CN104707658A - Pd/metal-organic framework compound catalyst as well as preparation method and application thereof - Google Patents
Pd/metal-organic framework compound catalyst as well as preparation method and application thereof Download PDFInfo
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- CN104707658A CN104707658A CN201510089157.0A CN201510089157A CN104707658A CN 104707658 A CN104707658 A CN 104707658A CN 201510089157 A CN201510089157 A CN 201510089157A CN 104707658 A CN104707658 A CN 104707658A
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Abstract
The invention discloses a Pd/metal-organic framework compound catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: dispersing MIL-100(Fe) in an ethanol-water mixed solution, adding polyvinylpyrrolidone and H2PdCl4 under continuous stirring, and performing reflux with an oil bath for 3 h at 90 DEG C so as to obtain the Pd/MIL-100(Fe) composite material, wherein during the process, Pd(2+) can be reduced by ethanol gradually. According to the invention, a simple and mild method for reducing precious metal by ethanol is adopted, high-dispersity precious metal Pd nano-particles grow on MIL-100(Fe) with a super-large specific area, and in the whole process, inert atmosphere, a strong reducing agent and heat treatment process are not required. The prepared Pd nano-particles are good in dispersity, and high in utilization ratio, and have the property of efficiently degrading medicines, personal care products or dyes in the water environment through photocatalysis at the room temperature.
Description
Technical field
The invention belongs to the catalysis technical field in the energy, environmental improvement, be specifically related to a kind of Pd/ metal organic framework compound Catalysts and its preparation method and application.
Background technology
Metallic organic framework (Metal-Organic Frameworks, MOFs) material is is node to a class with metal cation, have the general name of the micropore-mesopore metal organic coordination polymer that the organic ligand of multiple tooth coordination is connector.MOFs material is as the fresh combatants of new generation of porous material, having the feature common with conventional porous materials---the while of porous, the feature of MOFs material self, as duct can cut out, modifiability, it is functional that metal center is given, unsatuated metal site and dynamic frame shelf structure etc. make MOFs material be separated in gas storage, drug delivery, and all many-sides of optical, electrical, magnetics and photocatalysis etc. have huge application prospect.In recent years, the photocatalysis technology based on MOFs material gets more and more people's extensive concerning.
But in conjunction with the actual conditions of photocatalytic applications, we find that the photocatalysis technology based on MOFs material of at present research still also exists the low height of photo-generated carrier separative efficiency and the lower many problems of solar energy utilization ratio.For optimizing the performance of MOFs photochemical catalyst further, many functional entities are introduced in MOFs, such as metal oxide, material with carbon element and noble metal.Wherein the noble metal such as Au, Pd, Ag and Pt has the performances such as excellent electricity, catalysis, is of great value in basic research and practical application area and becomes current study hotspot.Noble metal nano particles is evenly spread in MOFs material surface or duct and make composite, the efficiency that the visible absorption performance that can not only strengthen MOFs material is separated with raising photo-generated carrier, and the cooperative effect of some novelties may be produced.The method being used for preparing noble metal/MOFs composite at present has a lot, and relatively more conventional having is following several: chemical reduction method, chemical vapour deposition (CVD) and electrochemical reduction.But said method also exists many weak points, such as: above reaction method is usually more consuming time, severe reaction conditions.The noble metal organic ligand of usual needs costliness.Usually need in course of reaction to add reducing agent such as sodium borohydride etc., and noble metal granule easily causes a large amount of reunions of particle in reduction process, average particle size is excessive, therefore effectively can not shift and be separated photo-generated carrier.MOFs is the very responsive class material of a kind of environment to external world, and strong reductant likely can affect to the structure of carrier itself in course of reaction.Therefore be necessary that exploitation is a kind of simple and noble metal is deposited on the surface of MOFs by effective method, and do not need complicated equipment, inert atmosphere and expensive organic ligand.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of Pd/MOFs Catalysts and its preparation method and application are provided, by gentleness, palladium ion is reduced into the surface of atomic deposition at carrier by simple ethanol reduction method, solve in prior art prepare noble metal/MOFs composite catalyst consuming time, the problem such as generally can not to be suitable for, obtained noble metal/MOFs composite can be applicable to photocatalysis field.This preparation method is simple, does not need equipment and inert atmosphere, the synthesis condition gentleness of complex and expensive, and can be extended in the application of other carrier.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Pd/MOFs catalyst, the particle diameter of Pd nano particle is 6 nm, and carrier is MIL-100 (Fe).
