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Method for preparing acrolein by catalyzed liquid-phase dehydration of glycerin by quaternary ammonium salt ionic liquid

A technology of ionic liquid and catalyzed glycerin, which is applied in the field of organic chemistry to achieve the effects of energy saving, low equipment corrosion and low price

Inactive Publication Date: 2016-01-20
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 1 mol of triethylamine in a four-necked flask, add 1 mol of bromo n-butane in a constant pressure titration funnel, add 250 mL of refined ethanol as a solvent, at 83 ℃, N 2 Reflux for 24h under protective conditions. Under high vacuum, the obtained mixture was rotary evaporated to remove the solvent and unreacted raw materials, and white crystals separated out, filtered and dried under vacuum for 48 hours to obtain crystals of butyl triethyl quaternary ammonium bromide [N 2224 ] Br. Weigh 0.025mol[N 2224 ]Br was dissolved in 30mL of distilled water, 2.5g of concentrated sulfuric acid was weighed to make a dilute solution, the two solutions were mixed, stirred, and 2.9g of Ag was added in batches 2 O(0.0125mol), react for 6h in the dark, filter to remove AgBr precipitate, and vacuum dry at 70℃. Obtain colorless transparent liquid [N 2224 ]HSO 4- .

[0017] Weigh the prepared [N 2224 ]HSO 4- Catalyst 0.01mol, glycerol 1.0mol, stirred and heated to 280°C, fully reacted, ...

Embodiment 2

[0019] [N 2224 ]HSO 4- The synthesis is as in Example 1. Weigh the prepared [N 2224 ]HSO 4- Catalyst 0.01mol, glycerol 1.0mol, stirring and heating to 350° C. to carry out batch reaction and fully react until no fractions are produced. Take samples for gas chromatography analysis. The analysis shows that the conversion rate of glycerol is 100% and the yield of acrolein is 49.6%.

Embodiment 3

[0021] [N 2224 ]HSO 4- The synthesis is as in Example 1. Weigh the prepared [N 2224 ]HSO 4- Catalyst 0.025mol, glycerol 1.0mol, stirring and heating to 280° C., to perform batch reaction, and fully react until no fraction is produced, take samples for gas chromatography analysis. The analysis showed that the conversion rate of glycerol was 100%, and the yield of acrolein was 70.3%.

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Abstract

The invention relates to the field of organic chemistry, in particular to a method for preparing acrolein by catalyzing the liquid-phase dehydration of glycerin with quaternary ammonium salt ionic liquids. The method uses quaternary ammonium salt ionic liquid as a catalyst, adopts semi-batch reaction technology, and prepares propylene from glycerin liquid phase dehydration at a reaction temperature of 280-350 °C and a molar ratio of ionic liquid to glycerol of 1.0:100-2.5:100. The conversion rate of aldehyde and glycerol was 100%, and the yield of acrolein was 37.8−70.3%. The invention utilizes biomass glycerol to prepare high value-added acrolein, and the raw material cost is low and the sources are extensive. The acidity of the catalyst can be adjusted, and the catalytic activity is high. The process is characterized by fast reaction rate, high selectivity, simple separation of product systems, safe and environmentally friendly process, and can realize 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 Patents(China)
IPC IPC(8): C07C47/22C07C45/52
Inventor 沈灵沁殷恒波颜晓波陆秀凤高军
Owner JIANGSU UNIV