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Method for preparing cyclic carbonate with chitosan loading type catalyst

A technology of supported catalysts and cyclic carbonates, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as difficult separation of homogeneous catalysts

Active Publication Date: 2012-03-28
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the existing homogeneous catalysts are difficult to separate, and to provide a method for preparing cyclic carbonates by catalyzing epoxy compounds and carbon dioxide cycloadditions with ionic liquid catalysts chemically supported by renewable resources chitosan , to reduce investment costs and simplify operation

Method used

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  • Method for preparing cyclic carbonate with chitosan loading type catalyst
  • Method for preparing cyclic carbonate with chitosan loading type catalyst
  • Method for preparing cyclic carbonate with chitosan loading type catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Preparation method of chitosan-loaded imidazole ionic liquid:

[0021] 1) Preparation of 1-(2-bromoethyl)-3-methylimidazolium bromide (a, m=2, X=Br) ionic liquid: In a three-necked flask, slowly drop N-methylimidazole to three Double molar equivalent of 1,2-dibromoethane was stirred at 50° C. for 24 h. After stopping the reaction, the solid product was washed with acetone and suction-filtered three times, then vacuum-dried at 50°C for 6 hours, and then used;

[0022] 2) chitosan chemical loading: 4g chitosan (deacetylation degree 80%, average molecular weight 5×10 4 ), 15g of 1-(2-bromoethyl)-3-methylimidazolium bromide aqueous solution (60wt%) and 30mL of isopropanol were added to a 100mL three-necked flask, and the reaction was stirred at 75°C for 24h. After stopping the reaction, adjust the pH value of the reaction system to 6, add ethanol to precipitate the product, wash and dry the product to obtain the product. Analysis and characterization showed that the load...

Embodiment 2

[0025] Chitosan-loaded quaternary phosphonium ionic liquid preparation method:

[0026] 1) Preparation of (3-chloropropyl)triphenylphosphonium chloride (b, x=3, R' is phenyl, X=Cl) ionic liquid: In a three-necked flask, slowly add triphenylphosphine into three Double molar equivalent of 1,3-dichloropropane, reacted with magnetic stirring at 80°C for 24h. After stopping the reaction, the solid product was washed with acetone and suction-filtered three times, then vacuum-dried at 50°C for 6 hours, and then used;

[0027] 2) chitosan chemical loading: 4g chitosan (deacetylation degree 80%, average molecular weight 5×10 4 ), 20g (3-chloropropyl) triphenylphosphonium chloride aqueous solution (80wt%) and 40mL isopropanol were added to a 100mL three-necked flask, and stirred at 80°C for 48h. After stopping the reaction, adjust the pH value of the reaction system to 7, add ethanol to precipitate the product, wash and dry the product to obtain the product. Analysis and characteriza...

Embodiment 3

[0029]

[0030] Implementation method: in 100mL stainless steel autoclave, add the 1-methyl-3-ethyl imidazole bromide (a, m= 2, X=Br) 0.5g (1.5mmol), 10mL propylene oxide (1a) (0.14mol), a closed reaction vessel, filled with an appropriate amount of pressure CO 2 , the temperature was controlled by a temperature controller to slowly rise to 120° C., and then the reaction pressure was controlled to 2.5 MPa, and the reaction was carried out for 4 hours. After the reaction, the reactor was cooled to room temperature, and excess CO was released slowly. 2 After the catalyst was separated by filtration, the obtained product (2a) was quantitatively analyzed by a gas chromatography-mass spectrometer, the selectivity was >99.8%, and the yield was 96%.

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Abstract

The invention relates to a method for preparing cyclic carbonate with chitosan loading type catalyst. The method is characterized in that epoxy compounds and carbon dioxide are taken as raw materials, chitosan loading type catalyst is used during the reaction process, and then cyclic carbonate is synthesized under the reaction conditions of 0.1 to 10 MPa, 40 to 160 DEG C and 0.3 to 10 hours. Based on the concerted catalysis action of reactive groups in the carrier, cyclic carbonate can be synthesized with high efficiency and high selectivity under the condition that no other assistant or promoter is required to be added.

Description

Technical field: [0001] The invention relates to a method for preparing cyclic carbonate by cycloaddition of epoxy compound and carbon dioxide. Background technique: [0002] The efficient capture and conversion of carbon dioxide has become one of the most challenging issues in this century. As an abundant C1 resource, carbon dioxide can be used to synthesize a variety of high value-added compounds, such as cyclic carbonate, dimethyl carbonate, isocyanate and so on. Among them, cyclic carbonate is a kind of green polar solvent with excellent performance, which is widely used in the synthesis of pharmaceutical and fine chemical intermediates. [0003] The homogeneous catalysts used in the reported methods for producing cyclic carbonates are mainly binary homogeneous catalytic systems composed of Lewis acid metals and Lewis bases, wherein the used Lewis metals such as alkali metal halides, alkaline earth metal halides , transition metal salts, transition metal complexes or t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/38C07D317/36B01J31/06
Inventor 张锁江孙剑成卫国王金泉陈曦张香平
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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