Preparation method: by ethanol, water, polyvinylpyrrolidone, H
2pdCl
4mix with carrier, after stirring 30 min, 90 DEG C of backflow 3 h.Finally products therefrom is centrifugal, wash away excess ions by deionized water after, 60 DEG C of vacuum drying, obtained Pd/MOFs catalyst.
Described Pd/MOFs catalyst can be applied to light at room temperature and urge falling and dissolve medicine in water environment and the field such as personal-care supplies or dyestuff.
Remarkable advantage of the present invention is:
1) the present invention was from noble metal method for preparing composite catalyst was different in the past: conventional method mainly passes through immersion reduction method, deposition-precipitation method carried noble metal at carrier surface, but preparation method of the present invention is gentle simple ethanol reduction method, in this process, complicated equipment, inert atmosphere and expensive organic ligand is not needed.Also solve the shortcoming destroying carrier structure in conventional method while strong reductant reduction noble metal simultaneously;
2) in the catalyst that obtains of preparation method of the present invention, palladium particle is less, even, and the particle diameter of prepared palladium nano-particles is about 6 nm, at carrier surface good dispersion, does not have agglomeration, and has stronger interaction between noble metal and carrier.Thus make the catalyst of preparation have good catalytic activity;
3) preparation method of the present invention's employing is simple, is conducive to large-scale popularization, has very large universality.Many noble metals (as gold, silver, platinum, copper, nickel etc.) can successfully adopt this technology to load on carrier.Therefore, by adding two or more precious metal salt, thus precious metal alloys loaded catalyst can be prepared, and the load capacity of noble metal can be changed by the addition changing precious metal salt to a great extent;
4) catalyst utilizing the present invention to prepare, can be applied to medicine in light at room temperature catalytic degradation water environment and personal-care supplies or dyestuff.This catalyst can carry out separating treatment easily, and recycling efficiency is high, has very high practical value and application prospect.And this catalyst also can be applicable to degradable organic pollutant, the process of such as room air and water; With energy aspect, such as photocatalytic water prepares the fields such as hydrogen.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst;
Fig. 2 is the transmission electron microscope picture of the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst;
Fig. 3 is that the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst room temperature photocatalytic degradation theophylline is active;
Fig. 4 is that the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst room temperature photocatalytic degradation brufen is active;
Fig. 5 is that the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst room temperature photocatalytic degradation bisphenol-A is active;
Fig. 6 is that the embodiment of the present invention 1 gained Pd/MIL-100 (Fe) catalyst room temperature photo-catalytic degradation of methyl-orange is active.
Detailed description of the invention
The present invention proposes a kind of general, noble metal/MOFs method for preparing composite catalyst and application thereof fast.Utilize the ethanol with certain reducing power as reducing agent, utilize its reducing power to react with the precious metal cation with oxidability in a heated condition.In this process, complicated equipment, inert atmosphere and expensive organic ligand is not needed.The carrier of photochemical catalyst of the present invention is MIL-100 (Fe).Using ethanol as the method for reducing agent reduction Pd ion, the particle diameter of Pd nano particle is about 6 nm.
