CN102189267B - Method for preparing highly-dispersed regular octahedral platinum nano particles - Google Patents
Method for preparing highly-dispersed regular octahedral platinum nano particles Download PDFInfo
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- CN102189267B CN102189267B CN 201110105032 CN201110105032A CN102189267B CN 102189267 B CN102189267 B CN 102189267B CN 201110105032 CN201110105032 CN 201110105032 CN 201110105032 A CN201110105032 A CN 201110105032A CN 102189267 B CN102189267 B CN 102189267B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 8
- 239000005416 organic matter Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- 150000001413 amino acids Chemical class 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 7
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical compound CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 235000019454 L-leucine Nutrition 0.000 claims description 3
- 239000004395 L-leucine Substances 0.000 claims description 3
- -1 Serine Chemical class 0.000 claims description 3
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims description 3
- 229940024606 amino acid Drugs 0.000 claims description 3
- 229960003136 leucine Drugs 0.000 claims description 3
- 230000035800 maturation Effects 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000001939 inductive effect Effects 0.000 abstract 3
- 229910002621 H2PtCl6 Inorganic materials 0.000 abstract 1
- 230000005070 ripening Effects 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000011550 stock solution Substances 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing highly-dispersed regular octahedral platinum nano particles. The method comprises the following steps of: 1, preparing chloroplatinic acid stock solution, namely dissolving 0.5 to 2g of chloroplatinic acid (H2PtCl6) in pure water to prepare chloroplatinic acid solution with the concentration of 50 to 400mM; 2, mixing organic matter mixed inducing solution, namely treating polyethylene glycol with the molecular weight of 600 to 2,000 to prepare aqueous solution with the concentration of 0.5 to 2M, and marking the aqueous solution as solution 1; treating one or more of more than 20 kinds of amino acid which is required by a human body to prepare the aqueous solution with the concentration of 0.5 to 2M, and marking the aqueous solution as solution 2; mixing the solution 1 and the solution 2 in a ratio of 1 to 1 to prepare the organic matter mixed inducing solution and marking the solution as solution 3; and 3, performing hydrothermal inducing, namely adding 30 to 60ml of the solution 3 into 100ml of a hydro-thermal reaction kettle, simultaneously adding 1 to 5ml of chloroplatinic acid solution with the concentration of 50 to 400Mm; and stirring the solution for half an hour, performing hydrothermal treatment at the temperature of between 150 and 200 DEG C for 3 to 8 hours, wherein after the hydrothermal treatment, the particle ripening placement time is 4 to 8 hours.
Description
Technical field
That the present invention relates to is a kind of preparation method of high degree of dispersion regular octahedral platinum nano particles.
Background technology
The generalized definition of nano particle reaches a nano level class particle for its particle size of general reference.And after its narrow sense is defined as particle size and reaches nanoscale, show a class particle of the physics and chemistry performance with different and general aggregate.
The pattern of nano particle and degree of crystallinity have important impact to its performance that shows, and prepare the size homogeneous, and pattern is regular, and the good nano particle of degree of crystallinity has great significance for nano material.Such particle often has good particle effect, and it is large to show as specific area, and the catalytic activity high can be widely used in catalytic field.
The method for preparing at present nano particle has a lot, such as hydro-thermal method, template, sol-gal process etc., however to obtain the size homogeneous, the nano particle that pattern is regular and degree of crystallinity is good is difficulty relatively.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, and provide a kind of method simple and easy, swift to operate, the nano particle profile rule of gained be uniformly dispersed, and productive rate is high, degree of crystallinity is good, the preparation method of the high degree of dispersion regular octahedral platinum nano particles that manufacture efficient is high.
