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Platinum/carbon nanotube catalyst and preparation method and application thereof

A carbon nanotube and platinum nanotechnology, which is applied in the field of platinum/carbon nanotube catalysts to achieve the effect of simple preparation and mild conditions

Inactive Publication Date: 2011-05-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, domestic and foreign studies on the heterogeneous asymmetric hydrogenation of α-keto esters have shown that a variety of structural and functional supports and chiral modifier catalysts have been tried, and compared in terms of reaction performance, stability, and practicability. , there is no heterogeneous catalyst that surpasses or can compete with the leading commercial platinum-alumina catalysts in the international market

Method used

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  • Platinum/carbon nanotube catalyst and preparation method and application thereof
  • Platinum/carbon nanotube catalyst and preparation method and application thereof
  • Platinum/carbon nanotube catalyst and preparation method and application thereof

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preparation example Construction

[0055] The preparation and asymmetric hydrogenation reaction of the platinum-carbon nanotube catalyst according to the present invention are respectively detailed as follows:

[0056] (1) Preparation of carbon nanotube support

[0057] Treat the purified carbon nanotubes with a certain geometric size with concentrated nitric acid (65-68%), heat them under stirring for 4-16 hours, and heat them at a temperature of 110-160°C, then wash and filter them, wash with water until the pH value of the filtrate is neutral, and place in 50 ~ 120 ℃ drying oven for 12 ~ 24h, to obtain functionalized carbon nanotube black carrier, used to prepare platinum / carbon nanotube catalysts (coded as Pt-in-CNTs) and Platinum / carbon nanotube catalyst (coded as Pt-out-CNTs) loaded on the outer surface of the carbon nanotube lumen.

[0058] (2) Ultrasonic treatment impregnation

[0059] Submerge the functionalized carbon nanotube carrier in an aqueous solution of chloroplatinic acid of a certain concen...

Embodiment 1

[0086] Preparation of functionalized carbon nanotube supports.

[0087]Weigh 4.0 grams of purified carbon nanotubes (average inner diameter 4-8nm, outer diameter 10-20nm) and place in a 250ml round-bottomed flask, put into a magnetic stirrer, add 200ml of concentrated nitric acid (65-68%), and put it under reflux Condenser, heated to 110-160°C in an oil bath, treated with stirring for 4-16 hours (h), cooled, washed and filtered with deionized water, washed until the pH of the filtrate was neutral, and then placed in an oven at 50-120°C The temperature is kept constant for 12-24 hours to obtain a functionalized carbon nanotube carrier.

Embodiment 2

[0089] Preparation of Platinum / Carbon Nanotube Catalysts Loaded with Platinum Nanoparticles in the Lumen of Carbon Tubes

[0090] 1) In a round bottom flask, add 2.72ml chloroplatinic acid aqueous solution (concentration is 18.5mg Pt / ml, 5% Pt load) into 20ml deionized water, mix evenly with electromagnetic stirring, then add 1.0g dry carbon nanotubes The carrier (which has been functionalized) is then placed in an ultrasonic oscillator, and the ultrasonic treatment is started for 1-4 hours.

[0091] 2) Take it out and continue to immerse under stirring for more than 12h.

[0092] 3) Slowly dry the material after step 2 from room temperature to 110°C at a rate of 0.5°C / min, and keep drying at this temperature for 48h.

[0093] 4) The catalyst precursor obtained in step 3 is reduced in an aqueous solution of sodium formate (the amount of sodium formate is about 10 to 20 times the molar amount of platinum carried on the catalyst, 70 to 120° C.). After reduction, filter, wash w...

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Abstract

The invention relates to a platinum / carbon nanotube catalyst suitable for multiphase asymmetric hydrogenation reaction. Platinum is loaded on a carbon nanotube carrier. A preparation method comprises the following steps of: heating a purified carbon nanotube in nitric acid, washing, filtering, washing by using water until the pH value of filtrate is neutral, drying to obtain the carbon nanotube carrier, soaking in aqueous solution of chloroplatinic acid, and performing ultrasonic treatment at room temperature; and stirring and impregnating a mixture of the carbon nanotube and the aqueous solution of chloroplatinic acid, raising the temperature to 110 DEG C from room temperature, drying at the temperature of 110 DEG C, grinding into fine powder, reducing by using aqueous solution of sodiumformate with heating, filtering, washing by using deionized water and drying. The invention also provides the preparation method of the catalyst and application of the catalyst to the multiphase asymmetric hydrogenation reaction.

Description

technical field [0001] The invention relates to a platinum / carbon nanotube catalyst suitable for heterogeneous asymmetric hydrogenation. [0002] The present invention also relates to a preparation method of the above-mentioned platinum / carbon nanotube catalyst. [0003] The present invention also relates to the application of the above-mentioned platinum / carbon nanotube catalyst Background technique [0004] Since the 1990s, people's demand for single-enantiomer chiral compounds is huge and rapidly increasing year by year. At present, this demand is concentrated in the fields of medicine, pesticides and fine chemicals. Taking the world's pharmaceutical market as an example, in 2005, the global market value of single enantiomer drug sales exceeded US$172 billion, with an annual growth rate of about 10%, and in 2008, the sales market value exceeded US$200 billion. Asymmetric catalysis (homogeneous asymmetric catalysis and heterogeneous asymmetric catalysis) plays an importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J21/18B01J37/00C07B53/00C07C29/149C07C31/20C07C33/26
CPCB01J21/185B01J37/0201B01J37/343B82Y30/00C07B35/02B01J23/42B01J35/23B01J37/009B01J37/16C07C67/30
Inventor 李灿陈志坚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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