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

A technology of ionic liquids and quaternary ammonium salts, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, etc., to achieve the effects of high activity, high product selectivity and yield, and low price

Inactive Publication Date: 2013-02-27
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 1 mol of triethylamine in a four-necked flask, add 1 mol of n-bromobutane into a constant pressure titration funnel, add 250 mL of refined ethanol as a solvent, and set the temperature at 83 °C under N 2 Under protective conditions, the reaction was refluxed for 24 h. Under high vacuum, the obtained mixture was rotatably evaporated to remove solvent and unreacted raw materials, and white crystals were precipitated, filtered, and vacuum-dried for 48 h to obtain butyl bromide triethyl quaternary ammonium salt crystals [N 2224 ] Br. Weigh 0.025 mol[N 2224 ]Br was dissolved in 30 mL of distilled water, and 2.5 g of concentrated sulfuric acid was weighed to make a dilute solution. The two solutions were mixed, stirred, and 2.9 g of Ag were added in batches. 2 O (0.0125 mol), react in the dark for 6 h, remove the AgBr precipitate by filtration, and dry under vacuum at 70 °C. A colorless transparent liquid [N 2224 ] HSO 4- .

[0017] Weigh the above-prepared [N 222...

Embodiment 2

[0020] [N 2224 ] HSO 4- Synthesis as in Example 1. Weigh the above-prepared [N 2224 ] HSO 4- Catalyst 0.01 mol, glycerin 1.0 mol, stirred and heated up to 350 °C for batch reaction, fully reacted until no distillate was produced, then sampled for gas chromatographic analysis. The analysis shows that the conversion rate of glycerol is 100%, and the yield of acrolein is 49.6%.

Embodiment 3

[0022] [N 2224 ] HSO 4- Synthesis as in Example 1. Weigh the above-prepared [N 2224 ] HSO 4- Catalyst 0.025 mol, glycerin 1.0 mol, stirred and heated up to 280 °C for batch reaction, fully reacted until no distillate was produced, then sampled for gas chromatographic analysis. The analysis showed that the conversion rate of glycerin was 100%, and the yield of acrolein was 70.3%.

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Abstract

The invention relates to the field of organic chemistry, and particularly relates to a method for preparing acraldehyde from liquid-phase dehydration of glycerin catalyzed by quaternary ammonium salt ionic liquid. In the method, the quaternary ammonium salt ionic liquid is used as a catalyst; a semi-batch reaction technology is employed; a reaction temperature is 280-350 DEG C; the molar ratio of the ionic liquid to glycerin is 1.0 : 100-2.5 : 100; acraldehyde is prepared from the liquid-phase dehydration of glycerin; the conversion rate of glycerin is 100%; and the yield of the product acraldehyde is 37.8-70.3%. High added-value acraldehyde is prepared by using biomass glycerin. The raw materials are low in cost and wide in resources. The acidity of the catalyst is adjustable; and the catalyst has high catalytic activity. The method has the characteristics of fast reaction rate and high selectivity. The product system is simple in separation; the process is safe and environment-friendly, and can realize industrialized 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陆秀凤高军
Owner JIANGSU UNIV
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