CN103831117A - Preparation method for synthesizing platinum nanoparticles supported magnetic hollow capsule type catalyst by taking polystyrene as soft template - Google Patents
Preparation method for synthesizing platinum nanoparticles supported magnetic hollow capsule type catalyst by taking polystyrene as soft template Download PDFInfo
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Abstract
The invention discloses a preparation method for synthesizing a platinum nanoparticles supported magnetic hollow capsule type catalyst by taking polystyrene as a soft template, relates to a preparation method of the magnetic catalyst and aims at solving the problems of low catalytic activity, poor stability and incapability of separating nanometer materials out of a reaction system after the synthesis is ended in the prior art. The method comprises the following steps: mixing polystyrene spheres with a platinum source, then adding polymer monomers, ferric oxide nanoparticles and ferric chloride hexahydrate, adding a potassium hydroxide solution under the protection of a nitrogen atmosphere, centrifugally washing and dipping a methylbenzene solution finally to obtain the platinum nanoparticles supported magnetic hollow capsule type catalyst. The platinum nanoparticles supported magnetic hollow capsule type catalyst is applicable to a preparation method for synthesizing the platinum nanoparticles supported magnetic hollow capsule type catalyst by taking polystyrene as the soft template.
Description
Technical field
The present invention relates to the preparation method of magnetic catalyst.
Background technology
Nano particle is because its unique physical chemistry and biological nature have attracted the notice of more and more scientific researchers.These characteristics make it be applied in widely energy conversion, sensor, biological medicine, especially catalyst aspect.Research shows, because nano particle has very high specific area, makes it have very high catalytic activity.But nano material also exists weak point in the process of practical application.On the one hand, can there is serious gathering in nano particle in solution, thereby caused the obvious reduction of its catalytic activity; On the other hand, catalysis finishes rear nano material and is difficult to separate from reaction system, not only affected the recycling of material, and residual nano material also can cause secondary pollution, these 2 serious obstructions nano particle in real-life extensive use.
Summary of the invention
The present invention will solve prior art and exist catalytic activity low, poor stability, catalysis finishes rear nano material and be difficult to the problem of separating from reaction system, and a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template is provided.
A preparation method for the magnetic hollow capsule type catalyst of synthetic supported platinum nano particle take polystyrene as soft template, specifically carries out according to following steps:
One, polystyrene sphere is joined in the aqueous solution in platinum source, stir, form dispersion liquid;
The concentration of aqueous solution in described platinum source is 0.001mol/L～10mol/L; The volume ratio of the aqueous solution in the quality of described polystyrene sphere and platinum source is 1mg:(0.1～0.5) mL;
Two, under the condition stirring, polymer monomer, ferric oxide nano particles and Iron trichloride hexahydrate are joined in the dispersion liquid that step 1 obtains successively, obtain reaction system, under nitrogen atmosphere protection, be the potassium hydroxide solution of 1mol/L～10mol/L to adding concentration in reaction system, reaction 1h～10h, obtains product;
Described polymer monomer and the mass ratio of ferric oxide nano particles are 1:(0.1～0.5); Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(0.1～0.5); The quality of described polymer monomer and concentration are that the volume ratio of the potassium hydroxide solution of 1mol/L～10mol/L is 1g:(1～100) mL; The volume ratio of the dispersion liquid that the quality of described polymer monomer and step 1 obtain is 1g:(100～10000) mL;
Three, be under 100r/min～9000r/min at rotating speed, product centrifugal treating 1min～30min that step 2 is obtained, then with deionized water washing 1 time～10 times, the product after being washed;
Four, the product after washing step 3 being obtained soaks 1h～15h in toluene solution, obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.
The invention has the beneficial effects as follows: the catalyst that 1, prepared by the present invention has the stability higher than general catalyst, avoided material because assembling the low problem of catalytic activity causing, in service life that can extending catalyst, reduce financial cost.
2, the prepared catalyst of the present invention has magnetic, can be separated by externally-applied magnetic fields such as magnet, easily realizes recycling, has solved the problem of secondary pollution.
3, the prepared catalyst of the present invention has very strong degradation to dyestuff in sewage.