The objective of the invention is to finish by following technical solution, the method comprises following several roads step: the 1) preparation of chloroplatinic acid stoste: with the chloroplatinic acid (H of 0.5g-2g
2PtCl
6) be dissolved in the pure water, be made into the platinum acid chloride solution that concentration is 50mM-400mM; 2) modulation of organic matter mixing induced liquid: at first be the aqueous solution that the polyethylene glycol of 600-2000 is mixed with 0.5-2M with molecular weight, be labeled as solution 1; Then with 1B, the L-leucine, one or more are mixed with the aqueous solution of 0.5-2M in 3 seed amino acids such as Serine, are labeled as solution 2; At last solution 1 and solution 2 are mixed with organic matter mixing induced liquid with the ratio of 1:1, are labeled as solution 3; 3) hydro-thermal revulsion: get 30ml-60ml mentioned solution 3 and add in the 100ml hydrothermal reaction kettle, the platinum acid chloride solution that adds simultaneously the 50mM-400mM of 1-5ml mixes, and is labeled as solution 4; After mentioned solution 4 stirred half an hour, carry out hydrothermal treatment consists, the processing time is 3-8 hour, and treatment temperature is the 150-200 degree, and particle maturation standing time is 4-8 hour after the hydrothermal treatment consists; 4) post processing of preparation products therefrom: the centrifuge tube that will fill product under the rotating speed of 5000-6500 rpm centrifugal 5-10 minute; Add afterwards absolute ethyl alcohol and clean 3-5 time until supernatant liquor is colourless; Then pour out supernatant liquor, add an amount of absolute ethyl alcohol and preserve stand-by.
Beneficial effect of the present invention: (1) nano platinum particle pattern is regular, and degree of crystallinity is better, and effecting reaction point is many, can be used for catalytic reaction, is conducive to the raising of catalytic reaction efficient.
(2) the method preparation process is simpler and easy, can be used for a large amount of fast generations, and manufacturing cycle is short.
(3) the method equipment needed thereby is simple, and preparation condition is controlled easily, and it is higher that product is prepared into power.
Description of drawings
Fig. 1 regular octahedron configuration nano platinum particle figure.
Fig. 2 is regular octahedron configuration nano platinum particle enlarged drawing.
Fig. 3 is the XRD test chart of regular octahedron configuration nano platinum particle.
The specific embodiment
The present invention will be described in detail below in conjunction with specific embodiment: method comprises following several roads step: the 1) preparation of chloroplatinic acid stoste: with the chloroplatinic acid (H of 0.5g-2g
2PtCl
6) be dissolved in the pure water, be made into the platinum acid chloride solution that concentration is 50mM-400mM; 2) modulation of organic matter mixing induced liquid: at first be the aqueous solution that the polyethylene glycol of 600-2000 is mixed with 0.5-2M with molecular weight, be labeled as solution 1; Then with 1B, the L-leucine, one or more are mixed with the aqueous solution of 0.5-2M in 3 seed amino acids such as Serine, are labeled as solution 2; At last solution 1 and solution 2 are mixed with organic matter mixing induced liquid with the ratio of 1:1, are labeled as solution 3; 3) hydro-thermal revulsion: get 30ml-60ml mentioned solution 3 and add in the 100ml hydrothermal reaction kettle, the platinum acid chloride solution that adds simultaneously the 50mM-400mM of 1-5ml mixes, and is labeled as solution 4; After mentioned solution 4 stirred half an hour, carry out hydrothermal treatment consists, the processing time is 3-8 hour, and treatment temperature is the 150-200 degree, and particle maturation standing time is 4-8 hour after the hydrothermal treatment consists; 4) post processing of preparation products therefrom: the centrifuge tube that will fill product under the rotating speed of 5000-6500 rpm centrifugal 5-10 minute; Add afterwards absolute ethyl alcohol and clean 3-5 time until supernatant liquor is colourless; Then pour out supernatant liquor, add an amount of absolute ethyl alcohol and preserve stand-by.
The present invention is on the basis that studies for a long period of time, by allotment gas chromatography mixture, successfully induces nano platinum particle Cheng Jing under hydrothermal condition.The present invention obtains a kind of nano platinum particle by multiple high polymer mixing water thermal induction legal system is standby, has following features: (1). and the nano platinum particle that makes is the regular octahedron configuration, and pattern is regular.
(2). the nano platinum particle that makes is without reunion, good dispersion, size homogeneous.
(3). the nano platinum particle degree of crystallinity that makes is good.
