CN105289737B - A kind of immobilized filter paper of Technique of Nano Pd and its preparation and application - Google Patents

A kind of immobilized filter paper of Technique of Nano Pd and its preparation and application Download PDF

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

The present invention relates to a kind of immobilized filter paper of Technique of Nano Pd and its preparation and application, filter paper is the PdCl by that will be adsorbed onto surface4 2‑In-situ reducing forms the immobilized filter paper of Technique of Nano Pd at palladium nano-particles.Filter paper is immersed in polyethylenimine solution, is washed, then be immersed in tetrachloro-palladium acid potassium solution, washes, obtains PEI/PdCl4 2‑Immobilized filter paper;By above-mentioned PEI/PdCl4 2‑Immobilized filter paper is immersed in sodium borohydride aqueous solution, impregnate after the completion of take out filter paper, washing, vacuum drying to get.Application of the immobilized filter paper of Technique of Nano Pd as catalyst.Preparation process of the present invention is simple, the preparation used time is few, is very suitable for industrialized production.The immobilized filter paper of Technique of Nano Pd prepared has the characteristics that high catalytic efficiency, reusing are good.Therefore it has broad application prospects in fields such as catalysis, environment remediations.

Description

A kind of immobilized filter paper of Technique of Nano Pd and its preparation and application
Technical field
The invention belongs to filter paper and its preparation and application field, more particularly to the immobilized filter paper of a kind of Technique of Nano Pd and its prepare and Using.
Background technology
Metal nano material occurs in recent years because becoming the hot spot of people research with many peculiar properties Many is reported about metal nano material in area researches such as sensor, drug, medical imaging, catalysis and environmental improvements, is being urged The achievement in research of its application of change field is especially prominent.Such as Claver et al. describe in detail palladium nano-particles to organic reaction The research (Claver et al.Chem.Soc.Rev.2011,40,4973-4985) of middle C-C cross-linking reactions catalysis, but do not have The fixed palladium nano-particles of carrier are to be not easily recycled and be difficult to reuse, and application potential can be also very restricted.It will Technique of Nano Pd is fixed or is assembled on nanofiber, and can effectively solving the above problems, (" a kind of Static Spinning containing nanoparticle palladium is multiple Close the preparation method of nanofiber mats ", Chinese invention patent, application number:201110259026.4;Huang et al.ACS Appl.Mater.Interfaces.2012,4(6),3054-3061).The experimental results showed that the composite wood that nanoparticle palladium is immobilized Material has excellent catalytic performance, while its repeat performance also greatly enhances, but the preparation of electro spinning nano fiber takes Length, cost are also higher, therefore this immobilized method actually practicability is not strong.
Filter paper is a kind of common filtering material, it has, and porosity is high, mechanical strength is good, cheap, chemical stabilization Property it is good the features such as, so using filter paper as the carrier of metal nanoparticle receive people widely concern and research.For example, Palladium nano-particles (Zheng et al.J.Phys.Chem.Lett.2015,6 (2), 230-238) are immobilized on filter by Zheng et al. Composite material is prepared on paper.Detailed process is to prepare stable palladium nano-particles with oleyl amine package palladium nano-particles first, Then it is immobilized on filter paper, then removes the oleyl amine on palladium nano-particles surface, it is immobilized to finally obtain Technique of Nano Pd Composite material.The experimental results showed that this material has excellent catalysis and repeat performance, the disadvantage is that the system of palladium nano-particles Standby process is complex, preparation condition is more harsh, and it is possible to cause to generate pollution to environment.Zboril et al. utilizes original The method of position reduction iron nano-particle is immobilized on filter paper (Zboril et al.Chem.Commun.2014,50 (99), It 15673-15676) is prepared into the magnetic coupling filter paper with high activity, the preparation method of the material is simple, highly practical.
Invention content
Technical problem to be solved by the invention is to provide a kind of immobilized filter paper of Technique of Nano Pd and its preparation and application, the present invention Method has that easy to operate, production cost is low, it is few, environmentally safe to prepare the used time, it is excellent to be very suitable for industrialized production etc. Point.
A kind of immobilized filter paper of Technique of Nano Pd of the present invention, the filter paper are the PdCl by that will be adsorbed onto surface4 2-It is in situ Palladium nano-particles are reduced into, the immobilized filter paper of Technique of Nano Pd is formed.Supported quantity of the palladium nano-particles on filter paper is 1.1-1.5%.
A kind of preparation method of the immobilized filter paper of Technique of Nano Pd of the present invention, including:
(1) filter paper is immersed in polyethylenimine solution, is washed, then be immersed in tetrachloro-palladium acid potassium solution, washed, obtain To PEI/PdCl4 2-Immobilized filter paper;Wherein the molar ratio of polyethyleneimine and tetrachloro-palladium potassium chlorate is 1:50;
(2) by above-mentioned PEI/PdCl4 2-Immobilized filter paper is immersed in sodium borohydride aqueous solution, impregnate after the completion of take out filter paper, Washing is dried in vacuo to get the immobilized filter paper of Technique of Nano Pd.
Polyethyleneimine is branched polymer, weight average molecular weight 25000 in the step (1).
Soaking time is 5min in the step (1).
A concentration of 15-20mg/mL of polyethylenimine solution in the step (1).
