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Ion liquid catalyst for synthesizing diethyl carbonate by urea alcoholysis and preparation method thereof

A technology of diethyl carbonate and ionic liquid, which is applied in the field of ionic liquid catalyst and its preparation, can solve problems such as safety hazards and equipment corrosion, and achieve the effects of good stability, low price and high catalyst activity

Inactive Publication Date: 2013-02-06
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production method of DEC uses highly toxic phosgene as raw material, causing serious equipment corrosion, safety hazards and environmental problems

Method used

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  • Ion liquid catalyst for synthesizing diethyl carbonate by urea alcoholysis and preparation method thereof
  • Ion liquid catalyst for synthesizing diethyl carbonate by urea alcoholysis and preparation method thereof
  • Ion liquid catalyst for synthesizing diethyl carbonate by urea alcoholysis and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Catalyst preparation:

[0019] Under the protection of nitrogen, weigh 13.9736g of BMIMCl into a three-necked flask, add 10.9040g of zinc chloride and 7.6168g of magnesium chloride respectively, react at 105°C for 48h, and put it in a desiccator for later use.

[0020] Application experiment one:

[0021] Weigh 20.86g of urea, 200ml of absolute ethanol and 7.23g of catalyst into the autoclave, at 190°C, the stirring rate is 900r / min, react for 6h, take out the reaction product after cooling, analyze and calculate the DEC by gas phase internal standard method yield.

[0022] Based on urea, the yield of DEC is 22.08%.

[0023] Application experiment two:

[0024] Weigh 20.86g of urea, 200ml of absolute ethanol and 9.04g of catalyst into the autoclave, at 190°C, the stirring rate is 800r / min, react for 6h, take out the reaction product after cooling, analyze and calculate the DEC by gas phase internal standard method yield.

[0025] Based on urea, the yield of DEC is ...

Embodiment 2

[0030] Catalyst preparation:

[0031] Under nitrogen protection, weigh 8.7335g of 1-methyl-3-butylimidazole chloride into a three-necked flask, add 13.6295g of zinc chloride, react at 110°C for 48h, and put it in a desiccator for later use.

[0032] Application experiment one:

[0033] Weigh 20.86g of urea, 200ml of absolute ethanol and 9.04g of catalyst into the autoclave, at 210°C, the stirring rate is 900r / min, react for 5h, take out the reaction product after cooling, analyze and calculate the DEC by gas phase internal standard method yield.

[0034] Based on urea, the yield of DEC is 20.32%.

[0035] Application experiment two:

[0036] Weigh 20.86g of urea, 200ml of absolute ethanol and 9.04g of catalyst into the autoclave, raise the temperature to 230°C, stir at 900r / min, and react for 1h. Then the temperature was lowered to 200°C, the stirring rate was 800r / min, and the reaction was carried out for 4h. After cooling, the reaction product was taken out, and the yie...

Embodiment 3-6

[0039] The selected precursors and reaction conditions are shown in Table 1, and the other reaction conditions are the same as those in Example 1 except that the added metal chlorides and their amounts are different. The catalysts prepared above were used to catalyze the alcoholysis of urea to synthesize DEC, and the yield of DEC was analyzed and calculated by the gas phase internal standard method, as shown in Table 1.

[0040] Table 1 Effects of different catalyst ratios and reaction conditions on the synthesis of DEC

[0041]

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Abstract

The invention provides a process for synthesizing diethyl carbonate by urea alcoholysis through an ion liquid catalyst. The catalyst is imidazole metal salts ion liquid. The method comprises the steps of adding absolute ethyl alcohol, urea and the catalyst into a high-pressure reaction kettle, wherein the agitation speed is 700-1000 r / min, the mol ratio of the absolute ethyl alcohol to the urea ranges from 5: 1 to 15: 1; the reaction temperature is 160-230 DEG C, the reaction time is 4-10 hours and the use amount of the ion liquid catalyst is 1-10% of the mass of raw materials; cooling to room temperature and separating to obtain a product; enabling 1-methylimidazole and n-chlorobutane (in a mol ratio of 1: 1) to react to synthesize an intermediate chlorinated 1-butyl-3-methylimidazole (BMIMCl); and further enabling the BMIMCl to react with a metal chloride to obtain a product. The added metal chloride is Lewis acid of zinc chloride, magnesium chloride, aluminum chloride, lead chloride, calcium chloride and the like, and is prepared by adding one or more of the Lewis acid to react according to a certain ratio. The method has the advantages of green environmental friendliness, high repeated utilization rate, simple process, no corrosion, selectivity of close to 100%, high yield (which is close to 30% to the greatest extent) and the like.

Description

technical field [0001] The invention relates to an ionic liquid catalyst for synthesizing diethyl carbonate by alcoholysis of urea and a preparation method thereof, belonging to the technical field of organic carbonate synthesis. Background technique [0002] Diethyl carbonate (DEC) is an important substance in carbonates, an important intermediate in organic synthesis, and has high industrial application value. DEC can be used as solvent, surfactant and lithium battery electrolyte additive, etc. The biggest potential use of DEC is as a fuel oxygen additive to replace the traditional methyl tert-butyl ether (MTBE). The oxygen value of DEC (40.6%) is much higher than that of MTBE (18.2%). When used as an oxygen-containing additive for gasoline and diesel fuel, it can improve the combustion performance of the fuel and reduce the emission of pollutants. The traditional production method of DEC uses highly toxic phosgene as raw material, causing serious equipment corrosion, sa...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C69/96C07C68/00
Inventor 范明明王辉张萍波倪邦庆
Owner JIANGNAN UNIV
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