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A kind of method for preparing dialkyl carbonate by alcoholysis of urea

A technology of dialkyl carbonate and urea alcohol, which is applied in the field of preparation of dialkyl carbonate, can solve the problems of high investment in pressurized equipment, difficult operation, unsatisfactory product yield, etc., and achieves good industrial application prospects, Good safety and low cost of process equipment

Active Publication Date: 2021-07-13
雷永诚 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the investment of pressurized equipment is high and the operation is difficult
[0011] (3) The reaction of urea with methanol and ethanol with low boiling point, the product yield is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] The reaction device is a 200 ml three-necked glass flask equipped with a rectification column with a diameter of 30 mm and a length of 300 mm filled with 2 mm*2 mm stainless steel θ rings, and a condenser. Take 10g of urea, 22g of methanol, 50g of sulfolane, 0.5g of nickel acetate, and 2g of triphenylphosphine in a three-necked flask, and heat it in an oil bath at 170°C. The system boils and refluxes at 85°C, and stirs and refluxes for 10 hours; After condensing, it enters the receiver, the system heats up to 130°C, and the light component liquid in the receiver is injected back into the reaction bottle to maintain the liquid level of the receiver, the system temperature is maintained at 130~150°C, and the reaction is stirred and refluxed for 15 hours. According to gas chromatography analysis, the yield of dimethyl carbonate was 89.3% based on the amount of input urea, and no methyl N-methyl formate was detected in the system.

Embodiment 2

[0065] The reaction device is the same as in Example 1. Take 10g of urea, 31g of ethanol, 50g of sulfolane, 0.5g of nickel acetate, and 2g of triphenylphosphine in a three-necked flask, and heat it in an oil bath at 170°C. The system boils and refluxes at 95°C, and stirs and refluxes for 8 hours; remove some light components from the system. After condensing, it enters the receiver, the system heats up to 130°C, and the light component liquid in the receiver is injected back into the reaction bottle to maintain the liquid level of the receiver, the system temperature is maintained at 130~150°C, and the reaction is stirred and refluxed for 15 hours. According to gas chromatography analysis, the yield of diethyl carbonate was 92.4% based on the amount of urea input.

Embodiment 3

[0067] The reaction device is the same as in Example 1. Take 10g of urea, 40g of n-propanol, 0.5g of nickel acetate, and 2g of triphenylphosphine in a three-necked flask, heat it in an oil bath at 170°C, and boil the system at 105°C to reflux, stir and reflux for 8 hours; the system is heated to 130°C, The temperature of the system was maintained at 130-150°C, and the reaction was stirred and refluxed for 15 hours. According to gas chromatography analysis, the yield of di-n-propyl carbonate was 93.6% based on the amount of urea input.

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PUM

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Abstract

The invention discloses a method for preparing dialkyl carbonate by alcoholysis of urea, which belongs to the field of chemical synthesis. More specifically, it relates to the preparation of dialkyl carbonates. Urea and alkyl monohydric alcohol are under normal pressure or reduced pressure, the reaction temperature is 70 ~ 150 ℃, and one or more of metal magnesium, calcium, aluminum, chromium, manganese, iron, cobalt, nickel, copper, or zinc One or more compounds containing electron-donating atoms nitrogen, phosphorus, oxygen, or sulfur are used as co-catalysts, stirred and refluxed for 6-30 hours to prepare dialkyl carbonate. The present invention prepares dialkyl carbonate with high selectivity and high yield at a lower reaction temperature under normal pressure or reduced pressure, and has simple process operation, high safety and low cost, and has good industrial application prospects .

Description

technical field [0001] The invention discloses a method for preparing dialkyl carbonate by alcoholysis of urea, which belongs to the field of chemical synthesis. More specifically, it relates to the preparation of dialkyl carbonates. Background technique [0002] Dialkyl carbonate is an important class of compounds, many of which have been commercially produced and widely used in industry. Dimethyl carbonate is a green chemical, widely used as a solvent in coatings, paints, lithium batteries and other industries, as a synthetic raw material for the clean production of polycarbonate, methyl carbamate, isocyanate and other products; diethyl carbonate It is an important solvent in the textile industry and battery production industry, and can also be used as a synthetic raw material for various chemicals; dipropyl carbonate is an important solvent in the battery production industry, and is also an important synthetic raw material; dibutyl carbonate is used in industry Producti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/00C07C69/96
CPCC07C68/00C07C269/00C07C271/12C07C69/96
Inventor 雷永诚雷永忠吕庆洪王毓
Owner 雷永诚
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