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Method for preparing acrolein through catalysis of glycerol liquid phase dehydration by using imidazole ion liquid

A technology of ionic liquid and catalyzed glycerol, which is applied in the field of organic chemistry to achieve the effects of avoiding side reactions, high activity, and low equipment corrosion

Inactive Publication Date: 2013-02-20
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

How to prolong the life of the catalyst, make the acidity of the catalyst controllable, and avoid the generation of side reactions has not been reported in the patent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 0.1 mol N-methylimidazole in a four-neck flask, add equimolar n-butane bromide into a constant pressure titration funnel, 2 Stirred under protected conditions for 12 h, the product was washed with ethyl acetate and then vacuum-dried for 8 h to obtain 0.1 mol 1-butyl-3-methylimidazolium bromide [Bmim]Br as a light yellow viscous oily liquid. Under ice-water bath conditions, equimolar concentrated sulfuric acid was added dropwise to [Bmim]Br, stirred for 20 h, and the product was washed with ether and then vacuum-dried to obtain the ionic liquid [Bmim]HSO 4 .

[0017] Weigh the [Bmim]HSO prepared above 4 Catalyst 1 mmol, glycerin 1.0 mol, stirred and heated up to 250 °C for batch reaction, fully reacted until no distillate was produced, and samples were taken for gas chromatographic analysis. Analysis showed that the conversion rate of glycerin was 100%, and the yield of acrolein was 30.5%.

Embodiment 2

[0019] [Bmim] HSO 4 Synthesis as in Example 1. Weigh the [Bmim]HSO prepared above 4 Catalyst 1 mmol, glycerin 1.0 mol, stirred and heated up to 350 °C for batch reaction, fully reacted until no distillate was produced, and samples were taken for gas chromatography analysis. The analysis shows that the conversion rate of glycerin is 100%, and the yield of acrolein is 45.1%.

Embodiment 3

[0021] [Bmim] HSO 4 Synthesis as in Example 1. Weigh the [Bmim]HSO prepared above 4 Catalyst 0.015 mol, glycerol 1.0 mol, stirred and heated up to 250 °C for batch reaction, fully reacted until no distillate was produced, then sampled for gas chromatographic analysis. Analysis showed that the conversion rate of glycerol was 100%, and the yield of acrolein was 32.3%.

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Abstract

The present invention relates to the field of organic chemistry, particularly to a method for preparing acrolein through catalysis of glycerol liquid phase dehydration by using an imidazole ion liquid. According to the method, an imidazole ion liquid is adopted as a catalyst, a semi-batch reaction is adopted, and glycerol liquid phase dehydration is performed at a reaction temperature of 250-350 DEG C and a molar ratio of the ion liquid to the glycerol of 0.1:100-1.5:100 to prepare the acrolein, wherein a glycerol conversion rate is 100%, and an acrolein yield is 30.5-68.2%. According to the present invention, the biomass glycerol is adopted to prepare the high added value acrolein, raw material cost is low, raw material sources are wide, acidity of the catalyst can be adjusted, catalytic activity is high, and the process has characteristics of fast reaction, high selectivity, simple product system separation, safe and environmental protection process, and industrial production.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing acrolein by catalyzing glycerin liquid-phase dehydration with ionic liquid. Background technique [0002] Acrolein is a simple unsaturated aldehyde with high chemical activity and is prone to polymerization and oxidation reactions. It is an important fine chemical intermediate and has a wide range of applications in coatings, papermaking, oil fields, and organic synthesis industries. application. The chemical properties of acrolein are unstable, and the synthesis process is complicated. At present, the synthesis methods of acrolein are mainly divided into three categories: condensation method (formaldehyde acetaldehyde gas phase condensation method, aldol condensation method), oxidation method (propylene oxidation method, propane oxidation method and allyl alcohol oxidation method) and decomposition method ( propylene ether pyrolysis). With the depletion...

Claims

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Application Information

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IPC IPC(8): C07C47/22C07C45/52
Inventor 沈灵沁殷恒波颜晓波张长华姜逸倩葛超群
Owner JIANGSU UNIV
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