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

An ionic liquid, a technology for catalyzing glycerol, which is applied in the field of organic chemistry to achieve the effects of high activity, high product selectivity and yield, and low price

Inactive Publication Date: 2013-02-20
JIANGSU UNIV
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  • 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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  • Method for preparing acrolein through catalysis of glycerol liquid phase dehydration by using pyridine ion liquid

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Experimental program
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Effect test

Embodiment 1

[0017] Take 0.1 mol of pyridine in a four-neck flask, add equimolar n-bromobutane into a constant pressure titration funnel, 2 Stirred under protective conditions for 12 h, the product was washed with ethyl acetate and then vacuum-dried for 8 h to obtain 0.1 mol of brominated n-butylpyridine [Bpy]Br as light yellow viscous oily liquid. At 90 °C, equimolar concentrated sulfuric acid was added dropwise to [BPy]Br, stirred for 6 h, the product was washed with ether and then dried in vacuum to obtain the ionic liquid [BPy]HSO 4 .

[0018] Weigh the [BPy]HSO prepared above 4 Catalyst 5 mmol, glycerin 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 32.5%.

Embodiment 2

[0020] [BPy]HSO 4 Synthesis as in Example 1. Weigh the [BPy]HSO prepared above 4 Catalyst 5 mmol, glycerin 1.0 mol, stirred and heated up to 300 °C for batch reaction, fully reacted until no distillate was produced, and samples were taken for gas chromatographic analysis. The analysis shows that the conversion rate of glycerol is 100%, and the yield of acrolein is 48.1%.

Embodiment 3

[0022] [BPy]HSO 4 Synthesis as in Example 1. Weigh the [BPy]HSO prepared above 4 Catalyst 0.012 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 chromatography analysis. Analysis showed that the conversion rate of glycerol was 100%, and the yield of acrolein was 50.3%.

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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 a pyridine ion liquid. According to the method, a pyridine ion liquid is adopted, 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 0.5:100-1.2:100 to prepare the acrolein, wherein a glycerol conversion rate is 100%, and an acrolein yield is 32.0-67.9%. 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/22C07C45/52
Inventor 沈灵沁殷恒波颜晓波张长华柳艳君
Owner JIANGSU UNIV
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