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Method of synthesizing diethyl carbonate by basic ionic liquid as catalyst

A technology of diethyl carbonate and liquid catalyst, applied in chemical instruments and methods, preparation of organic carbonates, preparation of organic compounds, etc., can solve the problems of difficult recycling, low product yield, equipment corrosion, etc., and achieve easy separation Recovery, high catalyst activity, and low equipment corrosion

Inactive Publication Date: 2014-03-19
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The yield of diethyl carbonate in the gas phase method is low, and there is a hidden danger of explosion in the reaction system; at the same time, most of the catalysts are noble metal salts. Because the reaction produces water as a by-product, the catalyst is easily decomposed when it encounters water, causing catalyst poisoning
The liquid phase method uses a copper-based catalyst, which has problems such as short life, serious equipment corrosion, product separation, and difficulty in recycling.
The carbon monoxide gas-phase catalytic coupling synthesis method consists of two steps of synthesis reaction and regeneration reaction. There is a problem of how to optimize the cycle matching in engineering scale-up, and nitrous acid is highly toxic and has potential safety hazards.
The second step of the urea alcoholysis synthesis method is controlled by thermodynamics, the yield of diethyl carbonate product is low (≤30%), and the metal-organic homogeneous catalyst is difficult to separate and recover from the product, with high toxicity and high price
The transesterification reaction of dimethyl carbonate is controlled by thermodynamics, and the transesterification reaction is a reversible reaction, the process route is relatively complicated, the product yield is low, and the raw material carbonate is restricted by the petrochemical industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Adopt batch tank type reactor, and reactor specification is 1000ml, is catalyzer with [Bmim]Im alkaline ionic liquid, and the mol ratio of raw material propylene carbonate and ethanol is 1:6, and the consumption of catalyzer accounts for raw material gross mass and is 2%, The reaction temperature is 65° C., the reaction pressure is 0.1 MPa, and the stirring speed is 600 r / min. Firstly, propylene carbonate is added into the reaction kettle and heated to the reaction temperature, then the alkaline ionic liquid is dissolved in ethanol, heated to the reaction temperature, and then the ethanol solution is added into the reaction kettle to carry out the reaction. After the reaction was completed, the mixture was analyzed by gas chromatography, and the conversion rate of propylene carbonate was 58.2%, and the yield of diethyl carbonate was 57.9%. After the reaction, the mixture is first separated from the catalyst by conventional vacuum distillation, and then separated by inte...

Embodiment 2

[0023] A batch tank reactor is adopted, the reactor specification is 1000ml, and [Bmim]OH basic ionic liquid is used as a catalyst, the molar ratio of the raw material propylene carbonate to ethanol is 1:2, and the consumption of the catalyst accounts for 0.1% of the total mass of the raw material, The reaction temperature is 30° C., the reaction pressure is 0.01 MPa, and the stirring speed is 200 r / min. Firstly, propylene carbonate is added into the reaction kettle and heated to the reaction temperature, then the alkaline ionic liquid is dissolved in ethanol, heated to the reaction temperature, and then the ethanol solution is added into the reaction kettle to carry out the reaction. After the reaction was completed, the mixture was analyzed by gas chromatography, and the conversion rate of propylene carbonate was analyzed to be 52.3%, and the yield of diethyl carbonate was 51.7%. The separation of catalyst and product is the same as in Example 1.

Embodiment 3

[0025] Adopt batch tank reactor, the reactor specification is 1000ml, with ChIm alkaline ionic liquid as catalyst, the mol ratio of propylene carbonate and ethanol is 1:12, the consumption of catalyst accounts for 8% of raw material gross mass, and reaction temperature is 125 °C, the reaction pressure is 0.5MPa, and the stirring speed is 1200r / min. Firstly, propylene carbonate is added into the reaction kettle and heated to the reaction temperature, then the alkaline ionic liquid is dissolved in ethanol, heated to the reaction temperature, and then the ethanol solution is added into the reaction kettle to carry out the reaction. After the reaction was completed, the mixture was analyzed by gas chromatography, and the conversion rate of propylene carbonate was 55.3%, and the yield of diethyl carbonate was 55.2%. The separation of catalyst and product is the same as in Example 1.

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Abstract

The invention belongs to the technical field of catalytic synthesis of carbonic ester by ionic liquids, and specifically relates to a method of synthesizing diethyl carbonate by a basic ionic liquid as a catalyst. According to the method, propylene carbonate and ethanol are taken as raw materials or ethylene carbonate and ethanol are taken as raw materials, and the basic ionic liquid is selected as the catalyst, so that diethyl carbonate is synthesized through ester exchange. Based on deficiencies of conventional catalysts (solid acids and alkalis, resin, alkali salt and the like) and advantages of the ionic liquid, the invention provides the method of synthesizing diethyl carbonate by the basic ionic liquid as the catalyst. The method has the advantages of high catalyst activity (selectivity is close to 100%, and yield is 45-65%), short synthetic route, mild reaction condition, less equipment corrosion, environment-friendliness, good stability of catalyst, easiness in separation and recovery, repeated use in maintaining high activity and the like.

Description

technical field [0001] The invention belongs to the technical field of organic carbonate synthesis, and in particular relates to a method for synthesizing diethyl carbonate by using an alkaline ionic liquid as a catalyst. technical background [0002] Diethyl carbonate is an important substance in carbonates. It can be used as an organic solvent with excellent performance, and can also be used as a synthetic intermediate and textile auxiliaries. It is widely used in lithium battery electrolyte additives and surfactants in the industrial field; in addition , the oxygen content of diethyl carbonate is 40.6%, which is much higher than that of methyl tert-butyl ether (18.2%). It can be used as an oxygen-containing additive for gasoline and diesel engine fuel to increase the octane number of the fuel, enhance the combustion performance, and reduce the Carbon dioxide emissions from gasoline exhaust. At the same time, as the United States and Western Europe restrict the use of met...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
CPCC07C68/065
Inventor 李玲吴承明董晓莲王红星叶长燊邱挺
Owner FUZHOU UNIV
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