A concentration of 10-15mg/mL of tetrachloro-palladium acid potassium solution in the step (1).
A concentration of 5-10mg/mL of sodium borohydride aqueous solution in the step (2).
Soaking time is 6-10min in the step (2);Vacuum drying time is 24-36h.
A kind of application of the immobilized filter paper of Technique of Nano Pd of the present invention, application of the immobilized filter paper of Technique of Nano Pd as catalyst.
For the catalytic performance of the immobilized filter paper of Technique of Nano Pd prepared by research, the present invention has studied the immobilized filter paper pair of Technique of Nano Pd respectively The catalytic effect of 4- nitrophenols and potassium bichromate reduction reaction.Use SEM (scanning electron microscope), EDS (power dissipations Spectrum), TEM (transmission electron microscope), TGA (thermogravimetric analysis), UV-vis (uv-vis spectra) characterize the immobilized filter paper of Technique of Nano Pd And its catalytic performance.Test result is as follows for it:
(1) test result of SEM
The test result of SEM shows:The immobilized filter paper of palladium nano-particles of the present invention, the surface of fiber in its SEM image The substance for fine granularity occur, may infer that it is palladium nano-particles.It should be apparent that palladium nano-particles are being filtered from Fig. 1 (b) The surface of paper fiber is evenly distributed, referring to attached drawing 1.
(2) test result of EDS
The test result of EDS, which confirms, impregnated the filter paper of palladium nano-particles solution there are palladium element, referring to attached drawing 2.
(3) TEM test results
TEM test results show that palladium nano-particles are adsorbed on the outer surface of filter paper fibre, a diameter of 3.0 ± 0.9nm, ginseng See attached drawing 3.
(4) TGA test results
TGA test results are shown:The immobilized filter paper of Technique of Nano Pd starts to decompose at 300 DEG C or so under nitrogen protection.Material exists After undergoing 900 DEG C of high-temperature process, remaining substance is the residue and palladium nano-particles after the decomposition of filter paper.By the way that palladium is calculated Nano particle is 1.1-1.5% in the supported quantity of filter paper.Referring to attached drawing 4.
(5) Catalysis experiments test result
By the immobilized filter paper of Technique of Nano Pd to the Catalysis experiments of Cr (VI) reduction reaction, it has been found that be between when reacted When 28min, the conversion ratio of Cr (VI) has just reached 98%, this illustrates that the material has very strong urge to Cr (VI) reduction reaction Change ability, referring to attached drawing 5.The present invention carries out 3 repetition Catalysis experiments to prepared material.The experimental results showed that with catalysis The increase of number, prepared material can still keep very high catalytic efficiency to Cr (VI) reduction reaction, referring to attached drawing 6. By the immobilized filter paper of Technique of Nano Pd to the Catalysis experiments of 4- nitrophenol reduction reactions, it has been found that when being 10min between when reacted, The conversion ratio of 4- nitrophenols has just reached 95%, and it is good that this illustrates that the composite material prepared has 4- nitrophenols Catalytic capability, referring to attached drawing 7.With the increase of catalysis number, still there is very strong catalytic capability, referring to attached drawing 8.
The present invention relates to 2 basic principles:
(1) the high molecular molecular structure of polyethyleneimine and surface characteristic are made full use of, by electrostatic interaction by polyethylene Imines self-assembles on filter paper.The amino and PdCl of polyethyleneimine are utilized simultaneously4 2-Between complexing make both substances It is combined together, and then makes PdCl4 2-Tively firm it is fixed on filter paper.
(2) it is PdCl by being adsorbed onto surface palladium nano-particles to be immobilized on filter paper4 2-In-situ reducing is received at palladium What rice grain was completed.
Palladium nano-particles are steadily immobilized on filter paper by the present invention using the method for LBL self-assembly and in-situ reducing.This Kind preparation method has the advantages that following two is big:First, this method is easy to operate, the used time is few, highly practical;Second is that prepare The grain size of palladium nano-particles is small and is evenly distributed on the surface of filter paper fibre, palladium nano-particles is immobilized on filter paper, this will be big Big improves palladium nano-particles recycling performance.Polyethyleneimine auxiliary palladium nano-particles are immobilized to also having two sides on filter paper The advantages of face:On the one hand directly immobilized on filter paper compared to by positive charge palladium ion in-situ reducing, polyethyleneimine auxiliary Immobilized that palladium nano-particles is made to be immobilized on the ability on filter paper and greatly enhance, another aspect polyethyleneimine is to palladium nano-particles packet The effect wrapped up in is also beneficial to reduce the aggregation prevented between particle, improves the uniformity that palladium nano-particles are distributed on filter paper.
Advantageous effect
(1) preparation method of the present invention is simple, easily operated, production efficiency is high, highly practical, while using environmental-friendly High molecular material and cheap filter paper, are very suitable for industrialized production;
(2) the palladium nano-particles size of the invention prepared is small, large specific surface area, stablizes, therefore has fabulous catalysis Activity;
(3) present invention is effectively stable by palladium nano-particles by electrostatic interaction, is fixed on filter paper with being evenly distributed, this Not only the efficient catalytic performance of palladium nano-particles, but also the recycling and reuse convenient for palladium nano-particles ensure that.
Description of the drawings
