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A kind of resin supported anionic acidic ionic liquid catalyst and application thereof

A technology of acidic ionic liquid and catalyst, which is applied in the application field of preparing polyoxymethylene dialkyl ether, can solve the problems of cumbersome preparation process and special raw material structure, and achieve the effect of wide sources, low cost and good activity

Active Publication Date: 2018-09-25
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of special raw material structure and tedious preparation process in existing polymer-loaded ionic liquids, and provide a resin-loaded anion acidic ionic liquid catalyst with simple preparation process, high activity, and convenient separation and recovery. , and provide the preparation method of this catalyst

Method used

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  • A kind of resin supported anionic acidic ionic liquid catalyst and application thereof
  • A kind of resin supported anionic acidic ionic liquid catalyst and application thereof
  • A kind of resin supported anionic acidic ionic liquid catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Disperse 50g of strongly acidic cation exchange resin Purolite CT175 in 250mL of toluene, add 37g of zwitterionic compounds, and react at 80°C for 24 hours; filter after the reaction, and then extract the filter cake with dichloromethane at 40°C for 24 hours, and then vacuum-dried at 70° C. for 12 hours to obtain the resin-supported anion acidic ionic liquid catalyst Cat-1.

Embodiment 2~13

[0035] The preparation steps and methods of Examples 2 to 13 are the same as in Example 1, except that the types of strongly acidic cation exchange resins and zwitterionic compounds are changed. The specific preparation conditions are shown in Table 1.

[0036] Table 1

[0037] Example

Embodiment 14

[0039] Take 0.3g of the catalyst Cat-1 synthesized in Example 1 and put it into a three-neck flask, then add 2.7g (0.03mol) of paraformaldehyde and 4.7g (0.045mol) of styrene, replace it with nitrogen for 3 times, and then stir the reaction at 80°C 10 hours. After the reaction, the organic phase was concentrated, and chromatographically separated on a silica gel column to obtain 4-phenyl-1,3-dioxane with a yield of 86%. The catalyst was separated by centrifugation, and the reaction of paraformaldehyde and styrene was catalyzed according to the same steps as above, and the product yield was 86% after repeating the first time. Repeat the second product yield 85%.

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Abstract

The invention discloses a resin-supported anionic acidic ionic liquid catalyst which is prepared through the following steps: strongly acidic cation exchange resin is dispersed in toluene; a zwitterionic compound is added, and a reaction is conducted at a temperature of 80-100 DEG C for 12-24h; filtering is carried out after the reaction is completed; a filter cake is extracted with dichloromethane under a temperature of 40-50 DEG C; and vacuum drying is carried out for 12-24h under a temperature of 60-80 DEG C. According to the invention, the strongly acidic cation exchange resin with sulfonic acid group is adopted as counter anion for preparing the supported anionic acidic ionic liquid. The preparation process is simple and feasible. After a reaction, the ionic liquid can be recycled after filtration or centrifugation, such that reaction cost is reduced. The method is an effective method for realizing ionic liquid supporting. The invention also discloses applications of the catalyst in Prins condensation reactions, acetal (ketal) reactions and reactions for preparing polyoxymethylene dialkyl ether. With the catalyst, a catalytic effect is good, catalyst dose is low, and catalyst recovery is convenient.

Description

technical field [0001] The invention relates to a resin-supported anionic acidic ionic liquid catalyst and its application, in particular to the application of the catalyst in Prins condensation reaction, acetal (ketone) reaction and reaction for preparing polyoxymethylene dialkyl ether. Background technique [0002] Ionic liquids are composed of anions and cations, and have strong designability, and can meet the needs of practical work through the functional design of anions or cations. The acid-functionalized ionic liquid obtained by introducing strong acidic groups with catalytic properties into the cationic structure of the ionic liquid has the characteristics of stronger acidity than ordinary protonic acids, low corrosion, good stability, and easy separation and circulation. It has been widely studied, and a large number of experiments have proved that acid-functionalized ionic liquid catalysts have good activity and higher selectivity. However, due to the relatively e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10C07C33/32C07C33/025C07C29/38C07D317/20C07C43/30C07C41/56
Inventor 夏春谷李臻许传芝孟雅莉
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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