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Sulfonated cellulose-based ionic liquid catalysts and preparation method thereof

A liquid catalyst and cellulose technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., to achieve mild reaction conditions, which are conducive to large-scale production and preparation processes simple effect

Inactive Publication Date: 2020-03-06
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the defects existing in the existing ionic liquid catalyst, the object of the present invention is to provide a kind of sulfonated cellulose-based ionic liquid and preparation method thereof

Method used

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  • Sulfonated cellulose-based ionic liquid catalysts and preparation method thereof
  • Sulfonated cellulose-based ionic liquid catalysts and preparation method thereof
  • Sulfonated cellulose-based ionic liquid catalysts and preparation method thereof

Examples

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Effect test

Embodiment 1

[0027] [PCM-pmim-HSO 3] Preparation of [P-TSA]: put dry 5g porous cellulose microspheres into 5mL epichlorohydrin and 10mL 3mol / L sodium hydroxide solution, shake the table at 25°C, react for 8h, and the microspheres Repeated washing and suction filtration until the pH of the filtrate is neutral, disperse 5g of microspheres and 5g of imidazole in DMF solvent in an oil bath at 80°C, react for 8h, add to toluene containing 1,3-propane sultone after repeated washing and suction filtration Oil bath in the solution at 50°C, react for 5h, wash and filter to obtain sulfonated cellulose-based ionic liquid intermediate [PCM-pmim-HSO 3 ]; Weigh 1g of sulfonated cellulose-based ionic liquid intermediate [PCM-pmim-HSO 3 ], dispersed in 3mL water, added dropwise 1mL 0.01mol / mL p-toluenesulfonic acid aqueous solution, slowly warmed up to 90°C, and reacted for 5h to obtain [PCM-pmim-HSO 3 ][P-TSA].

Embodiment 2

[0029] [PCM-pmim-HSO 3 ][CH 3 SO 3 ] preparation: put dry 5g porous cellulose microspheres into 6mL epichlorohydrin and 15mL 3mol / L sodium hydroxide solution, shake the table at 25°C, react for 5h, and wash the microspheres repeatedly to The pH of the filtrate is neutral, disperse 5g microspheres and 3g imidazole in DMF solvent, oil bath 70°C, react for 6h, wash and filter repeatedly, add to toluene solution containing 1,3-propane sultone, oil bath 50°C , reacted for 4h, and obtained the sulfonated cellulose-based ionic liquid intermediate [PCM-pmim-HSO 3 ]; Weigh 1g of sulfonated cellulose-based ionic liquid intermediate [PCM-pmim-HSO 3 ], dispersed in 5mL water, added dropwise 1mL 0.01mol / mL methanesulfonic acid aqueous solution, slowly raised to 90°C, and reacted for 5h to obtain [PCM-pmim-HSO 3 ][CH 3 SO 3 ].

Embodiment 3

[0031] [PCM-pmim-HSO 3 ][HSO 4 ] preparation: put dry 5g porous cellulose microspheres into 8mL epichlorohydrin and 16mL 3mol / L sodium hydroxide solution, shake the table at 25°C, react for 7h, and wash and suction filter the microspheres repeatedly until the end of the reaction. The pH of the filtrate is neutral, disperse 5g of microspheres and 10g of imidazole in DMF solvent, oil bath 75°C, react for 7h, wash and filter repeatedly, add to toluene solution containing 1,3-propane sultone, oil bath 40°C , reacted for 5h, washed and filtered to obtain the sulfonated cellulose-based ionic liquid intermediate [PCM-pmim-HSO 3 ]; Weigh 1 g of sulfonated cellulose-based ionic liquid cation [PCM-pmim-HSO 3 ], dispersed in 4mL aqueous solution, added dropwise 0.25mL sulfuric acid, slowly warmed up to 50°C, and reacted for 5h to obtain [PCM-pmim-HSO 3 ][HSO 4 ].

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Abstract

The invention relates to sulfonated cellulose-based ionic liquid catalysts and a preparation method thereof and belongs to the technical field of solid catalysts. By adopting the method, solubility ofan ionic liquid upon cellulose is overcome, and the cellulose is adopted as a matrix for synthesizing the ionic liquid. The preparation method comprises the following steps: by taking porous cellulose microspheres as a matrix, grafting imidazole and sulfonic acid groups to the cellulose microspheres by means of chemical grafting, and further bonding acidic anions by using intermolecular ionic bonds, so as to obtain a series of sulfonated cellulose-based ionic liquid catalysts. The prepared sulfonated cellulose-based ionic liquid catalysts have both biocompatibility of cellulose and high catalysis activity of ionic liquids, in addition, are low in production cost, wide in raw material source, easy to separate and high in repeated use time, and can be widely applied to various catalysis fields.

Description

technical field [0001] The invention relates to a sulfonated cellulose-based ionic liquid catalyst and a preparation method thereof, belonging to the technical field of solid catalysts. Background technique [0002] Ionic liquids are compounds composed of organic cations and organic or inorganic anions. Both the anions and cations are modifiable, and can be used as efficient catalysts in organic or inorganic reactions by introducing active groups. Despite the many advantages of ionic liquids, their widespread utilization is still limited by some disadvantages, such as high cost, high consumption, and difficult product separation. Besides, the high viscosity of ionic liquids not only limits their mass transfer during reactions but also makes their handling difficult. In order to solve these problems, immobilized ionic liquids have gradually received extensive attention. Immobilization of ionic liquids is to immobilize ionic liquids on carrier materials (such as: silica, mag...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/18B01J35/10
CPCB01J31/06B01J31/0295B01J31/0298B01J27/188B01J27/19B01J35/60
Inventor 付玉杰王希清刘天舒付浩然赵春健赵修华李妍妍姚丽萍朱亚伟沈忱
Owner NORTHEAST FORESTRY UNIVERSITY
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