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Method for preparing glycerin shrinkage benzaldehyde

A technology of benzaldehyde and glycerin, applied in the direction of organic chemistry, can solve the problems of strong corrosion of equipment, low active point density, long reaction time, etc., and achieve the effect of low corrosion of equipment, high conversion rate of glycerin and stable catalytic performance

Inactive Publication Date: 2012-10-03
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because these systems have many side reactions, strong corrosion to equipment, low product purity, complicated post-reaction treatment, and a large amount of acid waste residue and waste liquid produced have brought serious damage to the environment and caused secondary pollution, their use has been greatly restricted.
Although some solid acid catalysts developed later, such as heteropoly acid, niobic acid, molecular sieve, etc., overcome the above-mentioned shortcomings and simplify the post-treatment process, the active point density of the solid heterogeneous catalyst is low, and the relative activity is low. Easy to inactivate, generally requires longer reaction time and higher temperature, and tends to produce more by-products

Method used

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  • Method for preparing glycerin shrinkage benzaldehyde

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Experimental program
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Effect test

Embodiment 1

[0032] Add 2.33g (10mmol) bisulfate N-butylpyridine ([BPy]HSO) successively in reactor 4 ) ionic liquid and 27.6g (0.3mol) glycerol, stir and mix; then add 10.6g (0.1mol) benzaldehyde to the reaction kettle in sequence, heat slowly under stirring, and raise the temperature to 70°C to make the nucleophilic addition reaction proceed 120 minutes; Wherein, the mol ratio of glycerol and benzaldehyde is 3:1. After the reaction is over, the reaction kettle is left to stand, and the system is automatically divided into upper and lower layers. The upper layer is a mixture phase of reactants and products, and the lower layer is an ionic liquid and unreacted glycerin phase. Directly separate the upper oil phase for qualitative and quantitative NMR detection, and use CH for the lower layer 2 Cl 2Glycerin and ionic liquid are extracted and separated, and the ionic liquid can be recovered and reused by removing the organic solvent under reduced pressure. The oil phase was quantified wit...

Embodiment 2

[0034] In reactor, add 6.32g (20mmol) bisulfate radical 1-methyl-3-butylsulfonic acid base imidazoles ([BSMim]HSO) successively 4 ) ionic liquid and 13.8g (0.15mol) glycerol, stir and mix; then add 10.6g (0.1mol) benzaldehyde to the reaction kettle in turn, heat slowly under stirring, and raise the temperature to 25°C to allow the nucleophilic addition reaction to proceed 180 minutes; Wherein, the mol ratio of glycerol and benzaldehyde is 1.5:1. After the reaction is over, the reaction kettle is left to stand, and the system is automatically divided into upper and lower layers. The upper layer is a mixture phase of reactants and products, and the lower layer is an ionic liquid and unreacted glycerin phase. Directly separate the upper oil phase, conduct qualitative and quantitative NMR detection, and use CH 2 Cl 2 Glycerin and ionic liquid are extracted and separated, and the ionic liquid can be recovered and reused by removing the organic solvent under reduced pressure. Th...

Embodiment 3

[0036] Add 1.84g (5mmol) trifluoromethanesulfonate radical 1-methyl-3-butylsulfonate imidazole ([BSMim]CF) successively in the reactor 3 SO 3 ) ionic liquid and 46.045g (0.5mol) glycerol, stir and mix; then add 10.6g (0.1mol) benzaldehyde to the reaction kettle in turn, heat slowly under stirring, and raise the temperature to 50°C to make the nucleophilic addition reaction proceed 5 minutes; Wherein, the mol ratio of glycerol and benzaldehyde is 5:1. After the reaction is over, the reaction kettle is left to stand, and the system is automatically divided into upper and lower layers. The upper layer is a mixture phase of reactants and products, and the lower layer is an ionic liquid and unreacted glycerin phase. Directly separate the upper oil phase, conduct qualitative and quantitative NMR detection, and use CH 2 Cl 2 Glycerin and ionic liquid are extracted and separated, and the ionic liquid can be recovered and reused by removing the organic solvent under reduced pressur...

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Abstract

The invention discloses a method for preparing glycerin shrinkage benzaldehyde. The method comprises adding glycerin and benzaldehyde into ionic liquid serving as reaction media and catalysts to perform nucleophilic addition reaction, wherein anode ions and cathode ions of the ionic liquid at least contain one acid group. The method has the advantages of being environment-friendly, low in corrosion to devices, capable of effectively improving yield of the glycerin shrinkage benzaldehyde and the like. In addition, the catalysts can be repeatedly used.

Description

technical field [0001] The invention relates to the technical field of glycerin acetal (ketone), in particular to a method for preparing glycerin benzal. Background technique [0002] Vigorously developing biodiesel has important strategic significance for sustainable economic development, promoting energy substitution, reducing environmental pressure, controlling urban air pollution, and ensuring national energy security. However, the current method for producing biodiesel is mainly to transesterify animal and vegetable oils with low molecular weight alcohols (such as methanol, ethanol, etc.). As shown in Formula 1 below, Formula 1 is the reaction equation for preparing biodiesel in the prior art. This reaction process will co-produce a large amount of low-quality glycerol, about 1 ton of glycerol is produced for every 10 tons of biodiesel produced. [0003] Formula 1 [0004] With the increasing shortage of petroleum resources, countries around the world will continue...

Claims

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Application Information

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IPC IPC(8): C07D319/06
Inventor 王波
Owner BEIJING FORESTRY UNIVERSITY
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