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Method for synthesizing glycerol carbonate from glycerol

A technology of glycerol carbonate and glycerin, which is applied in the field of synthesis of glycerol carbonate, can solve the problems of complex process, environmental pollution, high cost, etc., and achieve the effect of simple process, easy separation and purification, and less impurities

Inactive Publication Date: 2013-03-06
PANJIN KELONG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems of high cost, complicated process and easy environmental pollution in the prior art for producing glycerol carbonate, the present invention proposes a method for preparing glycerol carbonate with glycerin and urea as raw materials and Lewis acid salt as catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take 92g of 1mol glycerin, 60g of 1mol urea, and 1.8g of catalyst sodium sulfate, put them into a four-necked bottle equipped with a condenser, agitator, thermometer, and node thermometer, first heat to 100°C to melt the materials, and the vacuum degree is 0.3KPa. Under high-speed stirring, the reaction was carried out for 5 hours at a reaction temperature of 120° C., and 122 g of crude glycerol carbonate was collected. A small amount of glycerin was removed from the crude glycerol carbonate by distillation under reduced pressure to obtain 112 g of glycerol carbonate. The glycerol carbonate yield is 73%, and the gas chromatogram results show that the glycerol carbonate purity is 95%.

Embodiment 2

[0014] Take 92g of 1mol of glycerin, 60g of 1mol of urea, and 1.8g of catalyst sodium sulfate, put them into a four-neck bottle equipped with a condenser, agitator, thermometer, and node thermometer, first heat to 100°C to melt the materials, and the vacuum degree is 0.3KPa. Under high-speed stirring, the reaction was carried out for 5 hours at a reaction temperature of 140° C., and 125 g of crude glycerol carbonate was collected. A small amount of glycerol was removed from the crude glycerol carbonate by distillation under reduced pressure to obtain 116 g of glycerol carbonate. The glycerol carbonate yield is 76%, and the gas chromatogram results show that the glycerol carbonate purity is 97%.

Embodiment 3

[0016] Take 92g of 1mol of glycerin, 60g of 1mol of urea, and 1.8g of catalyst sodium sulfate, put them into a four-neck bottle equipped with a condenser, agitator, thermometer, and node thermometer, first heat to 100°C to melt the materials, and the vacuum degree is 0.3KPa. Under high-speed stirring, the reaction was carried out for 8 hours at a reaction temperature of 140° C., and 126 g of crude glycerol carbonate was collected. A small amount of glycerol was removed from the crude glycerol carbonate by distillation under reduced pressure to obtain 118 g of glycerol carbonate. The glycerol carbonate yield is 77%, and the gas chromatogram results show that the glycerol carbonate purity is 97%.

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Abstract

The invention discloses a method for preparing glycerol carbonate, wherein glycerol and urea are used as raw materials and lewis acid salt is used as a catalyst. The preparation method comprises the following steps of: adding the glycerol, the urea and sodium sulfate into a four-mouth bottle provided with a condensing pipe, a stirrer, a thermometer and a point thermometer; heating to a molten material of 100 DEG C and keeping the vacuum degree at 0.3 KPa; reacting for 5-8 hours at the temperature of 100-180 DEG C under the condition of high-speed stirring; removing a small amount of solid impurity from a product through vacuum filtration to obtain rough glycerol carbonate; removing the glycerol from the rough glycerol carbonate through vacuum distillation to obtain glycerol carbonate with higher purity; and neutralizing and removing ammonia gas produced in the reaction process through a rotary vane oil pump and an absorption bottle filled with diluted phosphoric acid so as to improve the conversion rate of the glycerol. The method has the advantages of capability of improving the conversion rate of the glycerol, non-toxic reaction raw materials, high conversion rate of the glycerol, less impurity, simple process, easiness in subsequent separation and purification and capability of recycling the separated glycerol.

Description

technical field [0001] The invention relates to a method for synthesizing glycerol carbonate, in particular to a method for preparing glycerol carbonate by using glycerol urea as a raw material and Lewis acid salt as a catalyst. Background technique [0002] Glycerol carbonate is an important new chemical product. It is a cyclic carbonate with two important active groups, carbonyl and hydroxyl. Glycerol carbonate can be used as a highly polar solvent or a polymer intermediate. , Esters or acid derivatives undergo transesterification reactions to prepare other cyclic carbonates. Glycerol carbonate can undergo nucleophilic substitution with nucleophiles such as oxygen, nitrogen, and sulfur, and can be used as a raw material for preparing glycidol. It can also be used as a biological solvent, an important component of polyurethane coatings, and in the field of cosmetics. Due to the advantages of low toxicity, non-volatility, biodegradability, and environmental friendliness, g...

Claims

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Application Information

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IPC IPC(8): C07D317/36
Inventor 尹晓东秦立翠季春伟
Owner PANJIN KELONG FINE CHEM
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