A method and system for preparing cyclohexyl acetate and separating cyclohexane and acetic acid

A technology of cyclohexyl acetate and cyclohexane, which is applied in the direction of carboxylate preparation, chemical instruments and methods, distillation purification/separation, etc., can solve the problems of unsuitability for large-scale industrial production, high cost, and low output, and achieve Reduce investment cost and operating cost, reduce separation energy consumption, and shorten the effect of separation process

Active Publication Date: 2021-07-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Before the 1980s, cyclohexyl acetate was synthesized by the reaction of cyclohexanol and acetic acid, and the output was low cost, which was not suitable for large-scale industrial production; with the industrial production of cyclohexene by partial hydrogenation of benzene, in recent years, cyclohexene has been used A large number of studies related to the preparation of cyclohexyl acetate by the reaction of hexene and acetic acid appeared

Method used

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  • A method and system for preparing cyclohexyl acetate and separating cyclohexane and acetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] step one

[0094] Under normal pressure, benzene is partially hydrogenated to obtain a mass fraction of 75% cyclohexene, 25% cyclohexane, and the mixture of 10ppm benzene is added from the feed port of the reactive distillation tower with acetic acid of 2kg / h and 3kg / h. The mol ratio of cyclohexene is 2.7, establish tower still liquid level 60%, tower still heats up, control reaction section (2) reaction temperature 78~90 ℃, and set up tower top oil-water phase tank (5) oil phase liquid level 60% -80%, start the oil phase reflux pump (7) at the top of the tower, and control the oil phase reflux ratio to 10;

[0095] step two

[0096] Add water in the water phase area of ​​the oil-water phase tank (5), establish the water phase liquid level of 30-50%, start the water phase reflux pump (6) on the top of the tower, and adjust the water phase reflux flow rate to about 0.55kg / h (the amount of reflux water is the tower 10% of the sum of the top oil phase reflux and the mass...

Embodiment 2

[0100] step one

[0101] Under normal pressure, benzene is partially hydrogenated to obtain a mass fraction of 35% cyclohexene, 15% cyclohexane, and a mixture of 50% benzene is added from the feed port of the reactive distillation tower at 2 kg / h and 0.56 kg / h of acetic acid. The molar ratio of acetic acid to cyclohexene is 1.1, and the liquid level of the tower kettle is 60%, the temperature of the tower kettle is raised, the reaction temperature of the reaction section (2) is controlled at 78-100° C., and the oil-water phase tank (5) oil phase liquid at the top of the tower is established. Bit 60-80%, the oil phase reflux ratio is controlled to 0;

[0102] step two

[0103] Add water in the water phase area of ​​the oil-water phase tank (5), set up the water phase liquid level of 30-50%, start the water phase reflux pump (6) on the top of the tower, and adjust the water phase reflux flow rate to about 0.14kg / h (the amount of reflux water is the tower 11% of the sum of the ...

Embodiment 3

[0107] step one

[0108] Under normal pressure, benzene is partially hydrogenated to obtain a mass fraction of 1.025% cyclohexene, 98.775% cyclohexane, and a mixture of 0.2% benzene. Add 2 kg / h and 3 kg / h of acetic acid from the feed port of the reactive distillation tower, and the acetic acid The molar ratio with cyclohexene is 200, and the liquid level of the tower kettle is established at 60%, the temperature of the tower kettle is raised, the reaction temperature of the reaction section (2) is controlled at 78-90°C, and the oil-water phase tank (5) at the top of the tower is established. 60-80%, the oil phase reflux ratio is controlled at 2;

[0109] step two

[0110] Add water in the water phase area of ​​the oil-water phase tank (5), set up the water phase liquid level of 30-50%, start the water phase reflux pump (6) on the top of the tower, and adjust the water phase reflux flow rate to about 0.56kg / h (the amount of reflux water is the tower 9.0% of the sum of the top...

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Abstract

The invention relates to a method for removing acetic acid from cyclohexane in preparation of cyclohexyl acetate by reactive distillation, and belongs to the field of petrochemical technology development. In the present invention, the mixture of cyclohexene and cyclohexane obtained by partial hydrogenation of benzene is used as a raw material, and in the process of preparing cyclohexyl acetate by reacting with acetic acid in a reactive distillation tower, the water phase at the top of the reactive distillation tower is circulated and refluxed, and combined with Cyclohexane in the tower forms an azeotrope, thereby reducing or eliminating the azeotropy between cyclohexane and acetic acid, and obtaining cyclohexane with an acetic acid content of less than 5wt%; then distilling cyclohexane through a simple azeotropic rectification tower to remove cyclohexane acetic acid in. The invention has simple process, strong parameter controllability, low energy consumption and material consumption, and is convenient for large-scale industrial application.

Description

technical field [0001] The invention relates to a method for preparing cyclohexyl acetate by reactive distillation and removing acetic acid by cyclohexane, and belongs to the field of petrochemical technology development. Background technique [0002] Cyclohexyl acetate is a liquid with banana or apple aroma, and the fruity flavor prepared with it is widely used in food, beverage and cosmetic industries. In addition, cyclohexyl acetate has good solubility for resins, and is often used as an environmentally friendly solvent for high-grade paints and paints. Ethanol and cyclohexanol can be obtained by hydrogenation of cyclohexyl acetate. Ethanol is the raw material of ethanol gasoline, and cyclohexanol is the raw material of nylon 6 and nylon 66. The industrial application prospect of cyclohexyl acetate is broad. [0003] Before the 1980s, cyclohexyl acetate was synthesized by the reaction of cyclohexanol and acetic acid, and the output was low cost, which was not suitable fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04C07C67/54C07C13/18C07C7/06
CPCC07C7/06C07C67/04C07C67/54C07C69/14C07C13/18
Inventor 吴明旷志刚孙琦王英平王卉谯荣焦岳飞
Owner CHINA PETROLEUM & CHEM CORP
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