Multiphase unsymmetrical hydrogenated catalyst, preparation method and application thereof

A catalyst, asymmetric technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, metal/metal oxide/metal hydroxide catalysts, etc., to achieve high activity and optical selectivity Effect

Inactive Publication Date: 2008-10-15
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, FDU-14 is used as a carrier to support noble metal catalysts and is used in heterogeneous asymmetric catalytic reactions to synthesize chiral drugs or chiral drug precursors. There are no related reports.

Method used

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  • Multiphase unsymmetrical hydrogenated catalyst, preparation method and application thereof
  • Multiphase unsymmetrical hydrogenated catalyst, preparation method and application thereof
  • Multiphase unsymmetrical hydrogenated catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Taking chloroplatinic acid as an example, the preparation method of Pt / FDU-14 catalyst is illustrated. Specific steps are as follows:

[0022] (1) In 1.406g FDU-14, add about 20ml distilled water earlier, then drip 5ml chloroplatinic acid aqueous solution (concentration is 14.8mg Pt / ml) under electromagnetic stirring, the carrying capacity of metal platinum is 5.0% (weight percentage ), continued stirring and impregnating for 4-6 hours, evaporated the excess water in a water bath, and then dried the catalyst precursor in an oven at 80° C. overnight (about 16 hours).

[0023] (2) Calcining the catalyst precursor obtained in step 1 in a muffle furnace at 350° C. for 2 hours under vacuum.

[0024] (3) Put the catalyst precursor obtained in step 2 in sodium formate solution (the consumption of sodium formate is about 10 times of the molar amount of platinum contained in the catalyst, the temperature is 90° C., after reflux for 1 h, the catalyst is filtered and washed with ...

Embodiment 2

[0026] Same as Example 1, except that the temperature used in step (2) is 200° C., and the time is 0.5 hour. The prepared catalyst number is Cat-H 2 PtCl 6 -200. The dispersion degree of metal platinum on the surface of FDU-14 and the average size of platinum particles measured by CO chemisorption are shown in Table 1.

Embodiment 3

[0028] Same as Example 1, except that the temperature used in step (2) is 400° C., and the time is 4 hours. The prepared catalyst number is Cat-H 2 PtCl 6 -400. The dispersion degree of metal platinum on the surface of FDU-14 and the average size of platinum particles measured by CO chemisorption are shown in Table 1.

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Abstract

The invention relates to a heterogeneous catalyst used in an asymmetric catalytic hydrogenation reaction of Alpha-keto ester, and the preparation as well as the application thereof, and belongs to the technology field of a chemical catalyst and synthesis. The expression of the catalyst is Pt/FDU-14; when in preparation, platinic chloride or Tetrammine platinum (2) Chloride is used as an active component precursor, and FDU-14 is used as a carrier; part of catalyst precursor is vacuum-roasted in a muffle furnace after insuccation and torrefaction, and finally the catalyst precursor is deoxygenized in sodium formate water solution to prepare the heterogeneous catalyst, wherein, the dispersion degree of active component platinum on the surface of the FDU-14 is 0.14 to 0.35, the loading of metallic platinum is 5.0 percent, and the mean particle size of platinum particles ranges from 3.2 to 8.0nm. When the heterogeneous catalyst is used in the asymmetric catalytic hydrogenation reaction of ethyl pyruvate under the room temperature and the medium hydrogen pressure, high activity and optical selectivity more than 70 percent are obtained in acetic acid solution, and the heterogeneous catalyst can be repeatedly used for more than 15 times.

Description

technical field [0001] The invention relates to a heterogeneous catalyst for the asymmetric catalytic hydrogenation reaction of α-keto esters, a preparation method and application of the heterogeneous catalyst, and belongs to the technical field of chemical catalysts and synthesis. Background technique [0002] In the past ten years, people's demand for single-enantiomer chiral compounds is huge and increasing year by year. This demand is mainly reflected in the fields of medicine, pesticides and fine chemicals. Taking the pharmaceutical market as an example, in 2002, the global sales volume of single enantiomer drugs exceeded 159 billion US dollars (an increase of 8% compared with 2001). Asymmetric catalysis plays an important role in all methods to obtain single enantiomer compounds, and this method has been widely used in many types of asymmetric synthesis reactions. In addition to the advantages of easy separation, easy reuse of catalysts, and easy purification of produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J31/06C07B53/00C07B35/02
Inventor 李晓红沈亚丽吴鹏
Owner EAST CHINA NORMAL UNIV
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