The present invention is for a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template.
Accompanying drawing explanation
Fig. 1 is the SEM photo of polystyrene;
Fig. 2 is the product S EM photo after the washing that obtains of embodiment step 3;
Fig. 3 is the SEM photo of the magnetic hollow capsule type catalyst of the supported platinum nano particle prepared of embodiment step 4;
Fig. 4 is the TEM photo of the magnetic hollow capsule type catalyst of the supported platinum nano particle prepared of embodiment step 4;
Fig. 5 is the catalytic performance figure of the magnetic hollow capsule type catalyst of the supported platinum nano particle prepared of embodiment step 4; A is the curve that tetranitro phenol adds the ultraviolet-visible absorption spectroscopy test gained after NaOH and sodium borohydride; B is that tetranitro phenol adds after NaOH and sodium borohydride, then adds the curve of the ultraviolet-visible absorption spectroscopy test gained after hollow capsules type catalyst;
Fig. 6 is the photo that magnetic hollow capsule type catalyst one side of the supported platinum nano particle prepared of embodiment step 4 is not placed magnet;
Fig. 7 is that the magnetic hollow capsule type catalyst one of the supported platinum nano particle prepared of embodiment step 4 is sidelong the photo of putting magnet.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template described in present embodiment, specifically carries out according to following steps:
One, polystyrene sphere is joined in the aqueous solution in platinum source, stir, form dispersion liquid;
The concentration of aqueous solution in described platinum source is 0.001mol/L～10mol/L; The volume ratio of the aqueous solution in the quality of described polystyrene sphere and platinum source is 1mg:(0.1～0.5) mL;
Two, under the condition stirring, polymer monomer, ferric oxide nano particles and Iron trichloride hexahydrate are joined in the dispersion liquid that step 1 obtains successively, obtain reaction system, under nitrogen atmosphere protection, be the potassium hydroxide solution of 1mol/L～10mol/L to adding concentration in reaction system, reaction 1h～10h, obtains product;
Described polymer monomer and the mass ratio of ferric oxide nano particles are 1:(0.1～0.5); Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(0.1～0.5); The quality of described polymer monomer and concentration are that the volume ratio of the potassium hydroxide solution of 1mol/L～10mol/L is 1g:(1～100) mL; The volume ratio of the dispersion liquid that the quality of described polymer monomer and step 1 obtain is 1g:(100～10000) mL;
Three, be under 100r/min～9000r/min at rotating speed, product centrifugal treating 1min～30min that step 2 is obtained, then with deionized water washing 1 time～10 times, the product after being washed;
Four, the product after washing step 3 being obtained soaks 1h～15h in toluene solution, obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.
The beneficial effect of present embodiment is: the catalyst that 1, prepared by present embodiment has the stability higher than general catalyst, has avoided material because assembling the low problem of catalytic activity causing, and in service life that can extending catalyst, reduces financial cost.
2, the prepared catalyst of present embodiment has magnetic, can be separated by externally-applied magnetic fields such as magnet, easily realizes recycling, has solved the problem of secondary pollution.
3, the prepared catalyst of present embodiment has very strong degradation to dyestuff in sewage.
