Polyacid catalyst wrapped by cadmium-based polypyridine macro ring and preparation method thereof

A technology of acid catalyst and pyridine, which is applied in the field of multi-acid catalyst wrapped in cadmium-based polypyridine macrocycle and its preparation, can solve the problems of loading and other problems, and achieve the effects of simple preparation process, improved performance and easy separation

Inactive Publication Date: 2014-11-26
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the loading problem of simple polyoxometalate as a catalyst, so that it can provide more active sites in the catalytic process, greatly improve the catalytic performance, and facilitate recycling and reuse. Polyacid Catalysts Encapsulated by Cadmium-based Polypyridine Macrocycles

Method used

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  • Polyacid catalyst wrapped by cadmium-based polypyridine macro ring and preparation method thereof
  • Polyacid catalyst wrapped by cadmium-based polypyridine macro ring and preparation method thereof
  • Polyacid catalyst wrapped by cadmium-based polypyridine macro ring and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Synthesis of Quaternary Ammonium Salt of Keggin Phosphotungstic Acid Catalyst Encapsulated by Cadmium-based Polypyridine Macrocycle

[0049] Dissolve cadmium-based polypyridine macrocycle (0.008 mmol) in 10 ml of methanol and acetonitrile (1:6) mixed solvent, at the same time, [(n-C 4 h 9 ) 4 N] 4 HPW 11 M(H 2 O)O 39 (M=Ni) single transition metal substituted Keggin phosphotungstic acid quaternary ammonium salt (0.0251mmol) was dissolved in 10ml of acetonitrile to obtain acetonitrile solution of cadmium-based polypyridine macrocycle and acetonitrile solution of polyacid, under slow stirring Under normal temperature, the two solutions were mixed, stirred at room temperature for 24h, centrifuged for 10min, and the resulting solid was washed three times with acetonitrile (15ml), then twice with ethanol (10ml), and dried under natural conditions to obtain cadmium-based polypyridine Macrocyclic Nickel-Substituted Keggin Phosphotungstic Acid Catalysts. The yield is ab...

Embodiment 2

[0051] Synthesis of Quaternary Ammonium Salt of Keggin Phosphotungstic Acid Catalyst Encapsulated by Cadmium-based Polypyridine Macrocycle

[0052] Dissolve cadmium-based polypyridine macrocycle (0.0095 mmol) in 12 ml of methanol and acetonitrile (1:5) mixed solvent, at the same time, [(n-C 4 h 9 ) 4 N] 4 HPW 11 M(H 2 O)O 39 (M=Ni) single transition metal substituted Keggin phosphotungstic acid quaternary ammonium salt (0.0292mmol) was dissolved in 12ml of acetonitrile to obtain acetonitrile solution of cadmium-based polypyridine macrocycle and acetonitrile solution of polyacid, under slow stirring Under normal conditions, the two solutions were mixed, stirred at room temperature for 24 hours, and centrifuged for 12 minutes. The resulting solid was washed three times with acetonitrile (15ml), then washed twice with ethanol (10ml), and dried under natural conditions to obtain cadmium-based polypyridine Macrocyclic Nickel-Substituted Keggin Phosphotungstic Acid Catalysts....

Embodiment 3

[0054] Synthesis of Quaternary Ammonium Salt of Keggin Phosphotungstic Acid Catalyst Encapsulated by Cadmium-based Polypyridine Macrocycle

[0055] Dissolve cadmium-based polypyridine macrocycle (0.009 mmol) in 10 ml of methanol and acetonitrile (1:4) mixed solvent, at the same time, [(n-C 4 h 9 ) 4 N] 4 HPW 11 M(H 2 O)O 39 (M=Ni) single-transition metal substituted Keggin phosphotungstic acid quaternary ammonium salt (0.027mmol) was dissolved in 10ml of acetonitrile to obtain acetonitrile solution of cadmium-based polypyridine macrocycle and acetonitrile solution of polyacid, under slow stirring Under normal conditions, the two solutions were mixed, stirred at room temperature for 20 hours, centrifuged for 15 minutes, the resulting solid was washed three times with acetonitrile (20ml), and then washed twice with ethanol (10ml), and dried under natural conditions to obtain cadmium-based polypyridine Macrocyclic Nickel-Substituted Keggin Phosphotungstic Acid Catalysts. ...

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Abstract

The invention discloses a polyacid catalyst wrapped by cadmium-based polypyridine macro ring and a preparation method thereof; according to the method, the cadmium-based polypyridine macro ring and polyoxometallate are respectively dissolved in acetonitrile solution, then mutual dripped slowly, stood, and precipitated to obtain the needed catalyst. The catalyst is used in epoxidation of cyclooctene, the conversion rate is as high as 95.11%, and the selectivity is over 95.72%. The catalyst provided by the invention not only retains excellent catalytic performances of the polyacid componnet, can realize the catalyst recovery, improves the shortcoming that traditional polyacid catalysts cannot be recycled, and has the advantages of simple preparation process and high yield.

Description

technical field [0001] The invention relates to the technical field of catalyst materials, in particular to a polyacid catalyst wrapped with a cadmium-based polypyridine macrocycle and a preparation method thereof. Background technique [0002] Polyoxometalates (abbreviated as POMs, commonly known as polyacids) are metal-oxygen clusters rich in transition elements such as Mo, W, V, Nb and Ta in the framework structure. Due to the advantages of acidity, redox, low toxicity, and adjustable composition and structure, POMs have a wide range of applications in structure research, catalysis, medicine, photoelectrochemistry, etc., and are one of the research hotspots in the field of inorganic chemistry. At present, the catalytic chemistry of POMs has become one of the most promising research directions in the field of POMs science, and has attracted extensive attention from domestic and foreign scholars. Although POMs homogeneous catalysts have advantages in catalytic activity, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D301/12C07D303/04
CPCY02P20/50Y02P20/584
Inventor 许颜清席亚茹王金亮肖飞邹波胡长文
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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