Process for continuously preparing cyclic carbonate

A cyclic carbonate, process technology, applied in the field of continuous preparation of cyclic carbonate, can solve the problems of high cost, difficult separation of product and catalyst, harsh reaction conditions, etc.

Inactive Publication Date: 2011-11-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent 02112549.x discloses a method for catalyzing the synthesis of ethylene carbonate using tetraethylammonium bromide. The method is above 130°C and the pressure of carbon dioxide is above 3MPa, and the conversion rate of ethylene oxide is above 95%. , but this method requires

Method used

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  • Process for continuously preparing cyclic carbonate
  • Process for continuously preparing cyclic carbonate
  • Process for continuously preparing cyclic carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] exist figure 1 In the reaction process shown, the volume of the stirred tank R1 is 1 liter, and the volume of the flat-push tubular reactor R2 is 0.5 liters. The stirred tank is equipped with double-layer electromagnetic stirring with speed regulation, jacket heating, and a condensing coil inside. ; The temperature of the electric heating on the outer wall of the tubular reactor is controllable.

[0035]Zinc bromide (2 g) and methyl butyl imidazolium bromide (18 g) dissolved in ethylene carbonate (300 g) were added into the catalyst preparation kettle V5 to prepare a catalyst solution. High-purity carbon dioxide purge replacement system. The catalyst solution is injected into the continuous reaction system by the pump P3, and carbon dioxide and ethylene oxide raw materials are introduced. The temperature of reactors R1 and R2 is controlled at 140°C and 3.0Mpa. The temperature of the reaction liquid in the gas-liquid separator V1 is 60° C. and 0.5 MPa to separate the ...

Embodiment 2

[0046] The same operating conditions as in Example 1, the raw material is propylene oxide, and the catalyst configuration uses propylene carbonate. After HP MS6890 / 5973 chromatography-mass spectrometry and quantitative analysis, the purity of the product is greater than 99%, and the yield of propylene carbonate is 99%. The results of continuous reaction for 100 hours are listed in Table 1.

Embodiment 3

[0048] Same operating condition as embodiment 1, catalyzer changes zinc chloride and tetraethyl ammonium chloride into

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Abstract

The invention discloses a process for continuously preparing cyclic carbonate. According to the invention, an epoxy compound and carbon dioxide gas are adopted as raw materials, and a cycloaddition reaction is continuously carried out upon the raw materials with the existences of an ionic liquid catalyst and a zinc halogeno salt promoter. A combined separation by using a reduced-pressure gas-liquid separator and a thin film evaporator is carried out, such that cyclic carbonate produced from the reaction and microscaled unreacted epoxy compound are obtained through the separation. A residual solution containing the ionic liquid catalyst, the zinc halogeno salt promoter and cyclic carbonate is delivered into the reactor through circulation, and is used for catalyzing in the cycloaddition reaction. With the process provided by the invention, a purity of produced cyclic carbonate is higher than 99.5%, and a single pass conversion rate of the epoxy compound reaches 99.0%.

Description

technical field [0001] The invention discloses a process for continuously preparing cyclic carbonate. More specifically, the present invention relates to a process for the continuous preparation of cyclic carbonates by cycloaddition of carbon dioxide and epoxides. Background technique [0002] The preparation of cyclic carbonates by the addition of carbon dioxide and epoxy compounds is not only an effective way to fix carbon dioxide, but also the first step in the synthesis of dimethyl carbonate by transesterification. Cyclic carbonate is an organic solvent with high boiling point and high polarity with excellent performance. It is used in the synthesis of pharmaceutical and fine chemical intermediates, organic synthesis, cosmetics, metal extraction, and desulfurization and decarbonization in industrial sectors such as natural gas purification, urea and hydrogen production ( CO 2 ) are widely used in the field. In recent years, the market demand for cyclic carbonates as i...

Claims

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Application Information

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IPC IPC(8): C07D317/38
Inventor 夏春谷许传芝张愔陈静
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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