CN105289737A - Filter paper with fixedly-carried nano palladium, preparation and applications thereof - Google Patents

Filter paper with fixedly-carried nano palladium, preparation and applications thereof Download PDF

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CN105289737A
CN105289737A CN201510807618.3A CN201510807618A CN105289737A CN 105289737 A CN105289737 A CN 105289737A CN 201510807618 A CN201510807618 A CN 201510807618A CN 105289737 A CN105289737 A CN 105289737A
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filter paper
nano
technique
immobilized
palladium
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CN105289737B (en
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史向阳
刘雷
赵毅丽
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Donghua University
National Dong Hwa University
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Donghua University
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Abstract

The invention relates to a filter paper with fixedly-carried nano palladium, preparation and applications thereof. The nano palladium fixedly-carrying filter paper is prepared by in-situ reducing the PdCl4<2>, which is absorbed on the surface of the filter paper, into palladium nano particles. The nano palladium fixedly-carrying filter paper can be soaked in a potassium tetrachloro-palladate solution, and then the filter paper is washed by water to obtain a PEI/PdCl4<2> fixedly-carrying filter paper. The PEI/PdCl4<2> fixedly-carrying filter paper is soaked in a sodium borohydride water solution, and then the filter paper is taken out after soaking, is washed by water, and is finally dried in vacuum to obtain the target product. The nano palladium fixedly-carrying filter paper can be used as a catalyst. The preparation technology is simple, the preparation time is short, and thus the preparation method is very suitable for industrial production. The prepared nano palladium fixedly-carrying filter paper has the characteristics of high catalytic efficiency and good reusability, and thus has a wide application prospect in the fields of catalysis, environmental remediation, and the like.

