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Technology of preparing diethyl carbonate by urea alcoholysis method

A technology of diethyl carbonate and urea alcohol, which is applied in the field of urea alcoholysis to synthesize diethyl carbonate, can solve the problems of short life and low catalyst activity, and achieve the effects of reduced operating costs, high catalytic activity, and good stability

Active Publication Date: 2010-03-03
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention solves the problems of low catalyst activity and short service life in the prior art, thereby providing a process for synthesizing diethyl carbonate by urea alcoholysis

Method used

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  • Technology of preparing diethyl carbonate by urea alcoholysis method
  • Technology of preparing diethyl carbonate by urea alcoholysis method
  • Technology of preparing diethyl carbonate by urea alcoholysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 (adopts thermal decomposition method to prepare lead-potassium composite metal oxide catalyst)

[0018] Weigh lead carbonate 6.70g and potassium nitrate 5.15g, make the mass ratio of lead oxide and potassium oxide in the catalyst be 7: 3, adopt mechanical grinding method to mix it evenly, and roast at 900 ℃ in the muffle furnace for 6 Hours, lead-potassium composite metal oxide catalyst was prepared.

[0019] Catalyst catalyzed urea alcoholysis synthesis DEC reaction with above-mentioned prepared:

[0020] (1) Add 200mL (3.425mol) absolute ethanol in the 500mL high-pressure reactor that is equipped with distillation column, 30g (0.337mol) ethyl carbamate, the lead-potassium composite metal oxide prepared above 1.6g (accounting for total reaction system The mass percentage is 0.84%);

[0021] (2) Feed nitrogen into the reactor to replace the air therein. Then, pressurize with nitrogen, and use a back pressure valve to control the pressure during the react...

Embodiment 2-6

[0025] Embodiment 2-6 (preparation of binary composite metal oxide catalyst by thermal decomposition method)

[0026] The preparation conditions of the selected precursors and catalysts are shown in Table 1. The catalysts prepared above were used to catalyze the synthesis of DEC by urea alcoholysis. Except for the catalyst and its dosage, the other reaction conditions were the same as in Example 1.

[0027] Table 1 The preparation conditions of different composite metal oxide catalysts and the influence of the mass percentage of the catalyst in the total system on the performance of the catalyst

[0028]

Embodiment 7-10

[0029] Embodiment 7-10 (preparation of binary composite metal oxide catalyst by thermal decomposition method)

[0030] The preparation conditions of the selected precursors and catalysts are shown in Table 2. The catalysts prepared above were used to catalyze the synthesis of DEC by the urea alcoholysis method. Except for the catalyst and the ratio of raw materials, the other reaction conditions were the same as in Example 1. Table 2.

[0031] Table 2 The preparation conditions of different composite metal oxide catalysts and the influence of the molar ratio of absolute ethanol and ethyl carbamate on the performance of the catalyst

[0032]

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PUM

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Abstract

The invention belongs to the synthesis of organic carbonates and relates to a technology of synthesizing diethyl carbonate by a urea alcoholysis method. The technology comprises the steps of: adding anhydrous ethyl alcohol, ethyl carbamate and a catalyst into a high pressure reaction kettle, wherein the mole ratio of the anhydrous ethyl alcohol to the ethyl carbamate is 2 to 25, and the catalyst is combined metal oxide, and accounts for 0.5 to 10 percent of the whole system by mass percent; raising the temperature to 150 to 200 DEG C by stirring so as to carry out reaction for 1 to 15 hours; and taking out the reaction liquid after the reaction, and realizing the separation of the catalyst and the reaction liquid by simple filtration. The combined metal oxide is prepared by 2 to 3 metal oxide precursors among Li, Na, K, Ca, Mg, Ba, Sr, Al, Sn, Pb, La, Ti, W, Zr, Fe, Co, Ni, Cu and Zn through thermal decomposition method or coprecipitation method. The preparation method of the technology is simple, the catalyst activity is high, the stability is good, and the separation and recycling are easy.

Description

technical field [0001] The invention belongs to the synthesis of organic carbonates, in particular to a process for synthesizing diethyl carbonate by urea alcoholysis. technical background [0002] Diethyl carbonate (DEC) is an important organic compound with high industrial application value in energy, automobile, electronics, medicine and other fields. DEC can be used as a general solvent for synthetic resins, nitrocellulose, and cellulose ethers; as a surfactant and lithium battery fluid additive; for the synthesis of pharmaceuticals and pharmaceutical intermediates, etc. The biggest potential use of DEC is as a fuel oxygen additive to replace the traditional methyl tert-butyl ether (MTBE). The oxygen content of DEC (40.6%) is much higher than that of MTBE (18.2%). When used as an oxygen-containing additive for gasoline and diesel engine fuel, it can improve the combustion performance of the fuel and reduce the emission of pollutants. Compared with the other two possibl...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/00B01J23/14B01J23/78B01J21/10B01J23/04B01J23/02B01J23/835B01J23/30B01J23/80B01J23/06B01J37/03B01J37/08
CPCY02P20/584
Inventor 赵新强赵海龙郭莲安华良王延吉
Owner HEBEI UNIV OF TECH
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