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A kind of cyclodextrin-metal complex and its preparation method and application

A technology of metal complexes and cyclodextrins, which is applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the difficulty in product catalyst recovery, harsh reaction conditions, preparation Problems such as complex process, to achieve the effect of cheap and non-toxic materials, simple preparation process, and improved catalytic activity

Active Publication Date: 2022-04-29
HUNAN INSTITUTE OF ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although homogeneous catalysts have high catalytic activity, product purification and catalyst recovery are difficult; although heterogeneous catalysts are simple to separate, they generally have disadvantages such as harsh reaction conditions, solvent and / or auxiliary agents, and unsatisfactory activity, and the preparation process is complicated. expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Catalyst preparation: ultrasonically dissolve 97.3g (100mmol) α-cyclodextrin in 5L water, then add 14g (100mmol) hexamethylenetetramine and 92g MgBr 2 (500mmol), stirred at room temperature for 12h, and the solid powder was washed 4 times with ethanol after removing water by rotary evaporation, and dried in vacuum at 60°C for 12h, and the product was marked as α-CD-MgBr 2 -Hatm.

[0025] (2) Cycloaddition reaction: at room temperature, add α-CD-MgBr to a 30mL autoclave 2 -Hatm0.143mmol, internal standard biphenyl 0.15g, propylene oxide 28.6mmol, feed 2MPa CO under stirring at room temperature 2 , and then put the autoclave into an oil bath reactor with magnetic stirring at 90°C for 6h. After the reaction, place the autoclave in cold water to cool, and then release CO 2 , Take out the reactant, get the supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 99.8%, and the selectivity is 100%.

Embodiment 2

[0027] (1) Catalyst preparation: ultrasonically dissolve 56.7g (50mmol) of β-cyclodextrin in 5L of water, then add 35g (250mmol) of hexamethylenetetramine and 147g of CaI 2 (500mmol), stirred at room temperature for 12h, and the solid powder was washed 4 times with ethanol after removing water by rotary evaporation, and dried in vacuum at 60°C for 12h, and the product was designated as β-CD-CaI 2 -Hatm.

[0028] (2) Cycloaddition reaction: at room temperature, add β-CD-CaI sequentially into a 30mL autoclave 2 -Hatm0.72mmol, internal standard biphenyl 0.15g, epichlorohydrin 28.6mmol, feed 2MPa CO under stirring at room temperature 2 , and then put the autoclave into an oil bath reactor with magnetic stirring at 60°C for 9h. After the reaction, place the autoclave in cold water to cool, and then release CO 2 , Take out the reactant, take the supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 98.5%, and the selectivity is 9...

Embodiment 3

[0030] (1) Catalyst preparation: ultrasonically dissolve 129.7g (100mmol) γ-cyclodextrin in 5L water, then add 2.8g (20mmol) hexamethylenetetramine and 13.6g ZnCl 2 (100mmol), stirred at room temperature for 12h, and the solid powder was washed 4 times with ethanol after removing water by rotary evaporation, and dried in vacuum at 60°C for 12h, and the product was marked as γ-CD-ZnCl 2 -Hatm.

[0031] (2) Cycloaddition reaction: Add γ-CD-ZnCl to a 30mL autoclave at room temperature 2 -Hatm1.43mmol, internal standard biphenyl 0.15g, butylene oxide 28.6mmol, feed 2MPa CO under stirring at room temperature 2 , and then put the autoclave into an oil bath reactor with magnetic stirring at 80°C for 12h. After the reaction, place the autoclave in cold water to cool, and then release CO 2 , Take out the reactant, get the supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 98.6%, and the selectivity is 99.8%.

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Abstract

The invention discloses a cyclodextrin-metal complex and its preparation method and application. The cyclodextrin-metal complex is obtained by adding hexamethylenetetramine and metal halides into an aqueous solution of cyclodextrin, stirring and reacting . The invention adopts a one-pot method to use water as a solvent, and utilizes renewable cyclodextrin, cheap hexamethylenetetramine and metal halides as raw materials to synthesize a cyclodextrin-metal complex with a hydrophobic active center for catalysis CO 2 Cyclic carbonate is synthesized by cycloaddition reaction with epoxide, and the activity of the cyclodextrin-metal complex hardly changes after repeated recycling.

Description

technical field [0001] The invention belongs to CO 2 The technical field of cycloaddition, specifically relates to a kind of cyclodextrin-metal complex and its preparation method and in catalytic CO 2 Application in cycloaddition of cyclic carbonates with epoxides. Background technique [0002] In May 2020, scientists detected CO in the atmosphere 2 The concentration reached 417.2ppm, a record high. With waste CO 2 Synthesis of cyclic carbonates by cycloaddition reaction with epoxides is in line with the principle of sustainable development. There have been a large number of cycloaddition catalysts, including homogeneous catalysts such as metal halides, ionic liquids, organic bases, and metal complexes, and heterogeneous catalysts such as metal oxides, supported catalysts, polyionic liquids, and organometallic framework materials. was reported. Although homogeneous catalysts have high catalytic activity, product purification and catalyst recovery are difficult; althoug...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/18C07D317/36
CPCB01J31/2208B01J31/1835C07D317/36B01J2531/22B01J2531/23B01J2531/26B01J2531/0238B01J2531/0241
Inventor 兰东辉易兵蒲利黄芬朱恒俊区泽堂伍水生沈静邓人杰
Owner HUNAN INSTITUTE OF ENGINEERING
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