Description

A kind of immobilized filter paper of Technique of Nano Pd and Synthesis and applications thereof
Technical field
The invention belongs to filter paper and Synthesis and applications field thereof, particularly the immobilized filter paper of a kind of Technique of Nano Pd and Synthesis and applications thereof.
Background technology
Metal nano material is because have the focus that many peculiar properties become people's research, occur in recent years many about metal nano material at area research reports such as sensor, medicine, medical imaging, catalysis and environmental improvements, particularly outstanding in achievement in research of its application of catalytic field.The people such as such as Claver describe the (Claveretal.Chem.Soc.Rev.2011 of the research to C-C cross-linking reaction catalysis in organic reaction of palladium nano-particles in detail, 40,4973-4985), do not have the fixing palladium nano-particles of carrier to be not easily reclaim and be difficult to recycling, its application potential also can be very restricted.Fixed by Technique of Nano Pd or be assembled on nanofiber, can effectively solve the problem (" a kind of preparation method of the Static Spinning composite nanometer fiber felt containing nanoparticle palladium ", Chinese invention patent, application number: 201110259026.4; Huangetal.ACSAppl.Mater.Interfaces.2012,4 (6), 3054-3061).Experimental result shows that the immobilized composite of nanoparticle palladium has excellent catalytic performance, its repeat performance also strengthens greatly simultaneously, but the preparation of electro spinning nano fiber length consuming time, cost are also higher, therefore in fact practicality is not strong for this immobilized method.
Filter paper is a kind of common filtering material, the features such as porosity is high, mechanical strength good, low price, chemical stability are good that it has, and pays close attention to widely so filter paper is received people as the carrier of metal nanoparticle and studies.Such as, the people such as Zheng are prepared into composite by immobilized for palladium nano-particles (Zhengetal.J.Phys.Chem.Lett.2015,6 (2), 230-238) on filter paper.Detailed process first prepares stable palladium nano-particles with oleyl amine parcel palladium nano-particles, then that it is immobilized on filter paper, then removes the oleyl amine on palladium nano-particles surface, thus the composite that final acquisition Technique of Nano Pd is immobilized.Experimental result shows that this material has excellent catalysis and repeat performance, and shortcoming is that the preparation process of palladium nano-particles is comparatively complicated, preparation condition is comparatively harsh, and likely causes producing environment polluting.The people such as Zboril utilize the method for in-situ reducing by immobilized for iron nano-particle on filter paper (Zboriletal.Chem.Commun.2014,50 (99), 15673-15676) be prepared into and have highly active magnetic coupling filter paper, the preparation method of this material is simple, practical.
Summary of the invention
Technical problem to be solved by this invention is to provide the immobilized filter paper of a kind of Technique of Nano Pd and Synthesis and applications thereof, the inventive method have simple to operate, production cost is low, preparation used time few, environmentally safe, be very suitable for the advantages such as suitability for industrialized production.
The immobilized filter paper of a kind of Technique of Nano Pd of the present invention, described filter paper is by being adsorbed onto the PdCl of its surface 4 2-in-situ reducing becomes palladium nano-particles, forms the immobilized filter paper of Technique of Nano Pd.The supported quantity of palladium nano-particles on filter paper is 1.1-1.5%.
The preparation method of the immobilized filter paper of a kind of Technique of Nano Pd of the present invention, comprising:
(1) be immersed in polyethylenimine solution by filter paper, washing, then be immersed in tetrachloro-palladium acid potassium solution, washing, obtains PEI/PdCl 4 2-immobilized filter paper; Wherein the mol ratio of polymine and tetrachloro-palladium potassium chlorate is 1:50;
(2) by above-mentioned PEI/PdCl 4 2-immobilized filter paper is immersed in sodium borohydride aqueous solution, has soaked rear taking-up filter paper, washing, vacuum drying, obtains the immobilized filter paper of Technique of Nano Pd.
In described step (1), polymine is branched polymer, and weight average molecular weight is 25000.
In described step (1), soak time is 5min.
In described step (1), the concentration of polyethylenimine solution is 15-20mg/mL.
In described step (1), the concentration of tetrachloro-palladium acid potassium solution is 10-15mg/mL.
In described step (2), sodium borohydride aqueous solution concentration is 5-10mg/mL.
In described step (2), soak time is 6-10min; The vacuum drying time is 24-36h.
The application of the immobilized filter paper of a kind of Technique of Nano Pd of the present invention, the immobilized filter paper of described Technique of Nano Pd is as the application of catalyst.
For the catalytic performance of the immobilized filter paper of Technique of Nano Pd of research preparation, the present invention have studied the catalytic effect of the immobilized filter paper of Technique of Nano Pd to 4-nitrophenol and potassium bichromate reduction reaction respectively.SEM (SEM), EDS (power dissipation spectrum), TEM (transmission electron microscope), TGA (thermogravimetric analysis), UV-vis (uv-vis spectra) is used to characterize the immobilized filter paper of Technique of Nano Pd and catalytic performance thereof.Its test result is as follows:
(1) test result of SEM
The test result of SEM shows: the immobilized filter paper of palladium nano-particles of the present invention, and in its SEM image, the material of fine granularity appears in the surface of fiber, can infer it is palladium nano-particles.Clearly can find out that palladium nano-particles is even in the surface distributed of filter paper fibre, see accompanying drawing 1 from Fig. 1 (b).
(2) test result of EDS
The test result of EDS confirms that the filter paper soaking palladium nano-particles solution exists palladium element, see accompanying drawing 2.
(3) TEM test result
TEM test result shows that palladium nano-particles is adsorbed on the outer surface of filter paper fibre, and its diameter is 3.0 ± 0.9nm, see accompanying drawing 3.
(4) TGA test result
TGA test result shows: the immobilized filter paper of Technique of Nano Pd starts to decompose at about 300 DEG C under nitrogen protection.Material is after experience 900 DEG C of high-temperature process, and remaining material is residue after the decomposition of filter paper and palladium nano-particles.Be 1.1-1.5% by calculating palladium nano-particles at the supported quantity of filter paper.See accompanying drawing 4.
(5) Catalysis experiments test result
By the Catalysis experiments of the immobilized filter paper of Technique of Nano Pd to Cr (VI) reduction reaction, when we are 28min between finding when reacted, the conversion ratio of Cr (VI) just reaches 98%, which illustrate this material and have very strong catalytic capability, see accompanying drawing 5 to Cr (VI) reduction reaction.The present invention carries out 3 times to prepared material and repeats Catalysis experiments.Experimental result shows the increase along with catalysis number of times, and prepared material still can keep very high catalytic efficiency, see accompanying drawing 6 to Cr (VI) reduction reaction.By the immobilized filter paper of Technique of Nano Pd to the Catalysis experiments of 4-nitrophenol reduction reaction, when we are 10min between finding when reacted, the conversion ratio of 4-nitrophenol just reaches 95%, which illustrates the composite prepared and has good catalytic capability to 4-nitrophenol, see accompanying drawing 7.Along with the increase of catalysis number of times, it still has very strong catalytic capability, see accompanying drawing 8.
The present invention relates to 2 general principles:
