Method for preparing carbonic acid glyceride by catalytic reaction-azeotropic reification coupling

A technology of glycerol carbonate and azeotropic distillation, which is applied in the preparation of organic carbonates and organic chemistry, can solve the problems of complicated treatment process, large amount of dimethyl carbonate, and poisonous carbon monoxide, so as to achieve simple purification process and save use quantity, beneficial to the effect of recycling

Inactive Publication Date: 2010-06-02
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of these methods of using carbon monoxide to synthesize glycerol carbonate are that carbon monoxide is poisonous, and the reaction time is long, the reaction temperature is high, the reaction pressure is high, and the requirements for equipment are high.
However, there are many shortcomings in the current production method: 1. In terms of catalyst selection, the activity of immobilized enzymes is low and the price is expe

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Take 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 10.65 g of ethyl acetate and 0.224 g of calcium oxide and add them to the reaction kettle at the bottom of the tower, heat the bottom of the tower while stirring, and open the condenser at the top of the tower. When the temperature of the tower bottom is 67°C and the top of the tower is 58°C, start to extract the overhead distillate under the condition of the reflux ratio of 4, react for 1 hour, the temperature of the bottom of the tower reaches 91°C, and the temperature of the top of the tower reaches 61°C. React, stop heating, turn off condensed water. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, evaporate and remove the constant boiling agent in a vacuum, and obtain the glycerol carbonate product, the yield of glycerol carbonate is 86.5%, and the concentration of glycerol carbonate in the product is 85.0%.

Embodiment 2

[0028] Example 2: Take 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 17.58 g of n-hexane and 0.224 g of calcium hydroxide and add them to the reaction kettle at the bottom of the tower, heat the tower kettle while stirring, and open the condenser at the top of the tower. When the temperature of the tower bottom is 63°C and the top of the tower is 54°C, start to extract the overhead distillate under the condition of reflux ratio of 4, react for 0.8h, the temperature of the bottom of the tower reaches 90°C, and the temperature of the top of the tower reaches 56°C, at this time End the reaction, stop heating, turn off the condensed water. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, and evaporate the constant boiling agent in a vacuum to obtain a glycerol carbonate product with a glycerol carbonate yield of 92.5% and a glycerol carbonate concentration of 90.0% in the product.

Embodiment 3

[0029]Embodiment 3: Get 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 10.02g of dichloroethane and 0.112g of calcium oxide and join in the reaction kettle at the bottom of the tower, heat the tower kettle, stir simultaneously, open the condenser at the top of the tower, when the tower When the temperature of the still was 65°C and the top of the tower was 60°C, the overhead distillate was extracted under the condition of a reflux ratio of 4. After 0.5h of reaction, the temperature of the bottom of the tower reached 100°C and the temperature of the top of the tower reached 66°C. At this point, the reaction was terminated, the heating was stopped, and the condensed water was turned off. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, evaporate and remove the constant boiling agent in vacuo, and obtain the glycerol carbonate product, the yield of glycerol carbonate is 97.2%, and the concentration ...

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Abstract

The invention discloses a method for preparing carbonic acid glyceride by catalytic reaction-azeotropic reification coupling, and belongs to the technical field of fine chemistry. In the method, the catalytic reaction and the azeotropic rectification are finished in the same rectification tower; glycerol, dimethyl carbonate, a solid base catalyst and an azeotropic agent are added into a tower; the tower is heated while the raw materials are stirred; the tower operation temperature is between 60 and 120 DEG C; the tower top operation temperature is between 50 and 80 DEG C; a mixture of methanol and the azeotropic agent is taken out of the top of the tower in a reflux ratio of 2 to 6; the reaction time is 0.1 to 3 hours; the operational pressure of the top of the rectification tower is the normal pressure; the mol ratio of the dimethyl carbonate to the glycerol is 1-1.5:1; the reaction products in the tower are subjected to vacuum evaporation to remove the azeotropic agent and filtered to remove the catalyst; and finally the carbonic acid glyceride is obtained. The solid base catalyst in the method has the advantages of low in price, convenient recovery, and cyclically used. Due to the lower mol ratio of the methyl carbonate to the glycerol, the consumption of the methyl carbonate is lowered. The process for purifying the carbonic acid glycerol products is simple.

Description

technical field [0001] The invention relates to a method for preparing glycerol carbonate by glycerin and dimethyl carbonate, in particular to a method for preparing glycerol carbonate by coupling catalytic reaction-azeotropic distillation. Background technique [0002] Glycerol carbonate is a new type of important chemical product, which is a cyclic carbonate. Glycerol carbonate has a wide range of uses and a large market demand. It can be used as a solvent in the production of emulsifiers, paint removers, paints and cosmetics. Glycerol carbonate and its derivatives can also be used in the electrolyte of fuel cells, and can also be used as liquid membranes for the separation of carbon dioxide and nitrogen. Due to its active nature, glycerol carbonate can be used as an intermediate in the production of chemical products, for example, it can be used to produce glycidyl ether, and it can also be used to produce glycosides, cross-linked polymers, pharmaceutical intermediates, ...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
Inventor 李加波王涛郭强
Owner TSINGHUA UNIV
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