Synthetic method of glycerol carbonate

A technology of glycerol carbonate and synthesis method, which is applied in the direction of carbon dioxide or inorganic carbonate preparation, electrolytic organic production, organic chemistry, etc., can solve the problem of not finding a very satisfactory preparation process, not seeing glycerol carbonate, Synthesize the problems of high production cost to achieve the effect of alleviating the depletion of energy, reducing the extension of the industrial chain, and facilitating operation

Inactive Publication Date: 2012-03-21
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The problem that the above disclosed technologies exist is that they all need to react under corresponding catalysts, the cost of its synthetic production is high, the preparation process is complicated, and it is not easy to operate. Although glycerol carbonate is a very important chemical product, it has not been used in actual industrial production so far. However, a very satisfactory preparation process has not yet been found. So far, there have been no reports on the synthesis of economical and environmentally friendly glycerol carbonate at home and abroad.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] a. Preparation of electrolyte

[0023] After mixing 0.1M (0.0921g) glycerol with 0.1M (0.2572g) tetraethylammonium iodide and 10 mL of analytically pure N,N-dimethylformamide, put the cathode as a copper electrode and the anode In a one-chamber electrolytic cell with graphite rods, in which: glycerol is the substrate, N,N-dimethylformamide is the solvent after drying with 4? grade molecular sieves, tetraethylammonium iodide is the supporting electrolyte, tetraethylammonium Ammonium iodide and glycerol were analytically pure.

[0024] b. Electrolysis

[0025] Under normal pressure, carbon dioxide is passed into the electrolytic cell to saturation, and then at 8.37mA / cm 2 The current density is 25°C, constant current electrolysis is carried out, and the current flow is 193°C.

[0026] c. Esterification

[0027] After the electrochemical reaction is over, transfer the above electrolytic solution into the flask, add 0.3g of anhydrous potassium carbonate and 0.3mL of ana...

Embodiment 2

[0031] a. Preparation of electrolyte

[0032] After mixing 0.1M (0.0921g) glycerol with 0.1M (0.2572g) tetraethylammonium iodide and 10 mL of analytically pure N,N-dimethylformamide, put the cathode as a copper electrode and the anode In a one-chamber electrolytic cell with graphite rods, in which: glycerol is the substrate, N,N-dimethylformamide is the solvent after drying with 4? grade molecular sieves, tetraethylammonium iodide is the supporting electrolyte, tetraethylammonium Ammonium iodide and glycerol are analytically pure.

[0033] b. Electrolysis

[0034] Under normal pressure, carbon dioxide is passed into the electrolytic cell to saturation, and then at 8.37mA / cm 2 The current density is 0°C, the constant current electrolysis is carried out, and the current flow is 193C.

[0035] c. Esterification

[0036] After the electrochemical reaction is over, transfer the above electrolytic solution into the flask, add 0.3g of anhydrous potassium carbonate and 0.3mL of an...

Embodiment 3

[0040] a. Preparation of electrolyte

[0041] After mixing 0.1M (0.0921g) glycerol with 0.1M (0.2572g) tetraethylammonium iodide and 10 mL of analytically pure N,N-dimethylformamide, put the cathode as a copper electrode and the anode In a one-chamber electrolytic cell with graphite rods, in which: glycerol is the substrate, N,N-dimethylformamide is the solvent after drying with 4? grade molecular sieves, tetraethylammonium iodide is the supporting electrolyte, tetraethylammonium Ammonium iodide and glycerol are analytically pure.

[0042] b. Electrolysis

[0043] Under normal pressure, feed carbon dioxide into the electrolytic cell to saturation, and then use 10.01mA / cm 2 The current density is 25°C, and the constant current electrolysis is carried out, and the current flow is 193°C.

[0044] c. Esterification

[0045] After the electrochemical reaction is over, transfer the above electrolytic solution into the flask, add 0.3g of anhydrous potassium carbonate and 0.3mL of...

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Abstract

The invention discloses a synthetic method of glycerol carbonate. The synthetic method is characterized in that: N,N-dimethylformamide is mixed with tetraethyl ammonium iodide and glycerol to obtain an electrolyte, the electrolyte is saturated with CO2 at normal pressure and is electrolyzed under conditions of a constant current, and the electrolyte is esterified and distillated to prepare glycerol carbonate. Compared with the prior art, the synthetic method of the invention, which has the advantages of simple technology, convenient operation, safety, cheap and easily available raw material, effective utilization of a greenhouse effect gas carbon dioxide, substantial reduction of atmospheric pollution, realization of the high efficiency conversion of glycerol, and alleviation of the increasingly exhausted energy problem and has a very significant meaning to the environment protection, is a technical route with a good industrial synthetic value.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a synthesis method of glycerol carbonate. Background technique [0002] Glycerol carbonate, English name: glycerol carbonate, molecular formula C 4 h 6 o 4 , with a molecular weight of 118.09, is a colorless viscous liquid with a boiling point of 137-140°C 0.5mm Hg (lit.), irritating, slightly soluble in water and ether, and soluble in ester. Glycerol carbonate is a multifunctional compound with a wide range of applications and relatively promising market prospects. Glycerol carbonate can be used as a proton solvent, a liquid membrane for separating carbon dioxide and nitrogen, and an additive in lithium batteries; it is also an important organic synthesis intermediate, which can be used to synthesize polycarbonate and polyurethane; because it has no side effects, it has low toxicity , low evaporation, low ignition and moisturizing type, and can also be use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07C69/96C07C68/04
Inventor 王欢朱美侠吴腊霞鲍少华张贵荣陆嘉星
Owner EAST CHINA NORMAL UNIV
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