CN102189267B

CN102189267B - Method for preparing highly-dispersed regular octahedral platinum nano particles

Info

Publication number: CN102189267B
Application number: CN 201110105032
Authority: CN
Inventors: 王晟; 王騊; 许学飞
Original assignee: Zhejiang University of Technology ZJUT
Current assignee: Zhejiang University of Technology ZJUT
Priority date: 2011-04-26
Filing date: 2011-04-26
Publication date: 2013-04-10
Anticipated expiration: 2031-04-26
Also published as: CN102189267A

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

A kind of preparation method of high degree of dispersion regular octahedral platinum nano particles

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. 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.