Catalyst for synthesizing diethyl carbonate from urea and ethanol and its preparation method and application

A technology of diethyl carbonate and catalyst, applied in the field of solid base catalyst and preparation thereof, can solve the problems of environmental pollution, toxicity, easy loss, etc., and achieve the effects of easy separation and recovery, high catalytic activity and good stability

Active Publication Date: 2018-01-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are more or less deficiencies in economy and technology: the phosgene method, the raw material phosgene is highly toxic, and the by-product hydrochloric acid corrodes the equipment, causing serious environmental pollution; the oxidative carbonylation method of ethanol, CO is poisonous, and the reaction material is flammable Explosive; transesterification method, high cost of raw material DMC, poor selectivity
Zhao Xinqiang et al. (NO.CN101659616A) used oxides or composite oxides such as lead and zinc to catalyze the alcoholysis of urea to synthesize DEC. The highest yield of DEC was 20%. The catalyst used was highly toxic and easily lost, which was not conducive to industrial application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 25.981g La(NO 3 ) 3 In a beaker, add 400mL deionized water, stir and heat to 60°C, add ammonia water dropwise until the pH value is 9-10, continue to stir for 3 hours, age, filter and wash until neutral, dry at 80°C, and calcine at 500°C for 4 hours . Prepared solid base La 2 o 3 .

Embodiment 2

[0025] In the autoclave, add 2.060g urea, 20mL absolute ethanol, the catalyst prepared in 0.350g example 1, exhaust the air in the kettle with nitrogen, stir and heat up, control the reaction temperature to be 210°C, the pressure is 2.2MPa, and the rotating speed is 550r / min, reacted for 3 hours, the obtained results are shown in Table 1.

Embodiment 3

[0027] Take 50mL of deionized water and heat it to 65°C, slowly add 0.15mol of Mg(NO 3 ) 2 and 0.05mol of AL(NO 3 ) 3 The mixed solution of 150mL, 2.0mol / L (NH 4 ) 2 CO 3 Solution 150mL, adjust the pH value between 9-10 with 25% ammonia water after the dropwise addition, stir and react at 65°C for 3 hours, filter, wash until neutral, dry at 100°C for 12 hours, and then calcined at 450°C for 3 hours . Prepared solid base Mg x AL y o x+3y / 2 (x:y=1:1‐3:1).

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PUM

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Abstract

The invention relates to a catalyst for synthesizing diethyl carbonate from urea and ethanol. The catalyst is a solid base catalyst and is prepared by precipitation or co-precipitation. Make an aqueous solution of alkaline earth metals, transition metals and other metal soluble metal salts, drop a certain amount of precipitant, and adjust the pH value between 8‑12 to obtain a precursor, and then dry it at 50‑150 °C for 2‑ 24 hours, and finally calcined at 200-1000°C for 2-10 hours. The invention has the advantages of simple preparation of the catalyst, high activity, environmental friendliness, easy separation and recovery, and good stability.

Description

technical field [0001] The invention relates to a catalyst and its preparation method and application, in particular to a solid base catalyst for synthesizing diethyl carbonate from urea and ethanol, its preparation method and application. technical background [0002] Diethyl carbonate, referred to as DEC, contains carbonyl, ethoxy, and ethyl groups in the molecule, which have good reactivity. A series of important organic chemical products are derived from the reaction. DEC itself is a low-toxic substance, which will slowly hydrolyze when released into the environment to generate ethanol and carbon dioxide, and will not pollute the environment. Therefore, it is an environmentally friendly chemical. It is used in solvents, electrolytes, organic synthesis, pharmaceuticals and engineering plastics, etc. Fields are widely used. The oxygen content of 40.6% of diethyl carbonate is much higher than that of methyl tert-butyl ether (MTBE) (18.2%). As an oxygen-containing additive...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/10B01J21/10C07C69/96C07C68/00
Inventor 李会泉辛淑敏王利国李凤姣曹妍
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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