(1) make full use of the high molecular molecular structure of polymine and surface characteristic, by electrostatic interaction, polymine is self-assembled on filter paper.Utilize amino and the PdCl of polymine simultaneously 4 2-between complexing these two kinds of materials are combined, and then make PdCl 4 2-comparatively be securely fixed on filter paper.
(2) by immobilized for palladium nano-particles be PdCl by being adsorbed onto its surface on filter paper 4 2-in-situ reducing becomes palladium nano-particles to complete.
The present invention adopts the method for LBL self-assembly and in-situ reducing that palladium nano-particles is stably immobilized on filter paper.This preparation method has following two large advantages: one be that this method is simple to operate, the used time is few, practical; Two is that the particle diameter of the palladium nano-particles prepared is little and even in the surface distributed of filter paper fibre, and by immobilized for palladium nano-particles on filter paper, this will improve palladium nano-particles recycling performance greatly.Polymine assists that palladium nano-particles is immobilized also has the advantage of two aspects to filter paper: on the one hand compared to directly immobilized on filter paper by positive charge palladium ion in-situ reducing, polymine assists the immobilized immobilized ability on filter paper of palladium nano-particles that makes greatly to strengthen, polymine is also conducive to palladium nano-particles package action reducing the gathering prevented between particle on the other hand, improves the uniformity that palladium nano-particles distributes on filter paper.
beneficial effect
(1) preparation method of the present invention simple, be easy to operation, production efficiency is high, practical, adopts eco-friendly macromolecular material and cheap filter paper simultaneously, is very applicable to suitability for industrialized production;
(2) the palladium nano-particles size prepared of the present invention is little, specific area large, stablize, and therefore has fabulous catalytic activity;
(3) palladium nano-particles is stablized by electrostatic interaction, is fixed on filter paper with being evenly distributed by the present invention effectively, and this both ensure that the efficient catalytic performance of palladium nano-particles, was convenient to again the recovery and reuse of palladium nano-particles.
Accompanying drawing explanation
Fig. 1 is that the immobilized filter paper (b) of Technique of Nano Pd prepared by the present invention is schemed with the SEM of ordinary filter paper (a);
Fig. 2 is the EDS collection of illustrative plates of the immobilized filter paper of Technique of Nano Pd prepared by the present invention;
Fig. 3 is cross section TEM picture and the Technique of Nano Pd domain size distribution histogram thereof of the immobilized filter paper of Technique of Nano Pd prepared by the present invention; Comprising TEM picture (a) and high-resolution TEM picture (b) of Technique of Nano Pd and the grain size distribution (c) of Technique of Nano Pd on filter paper of the fiber cross section of the immobilized filter paper of Technique of Nano Pd;
Fig. 4 is the TGA figure of the immobilized filter paper of Technique of Nano Pd prepared by the present invention;
Fig. 5 is the UV-vis spectrogram of the catalytic reduction potassium bichromate of the immobilized filter paper of Technique of Nano Pd prepared by the present invention, and a-h represents the uv atlas at different time points (0,4,8,12,16,20,24,28min) reactant liquor respectively;
Fig. 6 is that the immobilized filter paper of Technique of Nano Pd prepared by the present invention repeats the catalytic efficiency contrast figure of catalysis to three of potassium bichromate reduction reaction times;
Fig. 7 is the UV-vis spectrogram of Technique of Nano Pd immobilized filter paper catalysis 4-nitrophenol reduction reaction prepared by the present invention, and a-m represents the uv atlas at different time points (0,1,2,3,4,6,8,12,20,28,36min) reactant liquor respectively;
Fig. 8 is that the immobilized filter paper of Technique of Nano Pd prepared by the present invention repeats the catalytic efficiency contrast figure of catalysis to four times of 4-nitrophenol reduction reaction.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Get 100mg polymine to be dissolved in 5mL distilled water and to be mixed with 20mg/mL aq. polyethyleneimine.Get 65mg tetrachloro-palladium potassium chlorate to be dissolved in 5mL distilled water and to be mixed with 13mg/mL tetrachloro-palladium acid aqueous solutions of potassium.Get 40mg sodium borohydride to be dissolved in 5mL distilled water and to be mixed with 8mg/mL sodium borohydride aqueous solution, stand-by.The ordinary filter paper of drying is immersed in above-mentioned prepared aq. polyethyleneimine, its surface is washed away not by the polymine adsorbed with distilled water after 5min, and then be immersed in tetrachloro-palladium acid potassium solution, soak 5min after washing equally, finally the filter paper after washing is immersed in sodium borohydride aqueous solution again, 10min after washing also by its vacuum drying 24h, namely obtains the immobilized filter paper of Technique of Nano Pd.Utilize SEM to observe the pattern of the immobilized filter paper of Technique of Nano Pd, clearly can observe the distribution of palladium nano-particles on filter paper fibre surface, see accompanying drawing 1.The test result of EDS confirms that the immobilized filter paper of Technique of Nano Pd exists palladium element, see accompanying drawing 2.Utilize the immobilized filter paper of tem observation Technique of Nano Pd, clearly can observe the distribution of palladium nano-particles in fibre section and the size of particle thereof, see accompanying drawing 3.TGA test result display palladium nano-particles content is in the material 1.1-1.5%, see accompanying drawing 4.
Embodiment 2
In a beaker, add magnetic agitation after 88.26mg potassium bichromate and 100mL water, be mixed with 3mM potassium bichromate solution, stand-by.Stir after getting the mixing of 10mL3mM potassium bichromate solution, 1.5mL formic acid solution and 15mL deionized water, immobilized for 20mg palladium nano-particles filter paper is immersed in this mixed solution.When magnetic agitation, the material prepared is utilized to carry out Catalysis experiments to potassium bichromate reduction reaction.Respectively at each catalysis time point of 0min, 4min, 8min, 12min, 16min, 20min, 24min and 28min, respectively get 0.5mL reaction solution and be diluted to 1mL to measure Cr (VI) concentration in the solution.UV-vis test result shows: along with the increase in reaction time, and the absworption peak (350nm) of Cr (VI) reduces rapidly.Be 28min in the reaction time, corresponding catalytic efficiency just can reach 98% (as Fig. 5).Carry out 3 times with the immobilized palladium nano-particles filter paper of same and repeat Catalysis experiments.After comparative experiments found that repeatedly catalysis, it still can keep very high catalytic efficiency (as Fig. 6).
Embodiment 3
First get 13.91mg4-nitrophenol and add magnetic agitation in the 10mL aqueous solution, be mixed with the light yellow 4-nitrophenol solution of 10mM, then get 378.3mg sodium borohydride and be dissolved in 1mL ice water solution, stand-by.Get 0.6mL10mM4-nitrophenol solution, 0.6mL10MNaBH 4stir after solution and the mixing of 16.8mL deionized water, immobilized for 20mg Technique of Nano Pd filter paper is immersed in this mixed solution.When magnetic agitation, the material of preparation is utilized to carry out Catalysis experiments to 4-nitrophenol.Respectively at each catalysis time point of 0min, 1min, 2min, 3min, 4min, 6min, 8min, 12min, 20min, 28min and 36min, respectively get 0.5mL reaction solution and be diluted to 1.5mL to measure 4-nitrophenol concentration in the solution.UV-vis test result shows: along with the increase in reaction time, and the absworption peak (400nm) of 4-nitrophenol reduces rapidly, simultaneously constantly the increasing of characteristic peak (300nm) of PAP.Be 10min in the reaction time, corresponding catalytic efficiency just can reach 95% (as Fig. 7).Carry out four times with the immobilized filter paper of same Technique of Nano Pd and repeat Catalysis experiments.After comparative experiments found that repeatedly catalysis, it still can keep very high catalytic efficiency (as Fig. 8).

