CN102189267A

CN102189267A - Method for preparing highly-dispersed regular octahedral platinum nano particles

Info

Publication number: CN102189267A
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: 2011-09-21
Anticipated expiration: 2031-04-26
Also published as: CN102189267B

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 octahedron nano platinum particle

Technical field

That the present invention relates to is a kind of preparation method of high degree of dispersion regular octahedron nano platinum particle.

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 and have different and the physics of general aggregate and a class particle of chemical property.

The pattern of nano particle and degree of crystallinity are prepared the size homogeneous to the performance important influence that it showed, 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 big to show as specific area, and characteristics such as catalytic activity height can be widely used in catalytic field.

The method that prepare at present nano particle has a lot, for example 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 relatively more difficult.

Summary of the invention

The objective 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 is uniformly dispersed, and the productive rate height, degree of crystallinity is good, produces the preparation method of the high high degree of dispersion regular octahedron nano platinum particle of preparation efficiency.

The objective of the invention is to finish by following technical solution, this 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, be labeled as solution 1 with molecular weight; Then with in the seed amino acid surplus the needed by human body 20 one or more, comprise L-lysine, the L-leucine, L-serines etc. are mixed with the aqueous solution of 0.5-2M, 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 the above-mentioned solution 3 of 30ml-60ml and add in the 100ml hydrothermal reaction kettle, add the platinum acid chloride solution of the 50mM-400mM of 1-5ml simultaneously; After above-mentioned solution 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; Adding absolute ethyl alcohol afterwards cleans 3-5 time and is colourless until supernatant liquor; Pour out supernatant liquor then, 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, helps the raising of catalytic reaction efficient.

(2) this method preparation process is simpler and easy, can be used for a large amount of generations fast, and manufacturing cycle is short.

(3) this 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 a 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, be labeled as solution 1 with molecular weight; Then with in the seed amino acid surplus the needed by human body 20 one or more, comprise L-lysine, the L-leucine, L-serines etc. are mixed with the aqueous solution of 0.5-2M, 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 the above-mentioned solution 3 of 30ml-60ml and add in the 100ml hydrothermal reaction kettle, add the platinum acid chloride solution of the 50mM-400mM of 1-5ml simultaneously; After above-mentioned solution 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; Adding absolute ethyl alcohol afterwards cleans 3-5 time and is colourless until supernatant liquor; Pour out supernatant liquor then, 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 allocating multiple organic admixture, successfully induces nano platinum particle Cheng Jing under hydrothermal condition.The present invention prepares a kind of nano platinum particle by multiple high polymer mixing water thermal induction method, has following characteristics: (1). and the nano platinum particle that makes is the regular octahedron configuration, and pattern is regular.

(2). the nano platinum particle that makes does not have 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 tangible 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 the three-dimensional stereovision of nano platinum particle from the depth of color.This nano platinum particle is better dispersed, and size distribution is even, does not have tangible agglomeration.Be expected in catalysis, high-tech areas such as medicine are used widely.

Fig. 2 is the XRD test.Nano platinum particle that XRD test demonstration is obtained 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 octahedron nano platinum particle, this 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, be labeled as solution 1 with molecular weight; Then with in the seed amino acid surplus the needed by human body 20 one or more, comprise L-lysine, the L-leucine, the L-serine is mixed with the aqueous solution of 0.5-2M, is 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 the above-mentioned solution 3 of 30ml-60ml and add in the 100ml hydrothermal reaction kettle, add the platinum acid chloride solution of the 50mM-400mM of 1-5ml simultaneously; After above-mentioned solution 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; Adding absolute ethyl alcohol afterwards cleans 3-5 time and is colourless until supernatant liquor; Pour out supernatant liquor then, add an amount of absolute ethyl alcohol and preserve stand-by.