The preparation process of MIL-100 (Fe) carrier is as follows: take a certain amount of iron powder (Fe) respectively by certain mol ratio, trimesic acid (H
3bTC) and the hydrofluoric acid of certain volume (HF), red fuming nitric acid (RFNA) (HNO
3) and water (H
2o), each ratio of component is n(Fe): n(H
3bTC): n(HF): n(HNO
3): n(H
2o)=1:0.67:2:0.6; 277, after mix and blend about 5 min, be transferred in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle.Put into electric heating air blast thermostatic drying chamber after airtight, after being warming up to 150 DEG C, constant temperature keeps 24 h.After reaction terminates, hydrothermal reaction kettle is left standstill and be cooled to room temperature, by sample filtering, after washing away with distilled water the excess ions be attached in precipitation, put into drying box freeze-day with constant temperature a few hours, obtain light crocus bulk crystals and be MIL-100 (Fe).Dried sample needs to be further purified with ethanol.First the ethanol of certain volume is added appropriate MIL-100 (Fe) (about 350 mL ethanol/1.0 g MIL-100 (Fe)), under 60 DEG C of conditions, constant temperature stirs 3h, filter, 60 DEG C of vacuum drying, obtained carrier MIL-100 (Fe).By ethanol, water, polyvinylpyrrolidone, H
2pdCl
4mix with carrier, after stirring 30 min, 90 DEG C of backflow 3 h.Finally products therefrom is centrifugal, wash away excess ions by deionized water after, 60 DEG C of vacuum drying, obtained Pd/MOFs catalyst.
embodiment 1
The preparation of Pd/MIL-100 (Fe) catalyst
By the water of the ethanol of 5 mL, 5 mL, 0.333g polyvinylpyrrolidone, 294 μ L H
2pdCl
4(10 mg/mL) mixes with 0.1 g carrier, stirs after 30 min make it to be uniformly dispersed, 90 DEG C of backflow 3 h.Finally products therefrom is centrifugal, wash away excess ions by deionized water after, 60 DEG C of vacuum drying, obtain Pd/MIL-100 (Fe) composite.Fig. 1 illustrates and schemes with the XRD of Pd/MIL-100 (Fe) catalyst synthesized by this preparation method.Fig. 2 illustrates the transmission electron microscope picture with Pd/MIL-100 (Fe) catalyst synthesized by this preparation method.
application examples 1
Pd/MIL-100 (Fe) composite catalyst light at room temperature catalytic degradation medicine and personal-care supplies activity
Experiment has selected three kinds of typical medicines and personal-care supplies as simulating pollution thing: theophylline, brufen and bisphenol-A.Specific experiment step is as follows: get in the medicine and personal-care supplies solution that catalyst that 5 mg are prepared into is scattered in 40 mL (20 mg/L), then add the H of 40 μ L
2o
2, and regulate solution ph to be 4.Above-mentioned dispersion liquid is in the dark adsorbed three hours with reach adsorption/desorption balance after, illumination of turning on light (wavelength is more than or equal to 420 nm).Along with the carrying out of reaction, certain interval of time measures the reaction solution of 3 mL, after centrifugation, gets supernatant liquor and carries out efficient liquid phase chromatographic analysis.In order to the conversion ratio (conversion) of analysis-reduction product, we utilize the reacted solution of efficient liquid phase chromatographic analysis:
Conversion (%) = [(C
0-C
t)/C
0]*100
Wherein C
0it is the initial concentration of pollutant.C
tthe concentration of pollutant after reaction a period of time.
As in Figure 3-5, Pd/MIL-100 (Fe) catalyst shows good photocatalytic activity to response situation.Through the reaction of 240 minutes, most of theophylline, brufen and bisphenol-A can be degraded.These results show that Pd/MIL-100 (Fe) catalyst has the medicine of photocatalytic degradation and the activity of personal-care supplies under higher aqueous phase normal temperature.
application examples 2
The activity of Pd/MIL-100 (Fe) composite catalyst room temperature photo-catalytic degradation of methyl-orange
Specific experiment step is as follows: get the catalyst that 5 mg are prepared into and be scattered in (20 mg/L) in the dye solution of 40 mL, then add the H of 40 μ L
2o
2, and regulate solution ph to be 4.Above-mentioned dispersion liquid is in the dark adsorbed three hours with reach adsorption/desorption balance after, illumination of turning on light (wavelength is more than or equal to 420 nm).Along with the carrying out of reaction, certain interval of time measures the reaction solution of 3 mL, after centrifugation, gets supernatant liquor and carries out ultraviolet-visible analysis of spectrum.Sweep limits is 200 ~ 800 nm.In order to the conversion ratio (conversion) of analysis-reduction product, the method for calculating is with above.