Fig. 1 is the SEM figures of the immobilized filter paper (b) of Technique of Nano Pd prepared by the present invention and 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 the section TEM pictures and its Technique of Nano Pd particle diameter distribution histogram of the immobilized filter paper of Technique of Nano Pd prepared by the present invention; Including the high-resolution TEM pictures of Technique of Nano Pd on the TEM pictures (a) and filter paper of the fiber cross section of the immobilized filter paper of Technique of Nano Pd (b) and the grain size distribution (c) of Technique of Nano Pd;
Fig. 4 is the TGA figures of the immobilized filter paper of Technique of Nano Pd prepared by the present invention;
Fig. 5 is the UV-vis spectrograms of the catalysis reduction potassium bichromate of the immobilized filter paper of Technique of Nano Pd prepared by the present invention, a-h difference Represent the uv atlas of (0,4,8,12,16,20,24,28min) reaction solution in different time points;
Fig. 6 is the catalysis that three times repeats catalysis of the Technique of Nano Pd immobilized filter paper of the invention prepared to potassium bichromate reduction reaction Efficiency compares figure;
Fig. 7 is that the immobilized filter paper of Technique of Nano Pd prepared by the present invention is catalyzed the UV-vis spectrograms of 4- nitrophenol reduction reactions, a-m Respectively represent the uv atlas of (0,1,2,3,4,6,8,12,20,28,36min) reaction solution in different time points;
Fig. 8 is that the immobilized filter paper of Technique of Nano Pd prepared by the present invention is urged what four repetitions of 4- nitrophenol reduction reactions were catalyzed Change efficiency compares figure.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Embodiment 1
It takes 100mg polyethyleneimines to be dissolved in 5mL distilled water and is configured to 20mg/mL aq. polyethyleneimines.It takes 65mg tetrachloro-palladium potassium chlorates, which are dissolved in 5mL distilled water, is configured to 13mg/mL tetrachloro-palladium acid aqueous solutions of potassium.Take 40mg sodium borohydrides molten Solution is configured to 8mg/mL sodium borohydride aqueous solutions in 5mL distilled water, for use.Dry ordinary filter paper is immersed in above-mentioned made In standby aq. polyethyleneimine, the polyethyleneimine that surface is not adsorbed is washed away with distilled water after 5min, then It is immersed in again in tetrachloro-palladium acid potassium solution, is equally to be washed after impregnating 5min, the filter paper after washing is finally immersed in boron hydrogen again Change in sodium water solution, washed after 10min and is dried in vacuo for 24 hours to get to the immobilized filter paper of Technique of Nano Pd.It is received using SEM observations The pattern of the rice immobilized filter paper of palladium, can clearly be observed that distribution of the palladium nano-particles on filter paper fibre surface, referring to attached drawing 1.The test result of EDS confirms the immobilized filter paper of Technique of Nano Pd, and there are palladium elements, referring to attached drawing 2.It is immobilized using tem observation Technique of Nano Pd Filter paper can clearly be observed that palladium nano-particles in the distribution of fibre section and its size of particle, referring to attached drawing 3.TGA is surveyed Test result shows that the content of palladium nano-particles in the material is 1.1-1.5%, referring to attached drawing 4.
Embodiment 2
Magnetic agitation after 88.26mg potassium bichromates and 100mL water is added into a beaker, it is molten to be configured to 3mM potassium bichromates Liquid, for use.It is stirred evenly after taking 10mL 3mM potassium bichromate solutions, 1.5mL formic acid solutions and the mixing of 15mL deionized waters, it will The immobilized palladium nano-particles filter paper of 20mg is immersed in the mixed solution.In the case of magnetic agitation, the material prepared is utilized Catalysis experiments are carried out to potassium bichromate reduction reaction.Respectively in 0min, 4min, 8min, 12min, 16min, 20min, 24min and The each catalysis time points of 28min respectively take 0.5mL reaction solutions to be diluted to 1mL to measure the concentration of Cr (VI) in the solution.UV- Vis test results show:With the increase in reaction time, the absorption peak (350nm) of Cr (VI) reduces rapidly.It is in the reaction time 28min, corresponding catalytic efficiency can reach 98% (such as Fig. 5).3 weights are carried out with the immobilized palladium nano-particles filter paper of same Multiple Catalysis experiments.Comparative experiments can still keep very high catalytic efficiency (such as Fig. 6) as a result, it has been found that repeatedly after catalysis.
Embodiment 3
It first takes 13.91mg 4- nitrophenols that magnetic agitation in 10mL aqueous solutions is added, is configured to the light yellow 4- nitre of 10mM Base phenol solution, then 378.3mg sodium borohydrides is taken to be dissolved in 1mL ice water solutions, for use.Take 0.6mL 10mM 4- nitrophenols Solution, 0.6mL 10M NaBH4It is stirred evenly after solution and the mixing of 16.8mL deionized waters, the immobilized filter paper of 20mg Technique of Nano Pd is soaked Bubble is in the mixed solution.In the case of magnetic agitation, Catalysis experiments are carried out to 4- nitrophenols using the material of preparation.Point Not in each catalysis time of 0min, 1min, 2min, 3min, 4min, 6min, 8min, 12min, 20min, 28min and 36min Point respectively takes 0.5mL reaction solutions to be diluted to 1.5mL to measure the concentration of 4- nitrophenols in the solution.UV-vis test results Show:With the increase in reaction time, the absorption peak (400nm) of 4- nitrophenols reduces rapidly, while the spy of 4-aminophenol Sign peak (300nm) constantly increases.It is 10min in the reaction time, corresponding catalytic efficiency can reach 95% (such as Fig. 7). Four repetition Catalysis experiments are carried out with the immobilized filter paper of same Technique of Nano Pd.Comparative experiments still may be used as a result, it has been found that repeatedly after catalysis To keep very high catalytic efficiency (such as Fig. 8).