Fig. 1 is that transmission electron microscope is observed to regular octahedron configuration nano platinum particle.As seen from Figure 2, this nano platinum particle is better dispersed, and size distribution is even, does not have obvious agglomeration.As seen from Figure 3, the nano platinum particle profile rule that obtains, the length of side is about about 20nm, and the corner is clear, and symmetry is good, and can find out from the depth of color the three-dimensional stereovision of nano platinum particle.This nano platinum particle is better dispersed, and size distribution is even, does not have obvious agglomeration.Be expected in catalysis, the high-tech areas such as medicine are used widely.
Fig. 2 is the XRD test.The nano platinum particle that XRD test demonstration obtains and (111) of simple substance Pt (JCPDS 04-0802), (200) and (220) face diffraction maximum matches, and what acquisition was described is the good platinum particles of degree of crystallinity.
Claims (1)
1. the preparation method of a high degree of dispersion regular octahedral platinum nano particles, the method comprises following several roads step: the 1) preparation of chloroplatinic acid stoste: with the chloroplatinic acid (H of 0.5g-2g
2PtCl
6) be dissolved in the pure water, be made into the platinum acid chloride solution that concentration is 50mM-400mM; 2) modulation of organic matter mixing induced liquid: at first be the aqueous solution that the polyethylene glycol of 600-2000 is mixed with 0.5-2M with molecular weight, be labeled as solution 1; Then with 1B, the L-leucine, one or more are mixed with the aqueous solution of 0.5-2M in 3 seed amino acids such as Serine, are labeled as solution 2; At last solution 1 and solution 2 are mixed with organic matter mixing induced liquid with the ratio of 1:1, are labeled as solution 3; 3) hydro-thermal revulsion: get 30ml-60ml mentioned solution 3 and add in the 100ml hydrothermal reaction kettle, the platinum acid chloride solution that adds simultaneously the 50mM-400mM of 1-5ml mixes, and is labeled as solution 4; After mentioned solution 4 stirred half an hour, carry out hydrothermal treatment consists, the processing time is 3-8 hour, and treatment temperature is the 150-200 degree, and particle maturation standing time is 4-8 hour after the hydrothermal treatment consists; 4) post processing of preparation products therefrom: the centrifuge tube that will fill product under the rotating speed of 5000-6500 rpm centrifugal 5-10 minute; Add afterwards absolute ethyl alcohol and clean 3-5 time until supernatant liquor is colourless; Then pour out supernatant liquor, add an amount of absolute ethyl alcohol and preserve stand-by.
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| CN102189267B true CN102189267B (en) | 2013-04-10 |
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| CN103143719B (en) * | 2012-12-21 | 2015-08-05 | 浙江理工大学 | A kind of preparation method of nano platinum particle supported platinum nano crystal |
| CN103055900A (en) * | 2013-01-28 | 2013-04-24 | 上海电力学院 | Pt/CdS composite visible-light-induced photocatalyst and preparation method thereof |
| CN103352254B (en) * | 2013-07-05 | 2016-01-20 | 浙江大学 | The octahedra Mock gold of the preparation method that a kind of octahedra Mock gold is nanocrystalline and preparation thereof is nanocrystalline |
| CN104384522A (en) * | 2014-09-23 | 2015-03-04 | 苏州禹净环境科技有限责任公司 | Preparing method of nanometer cage-shaped platinum particles |
| CN104451782B (en) * | 2014-12-01 | 2017-08-25 | 上海师范大学 | A kind of octahedral structure nano platinum particle and its synthetic method and application |
| CN104607652B (en) * | 2015-01-17 | 2017-04-12 | 南京师范大学 | Controllable precious metal nanocatalyst synthesis method with amino acid as soft templates |
| CN105789647B (en) * | 2016-03-16 | 2018-09-11 | 杭州同净环境科技有限公司 | A kind of preparation method of platinum nanometer hollow out pipe |
| CN106098389B (en) * | 2016-07-09 | 2018-06-26 | 江苏锡沂高新区科技发展有限公司 | The preparation method containing platinum electrode that automobile batteries uses |
| CN111069625B (en) * | 2020-01-06 | 2021-10-01 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
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Patent Citations (7)
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