As shown in Figure 6, Pd/MIL-100 (Fe) catalyst shows good photocatalytic activity to response situation.Through the reaction of 150 minutes, most of methyl orange can be degraded.These results show that Pd/MIL-100 (Fe) catalyst has Photocatalytic activity under higher aqueous phase normal temperature.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a Pd/ metal organic framework compound catalyst, is characterized in that: in Pd/MOFs, the particle diameter of Pd nano particle is 6 nm.
2. Pd/ metal organic framework compound catalyst according to claim 1, is characterized in that: carrier is metal-organic framework materials MIL-100 (Fe).
3. prepare a method for Pd/ metal organic framework compound catalyst as claimed in claim 1, it is characterized in that: by ethanol, water, polyvinylpyrrolidone, H
2pdCl
4mix with carrier, after stirring 30 min, 90 DEG C of backflow 3 h, centrifugal, washing, 60 DEG C of vacuum drying, obtained Pd/MOFs catalyst.
4. an application for Pd/ metal organic framework compound catalyst as claimed in claim 1, is characterized in that: described Pd/MOFs catalyst is used for medicine, personal-care supplies or dyestuff in light at room temperature catalytic degradation water environment.
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|---|---|---|---|---|
| CN105107505A (en) * | 2015-07-02 | 2015-12-02 | 上海应用技术学院 | Magnetic TiO2-porous carbon-Fe3O4 composite visible light photocatalyst and preparation method thereof |
| CN105233869A (en) * | 2015-09-22 | 2016-01-13 | 天津工业大学 | Preparation method and applications of porous composite material with peroxidase activity |
| CN105396619A (en) * | 2015-12-11 | 2016-03-16 | 华南理工大学 | MIL-100(Fe) silver phosphate composite photocatalyst, preparation and applications |
| CN105618142A (en) * | 2016-01-08 | 2016-06-01 | 福州大学 | Pd@MIL-100(Fe) as well as preparation method and application thereof |
| CN106732797A (en) * | 2016-12-08 | 2017-05-31 | 福州大学 | A kind of phosphotungstic acid loading type Pd metal organic framework catalyst |
| CN107262153A (en) * | 2017-08-07 | 2017-10-20 | 福州大学 | A kind of preparation method of Pd/MIL 100 (Fe) photochemical catalyst |
| CN107349963A (en) * | 2017-07-05 | 2017-11-17 | 辽宁大学 | A kind of composites of Pt@MIL 101 and its preparation method and application |
| CN107537571A (en) * | 2017-10-23 | 2018-01-05 | 南京工程学院 | A kind of multi-walled carbon nanotube noble metal catalyst and preparation method thereof |
| CN107834076A (en) * | 2017-11-16 | 2018-03-23 | 皖南医学院 | A kind of porous nano palladium, preparation method and applications, a kind of preparation method of porous palladium dydroxide nanosphere |
| CN107913741A (en) * | 2016-10-09 | 2018-04-17 | 天津工业大学 | A kind of preparation method of 199 load nano particle composite materials of MOF |
| CN108636453A (en) * | 2018-04-08 | 2018-10-12 | 浙江工业大学 | A kind of nano-noble metal catalyst and its preparation method and application of metal-organic framework material encapsulation |
| CN109647381A (en) * | 2017-10-12 | 2019-04-19 | 中国科学院福建物质结构研究所 | A kind of method of the mesoporous C-base composte material of controllable preparation platinum grain high degree of dispersion as highly effective hydrogen yield elctro-catalyst |
| CN111359660A (en) * | 2020-04-10 | 2020-07-03 | 蚌埠学院 | Method for preparing palladium-loaded polyimide nanosheet by microwave ionothermal method and application of palladium-loaded polyimide nanosheet in catalytic degradation of printing and dyeing wastewater |
