Process for synthesizing methyl carbonate by alcoholysis of urea with aliphatic diol as cyclic agent

A technology for aliphatic diol and dimethyl carbonate, which is applied in the field of urea alcoholysis to synthesize dimethyl carbonate, can solve problems such as difficult control, energy consumption, and unfavorable reactions are carried out normally, and achieves mild reaction conditions and easy recovery and regeneration. , the effect of not polluting the environment

Inactive Publication Date: 2005-01-26
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the reaction process, the decompression operation not only consumes energy, but also is difficult to control, which is not conducive to the normal progress of the reaction.
The common disadvantage of the two processes is that it is difficult to separate and recycle homogeneous and powdery catalysts from products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take Mg(CH 3 COO) 2 4H 2 O is dissolved in distilled water to form C Mg 2+ =0.8mol / L solution, then get Zn(CH 3 COO) 2 2H 2 O is added to the above solution to form C Zn 2+ =0.1mol / L solution; take a certain amount of 25% (wt%) ammonia water, and dilute it to 1.33mol / L ammonia water; keep the pH value at about 10, stir for 1h after the titration, then age for 24h, filter, and obtain The precipitate was dried and calcined in a muffle furnace at 600°C for 4 hours to prepare a composite metal oxide catalyst of Mg and Zn for future use.

[0013] Add 9g of urea, 46g of 1,2-propanediol, and 5g of the catalyst prepared above into a 250mL four-necked bottle, turn on the stirrer, heat to 170°C, and the reaction time is 3h. The four-necked bottle is equipped with a thermometer, reflux condenser, stirrer and Nitrogen inlet. The composition of the product was analyzed by gas chromatography, and the content of each component in the sample was determined by the external sta...

Embodiment 2

[0015] Take Co(NO 3 ) 2 2H 2 O1.12g, Zn(CH 3 COO) 2 2H 2 O6.72g, mixed and ground evenly, calcined at 450°C to 550°C for 4h to prepare a composite metal oxide catalyst of Co and Zn for future use.

[0016] Add 9g of urea, 46g of 1,2-propanediol, and 5g of the catalyst prepared above into a 250mL four-necked bottle, turn on the stirrer, heat to 170°C, and the reaction time is 3h. The four-necked bottle is equipped with a thermometer, reflux condenser, stirrer and Nitrogen inlet. The composition of the product was analyzed by gas chromatography, and the content of each component in the sample was determined by the external standard method by using a thermal conductivity detector. The yield of PC was determined to be 90%.

Embodiment 3

[0018] Composite oxides of Fe and Mg were prepared by equal volume impregnation. Prepare 0.12mol / L Fe(NO 3 ) 3 The aqueous solution was slowly added dropwise to the MgO carrier, and calcined at 450°C for 4h to obtain the catalyst, which was set aside.

[0019] Add 9g of urea, 46g of 1,2-ethylene glycol, and 5g of the catalyst prepared above into a 250mL four-necked bottle, turn on the stirrer, heat to 180°C, and the reaction time is 3h. The four-necked bottle is equipped with a thermometer, reflux condenser, and stir device and nitrogen inlet. The composition of the product was analyzed by gas chromatography, and the content of each component in the sample was determined by the external standard method by using a thermal conductivity detector. The yield of PC was determined to be 93%.

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Abstract

The invention discloses a process for synthesizing methyl carbonate by alcoholysis of urea with aliphatic diol as cyclic agent consisting two steps, (1) reacting urea with aliphatic diatomic alcohol (ethylene glycol or 1,2-methyl ethylene glycol) to synthesize ethylene carbonate ester or propylene carbonate ester, (2) subjecting ethylene carbonate ester or propylene carbonate ester with methanol ester to synthesize methylcarbonate.

Description

technical field [0001] The invention relates to a method for synthesizing dimethyl carbonate, in particular to a method for synthesizing dimethyl carbonate by alcoholysis of urea with aliphatic dihydric alcohol as a circulating agent. Background technique [0002] The method for synthesizing dimethyl carbonate by alcoholysis of urea with aliphatic dibasic alcohol as circulating agent comprises two steps, the first step is the reaction of urea and aliphatic dibasic alcohol (ethylene glycol or 1,2-propanediol) to synthesize ethylene carbonate Or propylene carbonate, the second step is to transesterify ethylene carbonate or propylene carbonate with methanol to synthesize dimethyl carbonate, and the by-product ethylene glycol or 1,2-propanediol is recycled to the first step reaction. In addition, ethylene carbonate (abbreviated as EC) and propylene carbonate (abbreviated as PC) are high-boiling organic solvents and organic synthesis intermediates with excellent performance, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/00C07C69/96
Inventor 赵新强张艳陈英王延吉
Owner HEBEI UNIV OF TECH
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