CN102189267A - 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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- CN102189267A CN102189267A CN 201110105032 CN201110105032A CN102189267A CN 102189267 A CN102189267 A CN 102189267A CN 201110105032 CN201110105032 CN 201110105032 CN 201110105032 A CN201110105032 A CN 201110105032A CN 102189267 A CN102189267 A CN 102189267A
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- chloroplatinic acid
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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
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 30
- 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 13
- 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
- 229940024606 amino acid Drugs 0.000 claims description 3
- 235000001014 amino acid Nutrition 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
- WPLOVIFNBMNBPD-ATHMIXSHSA-N subtilin Chemical compound CC1SCC(NC2=O)C(=O)NC(CC(N)=O)C(=O)NC(C(=O)NC(CCCCN)C(=O)NC(C(C)CC)C(=O)NC(=C)C(=O)NC(CCCCN)C(O)=O)CSC(C)C2NC(=O)C(CC(C)C)NC(=O)C1NC(=O)C(CCC(N)=O)NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C1NC(=O)C(=C/C)/NC(=O)C(CCC(N)=O)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)CNC(=O)C(NC(=O)C(NC(=O)C2NC(=O)CNC(=O)C3CCCN3C(=O)C(NC(=O)C3NC(=O)C(CC(C)C)NC(=O)C(=C)NC(=O)C(CCC(O)=O)NC(=O)C(NC(=O)C(CCCCN)NC(=O)C(N)CC=4C5=CC=CC=C5NC=4)CSC3)C(C)SC2)C(C)C)C(C)SC1)CC1=CC=CC=C1 WPLOVIFNBMNBPD-ATHMIXSHSA-N 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims 2
- 229960001153 serine Drugs 0.000 claims 1
- 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
- 150000008550 L-serines Chemical class 0.000 description 2
- 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
- 239000000126 substance Substances 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
- 230000006698 induction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000642 polymer Polymers 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 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)
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.
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| CN 201110105032 CN102189267B (en) | 2011-04-26 | 2011-04-26 | Method for preparing highly-dispersed regular octahedral platinum nano particles |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103143719A (en) * | 2012-12-21 | 2013-06-12 | 浙江理工大学 | Preparation method of platinum nanoparticle loaded platinum nanoparticle crystals |
| CN103352254A (en) * | 2013-07-05 | 2013-10-16 | 浙江大学 | Method for preparing octahedral platinoid alloy nanocrystals and octahedral platinoid alloy nanocrystal prepared through adopting same |
| 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 |
| CN104451782A (en) * | 2014-12-01 | 2015-03-25 | 上海师范大学 | Octahedral platinum nanoparticles as well as synthesis method and application thereof |
| CN104607652A (en) * | 2015-01-17 | 2015-05-13 | 南京师范大学 | Controllable precious metal nanocatalyst synthesis method with amino acid as soft templates |
| CN105789647A (en) * | 2016-03-16 | 2016-07-20 | 杭州禹净环境科技有限公司 | Preparation method of platinum nano hollow tube |
| CN106098389A (en) * | 2016-07-09 | 2016-11-09 | 王瑞明 | The preparation method containing platinum electrode that automobile batteries uses |
| CN111069625A (en) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002062509A1 (en) * | 2001-02-08 | 2002-08-15 | Hitachi Maxell, Ltd. | Metal alloy fine particles and method for production thereof |
| CN1678514A (en) * | 2002-07-03 | 2005-10-05 | 独立行政法人科学技术振兴机构 | Noble metal nanotube and method for preparation thereof |
| CN101132858A (en) * | 2004-11-17 | 2008-02-27 | 上游技术革新有限公司 | Multicomponent nanoparticles formed using a dispersing agent |
| CN101622090A (en) * | 2007-02-27 | 2010-01-06 | 三菱麻铁里亚尔株式会社 | The synthetic method of dispersion solution of metal nanoparticle and preparation method thereof and metal nanoparticle |
| CN101683693A (en) * | 2008-09-25 | 2010-03-31 | 三星电机株式会社 | Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed |
| CN101821039A (en) * | 2007-09-27 | 2010-09-01 | 巴斯夫欧洲公司 | Isolable and redispersable transition metal nanoparticles their preparation and use as ir absorbers |
| CN102009184A (en) * | 2009-09-04 | 2011-04-13 | 施乐公司 | Method for preparing metal nanoparticles, composition thereof and process of forming metal frame |
-
2011
- 2011-04-26 CN CN 201110105032 patent/CN102189267B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002062509A1 (en) * | 2001-02-08 | 2002-08-15 | Hitachi Maxell, Ltd. | Metal alloy fine particles and method for production thereof |
| CN1678514A (en) * | 2002-07-03 | 2005-10-05 | 独立行政法人科学技术振兴机构 | Noble metal nanotube and method for preparation thereof |
| CN101132858A (en) * | 2004-11-17 | 2008-02-27 | 上游技术革新有限公司 | Multicomponent nanoparticles formed using a dispersing agent |
| CN101622090A (en) * | 2007-02-27 | 2010-01-06 | 三菱麻铁里亚尔株式会社 | The synthetic method of dispersion solution of metal nanoparticle and preparation method thereof and metal nanoparticle |
| CN101821039A (en) * | 2007-09-27 | 2010-09-01 | 巴斯夫欧洲公司 | Isolable and redispersable transition metal nanoparticles their preparation and use as ir absorbers |
| CN101683693A (en) * | 2008-09-25 | 2010-03-31 | 三星电机株式会社 | Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed |
| CN102009184A (en) * | 2009-09-04 | 2011-04-13 | 施乐公司 | Method for preparing metal nanoparticles, composition thereof and process of forming metal frame |
Cited By (12)
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|---|---|---|---|---|
| CN103143719A (en) * | 2012-12-21 | 2013-06-12 | 浙江理工大学 | Preparation method of platinum nanoparticle loaded platinum nanoparticle crystals |
| 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 |
| CN103352254A (en) * | 2013-07-05 | 2013-10-16 | 浙江大学 | Method for preparing octahedral platinoid alloy nanocrystals and octahedral platinoid alloy nanocrystal prepared through adopting same |
| 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 |
| CN104451782A (en) * | 2014-12-01 | 2015-03-25 | 上海师范大学 | Octahedral platinum nanoparticles as well as synthesis method and application thereof |
| CN104607652A (en) * | 2015-01-17 | 2015-05-13 | 南京师范大学 | Controllable precious metal nanocatalyst synthesis method with amino acid as soft templates |
| CN105789647A (en) * | 2016-03-16 | 2016-07-20 | 杭州禹净环境科技有限公司 | Preparation method of platinum nano hollow tube |
| CN106098389A (en) * | 2016-07-09 | 2016-11-09 | 王瑞明 | The preparation method containing platinum electrode that automobile batteries uses |
| 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 |
| CN111069625A (en) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
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