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Cited By (20)
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| CN105107505A (en) * | 2015-07-02 | 2015-12-02 | 上海应用技术学院 | Magnetic TiO2-porous carbon-Fe3O4 composite visible light photocatalyst and preparation method thereof |
| CN105107505B (en) * | 2015-07-02 | 2017-11-28 | 上海应用技术学院 | A kind of magnetic TiO2Porous carbon Fe3O4Composite visible light catalyst and preparation method thereof |
| CN105233869A (en) * | 2015-09-22 | 2016-01-13 | 天津工业大学 | Preparation method and applications of porous composite material with peroxidase activity |
| CN105396619A (en) * | 2015-12-11 | 2016-03-16 | 华南理工大学 | MIL-100(Fe) silver phosphate composite photocatalyst, preparation and applications |
| CN105618142A (en) * | 2016-01-08 | 2016-06-01 | 福州大学 | Pd@MIL-100(Fe) as well as preparation method and application thereof |
| CN105618142B (en) * | 2016-01-08 | 2018-05-04 | 福州大学 | A kind of Pd@MIL-100 (Fe) and preparation method and application |
| CN107913741A (en) * | 2016-10-09 | 2018-04-17 | 天津工业大学 | A kind of preparation method of 199 load nano particle composite materials of MOF |
| CN106732797A (en) * | 2016-12-08 | 2017-05-31 | 福州大学 | A kind of phosphotungstic acid loading type Pd metal organic framework catalyst |
| CN107349963A (en) * | 2017-07-05 | 2017-11-17 | 辽宁大学 | A kind of composites of Pt@MIL 101 and its preparation method and application |
| CN107262153A (en) * | 2017-08-07 | 2017-10-20 | 福州大学 | A kind of preparation method of Pd/MIL 100 (Fe) photochemical catalyst |
| CN109647381A (en) * | 2017-10-12 | 2019-04-19 | 中国科学院福建物质结构研究所 | A kind of method of the mesoporous C-base composte material of controllable preparation platinum grain high degree of dispersion as highly effective hydrogen yield elctro-catalyst |
| CN109647381B (en) * | 2017-10-12 | 2020-08-28 | 中国科学院福建物质结构研究所 | Method for controllably preparing highly-dispersed mesoporous carbon-based composite material of platinum particles as efficient hydrogen production electrocatalyst |
| CN107537571A (en) * | 2017-10-23 | 2018-01-05 | 南京工程学院 | A kind of multi-walled carbon nanotube noble metal catalyst and preparation method thereof |
| CN107537571B (en) * | 2017-10-23 | 2020-09-18 | 南京工程学院 | Multi-walled carbon nanotube-based noble metal catalyst and preparation method thereof |
| CN107834076A (en) * | 2017-11-16 | 2018-03-23 | 皖南医学院 | A kind of porous nano palladium, preparation method and applications, a kind of preparation method of porous palladium dydroxide nanosphere |
| CN108636453A (en) * | 2018-04-08 | 2018-10-12 | 浙江工业大学 | A kind of nano-noble metal catalyst and its preparation method and application of metal-organic framework material encapsulation |
| CN108636453B (en) * | 2018-04-08 | 2020-11-13 | 浙江工业大学 | Nano noble metal catalyst packaged by metal organic framework material and preparation method and application thereof |
| CN111359660A (en) * | 2020-04-10 | 2020-07-03 | 蚌埠学院 | Method for preparing palladium-loaded polyimide nanosheet by microwave ionothermal method and application of palladium-loaded polyimide nanosheet in catalytic degradation of printing and dyeing wastewater |
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| CN113318794B (en) * | 2021-05-12 | 2022-07-22 | 江苏大学 | Preparation method and application of plasmon composite photocatalyst Pd/DUT-67 |
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Application publication date: 20150617 |
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