Preparation method of propylene carbonate

A technology of propylene carbonate and propylene oxide, which is applied in the field of preparation of propylene carbonate, can solve the problems of low yield and harsh reaction conditions, and achieve the effects of reasonable weight ratio, mild reaction conditions and easy realization

Inactive Publication Date: 2012-11-07
HUNAN KAIMEITE GASES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention will solve the technical problems of low yield and harsh reaction conditions in the in

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Get zinc fluoride and potassium iodide of 5ml propylene oxide and 0.8mol% catalytic amount and join in the reactor, the weight ratio of zinc fluoride and potassium iodide is 1.8: 0.8, makes reactor be in sealed state, fills into 1.8MPa excessive carbon dioxide, Place the reaction kettle in an electric heating mantle, set the heating temperature, and use a sensor to control the temperature, react at 90°C for 10 hours, place the reaction kettle in an ice-water bath, stop the reaction, mix the reaction solution, take 0.1894g of the reaction solution, Add 0.0934g of chlorobenzene as an internal standard, and then add 30ml of ethyl acetate as a solvent to form a mixed solution, and measure its concentration with a method established in a gas chromatograph to obtain a yield of 93%.

Embodiment 2

[0019] Get zinc fluoride and potassium iodide of 5ml propylene oxide and 1.5mol% catalytic amount and join in the reactor, the weight ratio of zinc fluoride and potassium iodide is 2.2: 1.2 makes reactor be in sealed state, fills into 2.0MPa excessive carbon dioxide, will The reaction kettle is placed in an electric heating mantle, the heating temperature is set, and the temperature is controlled by a sensor. React for 8 hours at 140°C. Place the reaction kettle in an ice-water bath to stop the reaction. Mix the reaction solution evenly. Take 0.2040g of the reaction solution and add 0.1022g chlorobenzene was used as an internal standard, and 30ml ethyl acetate was added as a solvent to form a mixed solution, and its concentration was measured by an established method in a gas chromatograph, and the yield was 90%.

Embodiment 3

[0021] Get the propylene oxide that 5ml molecular sieves dry and zinc fluoride and potassium iodide of 0.3mol% catalytic amount and join in the reactor, the weight ratio of zinc fluoride and potassium iodide is 2.0: 1.0, make reactor be in sealed state, be filled with 2.0MPa Excessive carbon dioxide, put the reaction kettle on the electric heating mantle, set the heating temperature, and use the sensor to control the temperature, react at 140°C for 9 hours, put the reaction kettle in an ice-water bath, stop the reaction, mix the reaction solution, take 0.1746g To the reaction solution, 0.0872g chlorobenzene was added as an internal standard, and 30ml ethyl acetate was added as a solvent to form a mixed solution. The concentration was determined by a method established in a gas chromatograph, and the yield was 97%.

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Abstract

The invention relates to preparation of propylene carbonate, particularly to a preparation method of propylene carbonate. The preparation method of propylene carbonate comprises the following steps: (1) based on carbon dioxide and epoxypropane as raw materials, adding epoxypropane and 0.3-3.0mol% of catalytic amounts of zinc fluoride and potassium iodide to a reaction kettle, and keeping the reaction kettle in a sealing state, wherein the weight ratio of zinc fluoride to potassium iodide is (1.8-2.2): (0.8-1.2); (2) filling 1.8-2.0MPa of excessive carbon dioxide, and performing reaction for 8-11h at 90-160 DEG C; (3) putting the reaction kettle to ice-water bath, and stopping reacting. The preparation method of propylene carbonate has the following advantages: 1) because zinc fluoride and potassium iodide are used as catalysts and the weight proportion is reasonable, a good synergic catalysis effect is achieved and the yield is more than 97%; and 2) the reaction pressure is 2.0MPa at most and the reaction temperature is 160 DEG C at most, so that the reaction condition is mild, the method is easy to realize and the cost can be saved.

Description

technical field [0001] The invention relates to the preparation of propylene carbonate, in particular to the industrial preparation of propylene carbonate by the synthetic method of carbon dioxide and propylene oxide. Background technique [0002] Propylene carbonate is not only an excellent organic solvent, but also an important organic chemical product, which has been widely used in the fields of organic synthesis, gas separation, electrochemistry and metal extraction. Especially in recent years, propylene carbonate has been widely used as a raw material for the synthesis of dimethyl carbonate by transesterification, which has played a role in promoting the research on the synthesis method of propylene carbonate. Propylene carbonate is mainly synthesized by methods such as transesterification, phosgene method, chloropropanol method, urea alcoholysis method, carbon dioxide and 1,2. propylene glycol synthesis method, carbon dioxide and propylene oxide synthesis method, among...

Claims

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Application Information

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IPC IPC(8): C07D317/36
Inventor 江国防孟凡燕张晓辉李文盛常纪良
Owner HUNAN KAIMEITE GASES
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