The specific embodiment two: present embodiment is different from the specific embodiment one: the diameter of the polystyrene sphere described in step 1 is 100nm～1000nm.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from one of specific embodiment one or two: a kind of in the aqueous solution that the aqueous solution in the platinum source described in step 1 is platinum chloride, the aqueous solution of platinic sulfate, the aqueous solution of cyaniding platinum or the aqueous solution of platinum oxide or wherein several mixture.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three: the volume ratio of the aqueous solution in the quality of the polystyrene sphere described in step 1 and platinum source is 1mg:(0.1～0.4) mL.Other is identical with the specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four: the polymer monomer described in step 2 is thiophene monomer, pyrrole monomer or aniline monomer.Other is identical with the specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five: in step 2, under nitrogen atmosphere protection, be the potassium hydroxide solution of 2mol/L to adding concentration in reaction system, reaction 4h～8h.Other is identical with the specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six: be under 7000r/min at rotating speed in step 3, the product centrifugal treating 15min that step 2 is obtained, again with deionized water washing 3 times, the product after being washed.Other is identical with the specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven: the product after the washing in step 4, step 3 being obtained soaks 9h～12h in toluene solution, obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.Other is identical with the specific embodiment one to seven.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment:
A kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template described in the present embodiment, specifically carries out according to following steps:
One, be that 100nm polystyrene sphere joins in the aqueous solution in 150mL platinum source by 500mg diameter, stir, form dispersion liquid;
The concentration of aqueous solution in described platinum source is 0.05mol/L; The aqueous solution that the aqueous solution in described platinum source is platinum chloride;
Two, under the condition stirring, 0.2g thiophene monomer, 0.07g ferric oxide nano particles and 0.05g Iron trichloride hexahydrate are joined in the dispersion liquid that step 1 obtains successively, obtain reaction system, under nitrogen atmosphere protection, be the potassium hydroxide solution of 2mol/L to adding 10mL concentration in reaction system, reaction 5h, obtains product;
Three, be under 7000r/min at rotating speed, the product centrifugal treating 10min that step 2 is obtained, then with deionized water washing 3 times, the product after being washed;
Four, the product after washing step 3 being obtained is 10h in 30mL toluene solution soaks, and obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.
As shown in Figure 1, as shown in Figure 2, as seen from the figure, its diameter increases the product S EM photo after the washing that embodiment step 3 obtains the SEM photo of polystyrene to some extent, and outward appearance is mellow and full, and synthetic composite is apparent fine.
The SEM photo of the magnetic hollow capsule type catalyst of supported platinum nano particle prepared by embodiment step 4 as shown in Figure 3, as seen from the figure, in figure, there is complete composite bead, also the composite bead that has part breakage, this shows that composite has formed hollow capsules type structure after polystyrene etching simultaneously.
As shown in Figure 4, as seen from the figure, spheroid is hollow structure to the TEM photo of the magnetic hollow capsule type catalyst of supported platinum nano particle prepared by embodiment step 4, and some nano particles in housing grappling simultaneously.
The catalytic performance figure of the magnetic hollow capsule type catalyst of supported platinum nano particle prepared by embodiment step 4 as shown in Figure 5, in figure, a is that 0.01g tetranitro phenol is dissolved in 30ml water, add 0.1gNaOH and 2g sodium borohydride, after ultrasonic concussion 20min, carry out the curve of ultraviolet-visible absorption spectra test gained; B is that 0.01g tetranitro phenol is dissolved in 30ml water, adds 0.1gNaOH and 2g sodium borohydride, then adds the curve that carries out ultraviolet-visible absorption spectra test gained after the ultrasonic concussion of the synthetic hollow capsules type catalyst of 0.015g 20min; Two curves of a and b contrast known, and hollow capsules type catalyst is had catalytic activity to tetranitro phenol by the reaction of sodium borohydride reduction.
The photo that magnetic hollow capsule type catalyst one side of supported platinum nano particle prepared by embodiment step 4 is not placed magnet as shown in Figure 6; The magnetic hollow capsule type catalyst one of supported platinum nano particle prepared by embodiment step 4 be sidelong put magnet photo as shown in Figure 7; As seen from the figure, the synthetic material situation in 10ml centrifuge tube in embodiment when Fig. 6 normally leaves standstill, material is in the bottom of centrifuge tube, Fig. 7 places after a magnet on centrifuge tube right side, material in embodiment is drawn onto on vertical tube wall by magnet, hence one can see that, and the magnetic hollow capsule type catalyst of supported platinum nano particle prepared by the present embodiment is magnetic.
