Ionic liquid solid acid synthesized by using cycloheximide and heteropoly acid radical and preparation method thereof

A technology of cyclohexyl imine and ionic liquid, which is applied in the field of preparation of ionic liquid-type solid acid, can solve the problems of difficult separation, high production cost, and large amount of catalyst, and achieve the problems of easy dissolution, high catalytic activity, and cost reduction Effect

Inactive Publication Date: 2012-06-27
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently developed SO3H-functionalized imidazole-based acidic ionic liquid is widely used in reactions such as esterification and alkylation, and has high catalytic activity, but the price of imidazole is relatively expensive , the production cost is higher, the amount of catalyst is larger, and the separation is more difficult

Method used

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  • Ionic liquid solid acid synthesized by using cycloheximide and heteropoly acid radical and preparation method thereof
  • Ionic liquid solid acid synthesized by using cycloheximide and heteropoly acid radical and preparation method thereof
  • Ionic liquid solid acid synthesized by using cycloheximide and heteropoly acid radical and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Dissolve 12.215g of 1,3-propane sultone in 100ml of toluene, add 9.915g of cyclohexyl imine dropwise under ice bath and vigorous stirring, and its 1,3-propane sultone and cyclohexyl imine The molar ratio is 1:1. After dropping, react at 30°C, 70°C, and 100°C for 8 hours. The reactant is filtered, and the filter cake is washed with ethyl acetate and ether three times in turn, and dried at 100°C to obtain The masses of the white ionic liquid precursor 1-(propyl-3-sulfonic acid) cycloheximide inner salt (HMI-PS) were 18.60g, 21.47g, and 20.91g, respectively.

[0028] Step 2: Dissolve 6.639g HMI-PS in water, and add 28.80g aqueous solution of dodecatungstophosphoric acid with a molar ratio of 1:3 dropwise at room temperature under electric stirring. After dropping, react at room temperature for 40h. The water was distilled off under reduced pressure at ℃, and the obtained solid was dried at 100 ℃ to obtain a gray-brown ionic liquid-type solid acid 1-(propyl-3-sulfon...

Embodiment 2

[0030] Dissolve 12.215g of 1,3-propane sultone in 150ml of toluene, add 14.873g of cyclohexyl imine dropwise under ice bath and strong stirring, the molar ratio of 1,3-propane sultone to cyclohexyl imine The ratio is 1:1.5, after dropping, react at 30°C, 70°C, and 100°C for 8 hours, the reactant is filtered, the filter cake is washed with ethyl acetate and ether three times in turn, and dried at 100°C to obtain a white ionic liquid The masses of the precursor 1-(propyl-3-sulfonic acid) cycloheximide internal salt (HMI-PS) were 18.80g, 21.77g, and 20.97g, respectively.

[0031] Dissolve 6.639g of HMI-PS in water, and add 57.60g of dodecatungstophosphoric acid aqueous solution with a molar ratio of 1:6 dropwise at room temperature under electric stirring. The water was removed by pressure distillation, and the resulting solid was dried at 100°C to obtain a gray-brown ionic liquid-type solid acid 1-(propyl-3-sulfonic acid)cyclohexylimide dodecatungstophosphate ([HMIPS] 3 PW 12 ...

Embodiment 3

[0033] Step 1: Dissolve 12.215g of 1,3-propane sultone in 100ml of toluene, add 9.915g of equimolar cycloheximide dropwise under ice bath and strong stirring, and react at 70°C for 2h respectively. After 8h and 15h, the reactant was filtered, the filter cake was washed three times with ethyl acetate and diethyl ether in turn, and dried at 100°C to obtain the white ionic liquid precursor HMI-PS with the masses of 16.32g, 21.47g, and 21.55g, respectively. .

[0034] The second step: the same as the second step of Example 1.

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Abstract

The invention relates to an ionic liquid solid acid synthesized by using cycloheximide and a heteropoly acid radical and a preparation method thereof, relating to the technical field of ionic liquids. The solid acid is shown as a chemical structural general formula in the specifications, wherein n=3 or 4; and M is W (wolfram) or Mo (molybdenum). The ionic liquid solid acid is generated by taking cycloheximide as a cation main body, introducing a sulfonic functional group by undergoing a quaternary amination reaction, and reacting with Keggin heteropoly acid. The ionic liquid solid acid is prepared with a simple preparation method, has very high Bronsted acidity, and has high catalytic activity on an acid catalysis esterification reaction; and most synthesized ionic liquid solid acids can be dissolved into most acids or alcohols, but are insoluble in most esters, so that the ionic liquid solid acid serves as a reaction control self-separating catalyst in a catalytic esterification reaction, and esters are separated from the catalyst by easily filtering.

Description

technical field [0001] The present invention relates to a kind of ionic liquid type solid acid and preparation method thereof, especially a kind of Keggin (with H 3 PW 12 o 40 ·5H 2 O structure) type heteropolyacid group is the preparation method of the ionic liquid type solid acid of anion. Background technique [0002] The traditional production process of esterification is alkyd esterification using concentrated sulfuric acid as a catalyst, which has problems such as polluting the environment and corroding equipment. It is of great significance to develop environmentally friendly and efficient esterification catalysts to replace traditional catalysts. Ionic liquids are a new class of solvents. Compared with traditional solvents, ionic liquids have a series of advantages such as wide liquid range, good chemical and thermal stability, and low vapor pressure. Ionic liquids are generally composed of a large organic cation and a relatively small inorganic or organic ani...

Claims

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Application Information

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IPC IPC(8): C07D295/088B01J31/18C07C67/08C07C69/14C07C69/704
Inventor 李工王树立徐恒于永涛
Owner CHANGZHOU UNIV
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