Claims (4)

1. a kind of preparation method of the immobilized filter paper of Technique of Nano Pd, including:
(1) filter paper is immersed in polyethylenimine solution, is washed, then be immersed in tetrachloro-palladium acid potassium solution, washed, obtain PEI/PdCl4 2-Immobilized filter paper;Wherein, the molar ratio of polyethyleneimine and tetrachloro-palladium potassium chlorate is 1:50;Soaking time is 5min;A concentration of 15-20mg/mL of polyethylenimine solution;A concentration of 10-15mg/mL of tetrachloro-palladium acid potassium solution;
(2) by above-mentioned PEI/PdCl4 2-Immobilized filter paper is immersed in sodium borohydride aqueous solution, and filter paper, water are taken out after the completion of impregnating It washes, be dried in vacuo to get the immobilized filter paper of Technique of Nano Pd;Wherein, a concentration of 5-10mg/mL of sodium borohydride aqueous solution.
2. a kind of preparation method of the immobilized filter paper of Technique of Nano Pd according to claim 1, it is characterised in that:Gather in step (1) Aziridine is branched polymer, weight average molecular weight 25000.
3. a kind of preparation method of the immobilized filter paper of Technique of Nano Pd according to claim 1, it is characterised in that:The step (2) Middle soaking time is 6-10min;Vacuum drying time is 24-36h.
4. a kind of preparation method of the immobilized filter paper of Technique of Nano Pd according to claim 1, it is characterised in that:The Technique of Nano Pd is solid Carry application of the filter paper as catalyst.
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CN102409531A (en) * 2011-09-02 2012-04-11 东华大学 Method for preparing electrospun composite nanoscale fiber felt containing nanoscale palladium particles
CN102512991A (en) * 2011-12-23 2012-06-27 天津工业大学 Polymer catalytic membrane containing palladium metal activity functional layer and preparation method thereof
CN105056993A (en) * 2015-08-13 2015-11-18 东华大学 Au PENPs (PEGylated PEI-entrapped AuNPs) immobilizing filter paper as well as preparation and application thereof

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