Direct synthesis process of methyl carbonate

A dimethyl carbonate, direct technology, applied in carbon dioxide or inorganic carbonate preparation, bulk chemical production, organic chemistry, etc., can solve the problems of poor selectivity and low yield, and achieve high yield and good selectivity Effect

Inactive Publication Date: 2004-09-08
INST OF CHEM CHINESE ACAD OF SCI
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Problems solved by technology

[0007] The purpose of the present invention is to overcome the low yield of prior art, the defect of poor selectivity, thereby provide a kind of yield height, the method for the direct synthesis of dimethyl carbonate with good selectivity, the method uses catalyzer, in compression or supercritical carbon dioxide Direct synthesis of dimethyl carbonate from alkylene oxide, carbon dioxide and methanol

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  • Direct synthesis process of methyl carbonate

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Experimental program
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Effect test

Embodiment 1

[0017] Add 0.44g (10mmol) of oxirane in reaction vessel, methanol 1.28g (40mmol) and carbon dioxide 6.1g (139mmol), add the catalyst 0.25g of 3.19wt% of reaction mixture weight, catalyst is KI 30wt%, ZnO55wt% and K 2 CO 3 15% by weight of the composition. Stir, heat up to 150°C, and react for 2 hours. The temperature was lowered to 120° C., and the reaction was continued for 2 hours. After the reaction was finished, it was cooled, filtered, and the catalyst was removed, and the filtered reaction solution was analyzed by gas chromatography. The conversion rate of ethylene oxide was 99.3%, and the selectivity of dimethyl carbonate was 70.8%.

Embodiment 2

[0019] In reaction vessel, add propylene oxide 0.58g (10mmol), methyl alcohol 1.92g (60mmol) and carbon dioxide 8.8g (200mmol), add the catalyzer 0.23g of 2.03wt% of reaction mixture weight, catalyzer is KCl 45wt%, ZrO40wt% and Na 2 CO 3 15% by weight of the composition. Stir, heat up to 160°C, and react for 4 hours. The temperature was lowered to 130° C., and the reaction was continued for 4 hours. After the reaction, supercritical CO 2 Extraction, the obtained reaction solution was analyzed by gas chromatography, the conversion rate of propylene oxide was 98.2%, and the selectivity of dimethyl carbonate was 41.5%.

Embodiment 3

[0021] Add phenyloxirane 0.72g (6mmol) in reaction vessel, methyl alcohol 1.92g (60mmol) and carbon dioxide 5.3g (120mmol), add the catalyzer 0.32g of 4.03wt% of reaction mixture weight, catalyzer is KBr 25wt%, Composition of NaX type molecular sieve 60wt% and NaOH 15wt%. Stir, heat up to 170°C, and react for 3 hours. The temperature was lowered to 110° C., and the reaction was continued for 6 hours. After the reaction, supercritical CO 2 Extraction, the obtained reaction liquid was analyzed by gas chromatography, the conversion rate of phenyloxirane was 98.5%, and the yield rate of dimethyl carbonate was 54.8%.

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Abstract

The direct synthesis process of methyl carbonate includes adding epoxy alkane, methanol and CO2 in the molar ratio of 1 to 2-10 to 10-20 and catalyst in the amount of 2-8 wt% of reactant mixture into reactor; stirring and heating to 150-170 deg.c for reaction of 2-6 hr and lowering the temperature to 110-140 deg.c for reaction of another 2-6 hr; cooling, filtering to eliminate catalyst or supercritical extraction to obtain reactant solution containing methyl carbonate. The catalyst is one kind of composite including active component potassium iodide in 5-60 wt%; assistant K2CO3, KOH, Na2CO3 or NaOH in 0-20 wt% and carrier metal oxide or zeolite molecular sieve in 40-90 wt%. The direct synthesis process of the present invention has high yield and high selectivity.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a method for directly synthesizing dimethyl carbonate from alkylene oxide, carbon dioxide and methanol by using a catalyst. Background technique [0002] Dimethyl Carbonate (Dimethyl Carbonate is called for short DMC) because of its excellent chemical properties, can be used as a kind of green organic synthesis intermediate and gasoline additive, and its synthesis and application have received extensive attention in recent years (Y.Ono., Appl. Catal. A:, 1997, 155, 133). Synthesis of dimethyl carbonate directly from alkylene oxide, carbon dioxide, and methanol (as shown in the figure below), due to the use of abundant and cheap greenhouse gas carbon dioxide, the process is simple, and the cyclic carbonate and diols produced at the same time have also been developed to a certain extent market and is therefore a fairly competitive approach. [0003] [0004] R = Ph, C n h 2n+1 (n=0~4) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/04C07C69/96
CPCY02P20/54
Inventor 常雁红韩布兴姜涛刘志敏何俊杨冠英杜记民黄莹
Owner INST OF CHEM CHINESE ACAD OF SCI
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