Imidazole grafting-type ionic liquid catalyst and preparation method and application

A technology of ionic liquid and catalyst, which is applied in the field of imidazole-based grafted ionic liquid catalyst and its preparation, can solve the problems of low catalytic activity and selectivity, harsh reaction conditions, etc., achieve good catalytic effect, mild reaction conditions, and easy repeated use Effect

Inactive Publication Date: 2010-09-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
0 Cites 35 Cited by

AI-Extracted Technical Summary

Problems solved by technology

At present, the heterogeneous catalysts used in cycloaddition reactions mainly include metal oxides, supported metal complexe...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Abstract

The invention relates to an imidazole grafting-type ionic liquid catalyst, which is hydroxide of 1-propyl (triethoxysilyl)-3-methylimidazole grafted on a carrier. The representation formula of the imidazole grafting-type ionic liquid catalyst is [Smim]OH/X and a mass grafting amount of ionic liquid is between 5 and 25 percent, wherein Smim represents 1-propyl (triethoxysilyl)-3-methylimidazole; and X represents the meso-porous carrier. The imidazole grafting-type ionic liquid catalyst has the advantages of good catalytic effect, high conversion rate of propylene oxide, 100 percent of selectivity of propene carbonate, mild reaction condition and capability of being recycled better.

Application Domain

Technology Topic

GraftingPropylene oxide +7

Examples

  • Experimental program(9)

Example Embodiment

[0016] Example 1:
[0017] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 80mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained [Smim]Cl and 1mol potassium hydroxide to 80mL of anhydrous dichloromethane, stir vigorously for 10h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 70℃ for 10h . Add the obtained 2.3g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 50mL of anhydrous toluene, stir and reflux for 12h, extract with dichloromethane for 10h, and vacuum dry at 70℃ for 10h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH/SiO 2 , The mass grafting amount of ionic liquid is 5%. The grafted ionic liquid catalyst of propylene oxide and imidazole was added to the 80mL reactor at a molar ratio of 1:1.8, and then filled with 2MPa CO 2. Under stirring conditions, the temperature was raised to 120°C, and the reaction was conducted for 8 hours. The product was centrifuged to settle, and the supernatant was taken for analysis by gas chromatography. The results are shown in Table 1.

Example Embodiment

[0018] Example 2:
[0019] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 100mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained [Smim]Cl and 1mol potassium hydroxide to 100mL of anhydrous dichloromethane, stir vigorously for 16h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry under vacuum at 90℃ for 16h . Add the obtained 4.6g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 70mL of anhydrous toluene, stir and reflux for 18h, extract with dichloromethane for 16h, and vacuum dry at 90℃ for 16h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH/SiO 2 , The mass grafting amount of ionic liquid is 10.5%. The grafted ionic liquid catalyst of propylene oxide and imidazole was added to the 80mL reactor at a molar ratio of 1:1, and then filled with 2MPa CO 2. Under stirring conditions, the temperature was raised to 120°C, and the reaction was conducted for 8 hours. The product was centrifuged to settle, and the supernatant was taken for analysis by gas chromatography. The results are shown in Table 1.

Example Embodiment

[0020] Example 3:
[0021] Add 1mol of methylimidazole and 1mol of chloropropyltriethoxysilane to 120mL of toluene solvent, stir and reflux until the layers are separated, and remove the lower viscous liquid (1-chloropropyl(triethoxysilyl)-3 -Methylimidazole chloride crude product), washed 3 times with ethyl acetate, and dried in vacuum. Add the obtained substance [Smim]Cl and 1mol potassium hydroxide to 120mL of anhydrous dichloromethane, stir vigorously for 20h at room temperature, filter off the precipitate, remove the solvent by rotary evaporation, wash 3 times with ether, and dry at 110°C under vacuum 20h. Add the obtained 9.1g ionic liquid to a 0.3mol silica gel carrier uniformly dispersed in 90mL of anhydrous toluene, stir and reflux for 20h, extract with dichloromethane for 18h, and vacuum dry at 110℃ for 20h to obtain heterogeneous grafted ions Liquid catalyst [Smim]OH/SiO 2 , The mass grafting amount of ionic liquid is 17%. The grafted ionic liquid catalyst of propylene oxide and imidazole was added to the 80mL reactor at a molar ratio of 1:1.4, and then filled with 2MPa CO 2. Under stirring conditions, the temperature was raised to 120°C, and the reaction was conducted for 8 hours. The product was centrifuged to settle, and the supernatant was taken for analysis by gas chromatography. The results are shown in Table 1.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

no PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Similar technology patents

Synthesis method of aromatic vinyl trifluoromethylthio ether compound

Owner:万博新材料科技(南通)有限公司

Classification and recommendation of technical efficacy words

  • Improve conversion rate
  • Good catalytic effect
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products