Claims (8)
1. a preparation method for the magnetic hollow capsule type catalyst of synthetic supported platinum nano particle take polystyrene as soft template, is characterized in that a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template carries out according to following steps:
One, polystyrene sphere is joined in the aqueous solution in platinum source, stir, form dispersion liquid;
The concentration of aqueous solution in described platinum source is 0.001mol/L～10mol/L; The volume ratio of the aqueous solution in the quality of described polystyrene sphere and platinum source is 1mg:(0.1～0.5) mL;
Two, under the condition stirring, polymer monomer, ferric oxide nano particles and Iron trichloride hexahydrate are joined in the dispersion liquid that step 1 obtains successively, obtain reaction system, under nitrogen atmosphere protection, be the potassium hydroxide solution of 1mol/L～10mol/L to adding concentration in reaction system, reaction 1h～10h, obtains product;
Described polymer monomer and the mass ratio of ferric oxide nano particles are 1:(0.1～0.5); Described polymer monomer and the mass ratio of Iron trichloride hexahydrate are 1:(0.1～0.5); The quality of described polymer monomer and concentration are that the volume ratio of the potassium hydroxide solution of 1mol/L～10mol/L is 1g:(1～100) mL; The volume ratio of the dispersion liquid that the quality of described polymer monomer and step 1 obtain is 1g:(100～10000) mL;
Three, be under 100r/min～9000r/min at rotating speed, product centrifugal treating 1min～30min that step 2 is obtained, then with deionized water washing 1 time～10 times, the product after being washed;
Four, the product after washing step 3 being obtained soaks 1h～15h in toluene solution, obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.
2. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1, the diameter that it is characterized in that the polystyrene sphere described in step 1 is 100nm～1000nm.
According to claim 1 a kind of take polystyrene as soft template the preparation method of the magnetic hollow capsule type catalyst of synthetic supported platinum nano particle, a kind of in the aqueous solution that the aqueous solution that it is characterized in that the platinum source described in step 1 is platinum chloride, the aqueous solution of platinic sulfate, the aqueous solution of cyaniding platinum or the aqueous solution of platinum oxide or wherein several mixture.
4. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1, is characterized in that the volume ratio of the quality of the polystyrene sphere described in step 1 and the aqueous solution in platinum source is 1mg:(0.1～0.4) mL.
5. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1, is characterized in that the polymer monomer described in step 2 is thiophene monomer, pyrrole monomer or aniline monomer.
6. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1; it is characterized in that in step 2 under nitrogen atmosphere protection; be the potassium hydroxide solution of 2mol/L to adding concentration in reaction system, reaction 4h～8h.
7. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1, it is characterized in that in step 3 being under 7000r/min at rotating speed, the product centrifugal treating 15min that step 2 is obtained, again with deionized water washing 3 times, the product after being washed.
8. a kind of preparation method who synthesizes the magnetic hollow capsule type catalyst of supported platinum nano particle take polystyrene as soft template according to claim 1, product after the washing that it is characterized in that in step 4, step 3 being obtained soaks 9h～12h in toluene solution, obtains the magnetic hollow capsule type catalyst of supported platinum nano particle.
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Cited By (3)
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| CN104998683A (en) * | 2015-06-16 | 2015-10-28 | 厦门大学 | Nano precious metal load polymer vesica and preparing method thereof |
| WO2016090575A1 (en) * | 2014-12-10 | 2016-06-16 | 深圳市森日有机硅材料有限公司 | Microencapsulated platinum metal catalyst and preparation method therefor |
| CN112121862A (en) * | 2020-10-15 | 2020-12-25 | 江西赣江新区有机硅创新研究院有限公司 | Magnetic immobilized platinum catalyst and preparation method and application thereof |
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Cited By (4)
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| WO2016090575A1 (en) * | 2014-12-10 | 2016-06-16 | 深圳市森日有机硅材料有限公司 | Microencapsulated platinum metal catalyst and preparation method therefor |
| CN104998683A (en) * | 2015-06-16 | 2015-10-28 | 厦门大学 | Nano precious metal load polymer vesica and preparing method thereof |
| CN104998683B (en) * | 2015-06-16 | 2017-09-15 | 厦门大学 | A kind of nano-noble metal load aggregation thing vesica and preparation method thereof |
| CN112121862A (en) * | 2020-10-15 | 2020-12-25 | 江西赣江新区有机硅创新研究院有限公司 | Magnetic immobilized platinum catalyst and preparation method and application thereof |
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Application publication date: 20140604 |