Claims (10)

1. the immobilized filter paper of Technique of Nano Pd, is characterized in that: described filter paper is by being adsorbed onto the PdCl of its surface 4 2-in-situ reducing becomes palladium nano-particles, forms the immobilized filter paper of Technique of Nano Pd.
2. the immobilized filter paper of a kind of Technique of Nano Pd according to claim 1, is characterized in that: the supported quantity of palladium nano-particles on filter paper is 1.1-1.5%.
3. a preparation method for the immobilized filter paper of Technique of Nano Pd, comprising:
(1) be immersed in polyethylenimine solution by filter paper, washing, then be immersed in tetrachloro-palladium acid potassium solution, washing, obtains PEI/PdCl 4 2-immobilized filter paper; Wherein the mol ratio of polymine and tetrachloro-palladium potassium chlorate is 1:50;
(2) by above-mentioned PEI/PdCl 4 2-immobilized filter paper is immersed in sodium borohydride aqueous solution, has soaked rear taking-up filter paper, washing, vacuum drying, obtains the immobilized filter paper of Technique of Nano Pd.
4. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in step (1), polymine is branched polymer, and weight average molecular weight is 25000.
5. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in described step (1), soak time is 5min.
6. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in described step (1), the concentration of polyethylenimine solution is 15-20mg/mL.
7. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in described step (1), the concentration of tetrachloro-palladium acid potassium solution is 10-15mg/mL.
8. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in described step (2), sodium borohydride aqueous solution concentration is 5-10mg/mL.
9. the preparation method of the immobilized filter paper of a kind of Technique of Nano Pd according to claim 3, is characterized in that: in described step (2), soak time is 6-10min; The vacuum drying time is 24-36h.
10. an application for the immobilized filter paper of Technique of Nano Pd as claimed in claim 1, is characterized in that: the immobilized filter paper of described Technique of Nano Pd is as the application of catalyst.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107497483A (en) * 2017-07-11 2017-12-22 南阳师范学院 A kind of paper substrate palladium composite catalyst and its preparation and application

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