite and sacrifice agent triethylamine or triethanolamine, nitrogen deoxygenation 30 minutes, illumination 4 hours under the LED of approximate sunshine, centrifugation obtains Nanoscale Iron, then joins photolysis water hydrogen in other system.
Described method is that sample solution adopts visible LED light photograph, and uses gas chromatographic detection amounts of hydrogen, and continuous illumination, after 12 hours, is led to nitrogen, continued illumination 12 hours after deoxygenation for second day again.Along with the prolongation of light application time, the hydrogen-producing speed of sample solution reduces, until hydrogen output no longer increases.
Described method is by the Fe nanometer particles centrifugation of photo-reduction generation out, spend deionized water more than 5 times, join in the sample cell containing fluorescein sensitising agent and triethylamine (triethanolamine) the sacrifice agent aqueous solution, can continue to produce hydrogen by system after nitrogen deoxygenation.
Experimental result shows, sample solution is after illumination 30min, start have black particle thing to occur in pipe, system also starts to produce hydrogen, continue illumination black particle thing can be on the increase, hydrogen generation rate increases, and illumination is after 4 hours, molysite reduces completely substantially, at this time produces hydrogen and enters the fastest period.Due to the continuous consumption of sacrifice agent, illumination after 10 hours system hydrogen-producing speed can decline, total amounts of hydrogen continues to increase, illumination after 20 hours hydrogen total amount not in increase.By the black particle centrifugation in system out, wash 5 times by deionized water, join the sample cell that another contains fluorescein and triethylamine (triethanolamine) aqueous solution, after nitrogen deoxygenation, illumination can continue to produce hydrogen.
Outstanding meaning of the present invention is:
1. different with the method for traditional electronation, the present invention uses the method for photo-reduction to obtain Fe nanometer particles.
2.LED lamp is very similar to the sunshine visible part that earth surface receives, can well analog solar.
3. the Fe nanometer particles obtained that reduces is the catalyst that a kind of activity is higher, reusable in the system of photolysis water hydrogen.
Accompanying drawing explanation
The TEM photo of Fig. 1 Fe nanometer particles
The XRD of Fig. 2 Fe nanometer particles
Fig. 3 photo-reduction system hydrogen output is with the change of light application time
Detailed description of the invention
The preparation of Fe nanometer particles
Embodiment: by 10mg organic dyestuff (as fluorescein), 1mL triethylamine (triethanolamine) and 3mg FeCl
3join in 30mL deionized water, 3W × 6LED illumination.After having black particle produce raw, centrifugation, wash 5 times, ethanol is washed, and obtains iron nano-particle, carries out TEM and XRD test.
Photochemical catalyzing
Embodiment one: photolysis water hydrogen occurs in be prepared in the reaction system of Fe nanometer particles, when starting in system to produce Fe nanometer particles, just has hydrogen to start to produce.Reaction vessel is 60mL quartz test tube, and deionized water water volume is 30mL, adds 10mg organic dyestuff (as fluorescein), 1mL triethylamine and 3mg FeCl
3after, logical nitrogen 30min removes the oxygen above solution neutralization solution, uses rubber stopper seal.LED lamplight photograph, hydrogen GC-14C (Shimadzu) gas chromatograph produced in system detects,
molecular sieve column (3m × 2mm), thermal conductivity cell detector (TCD), carrier gas is nitrogen, adopts external standard method to measure.
Embodiment two: centrifugation is obtained Fe nanometer particles and join in the 30mL deionized water solution that 10mg organic dyestuff (fluorescein) and 1mL triethylamine are housed, other steps and experiment condition identical with embodiment one.
Claims (5)
1. visible ray reduction molysite produces a method for Fe nanometer particles, and gained Fe nanometer particles can be used as the catalyst of photocatalysis hydrogen production.
2. according to method described in claim 1, it is characterized in that, organic dyestuff is the sensitising agent of system.
3. according to method described in claim 1, it is characterized in that, whole process must have visible ray to participate in.
4. the photo-reduction molysite according to any one of claims 1 to 3 produces a method for Nanoscale Iron, and adopt pure water as solvent, triethylamine or triethanolamine are electron donor, utilizes the LED light source of approximate sunshine to irradiate sample solution, until hydrogen no longer produces.
5. the nano-iron particle described in claim 4, can obtain in centrifugation, joins the catalyst of other systems continuation as Photocatalyzed Hydrogen Production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310495758.2A CN104550994A (en) | 2013-10-22 | 2013-10-22 | Method for visible light reducing ferric salt to iron nanoparticles in water solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310495758.2A CN104550994A (en) | 2013-10-22 | 2013-10-22 | Method for visible light reducing ferric salt to iron nanoparticles in water solution |
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| CN104550994A true CN104550994A (en) | 2015-04-29 |
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| CN201310495758.2A Pending CN104550994A (en) | 2013-10-22 | 2013-10-22 | Method for visible light reducing ferric salt to iron nanoparticles in water solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642913A (en) * | 2016-03-25 | 2016-06-08 | 北京理工大学 | Method for preparing polymorphic gold nano-structure by using laser-inducing material through reduction |
| CN108722395A (en) * | 2018-06-25 | 2018-11-02 | 北方民族大学 | A kind of platinum nano catalyst and its hydrogen production process prepared using vinifera residue |
-
2013
- 2013-10-22 CN CN201310495758.2A patent/CN104550994A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642913A (en) * | 2016-03-25 | 2016-06-08 | 北京理工大学 | Method for preparing polymorphic gold nano-structure by using laser-inducing material through reduction |
| CN105642913B (en) * | 2016-03-25 | 2017-09-22 | 北京理工大学 | A kind of method that laser-induced material reproducibility prepares polymorphic gold nano structure |
| CN108722395A (en) * | 2018-06-25 | 2018-11-02 | 北方民族大学 | A kind of platinum nano catalyst and its hydrogen production process prepared using vinifera residue |
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Application publication date: 20150429 |