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Method for producing cyclohexyl acetate through reaction rectification

A technology of cyclohexyl acetate and reactive distillation, which is applied in the field of reactive distillation to prepare cyclohexyl acetate, can solve the problems of high cost, unsuitability for large-scale industrial production, and low output, so as to prolong life, avoid side reactions, The effect of reducing by-products

Active Publication Date: 2018-04-20
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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  • Method for producing cyclohexyl acetate through reaction rectification
  • Method for producing cyclohexyl acetate through reaction rectification
  • Method for producing cyclohexyl acetate through reaction rectification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] In this process, the circulating mass flow rate of the solvent divided by the raw material feed mass flow rate is set to 1;

[0045] Reactive distillation column start-up test

[0046] step one

[0047] Under normal pressure, add solvent hexanaphthene from feed inlet 10, set up tower still liquid level 60%, tower still heats up, set up tower top reflux tank 5 cyclohexane liquid level 40%, start tower top reflux pump 6, tower top The cyclohexane pumped back by the reflux pump 6 enters the rectifying section 3 through the second interface 12 and establishes a total reflux of the reactive distillation tower, with a reflux rate of 4 kg / h;

[0048] step two

[0049] Add acetic acid from the feed port (10) at a flow rate of 3kg / h, and gradually increase the temperature of the tower kettle to 118°C, the temperature of the stripping section is 90°C, and the temperature of the reaction section and rectification section is 79-81°C;

[0050] step three

[0051] Control cyclohe...

Embodiment 2

[0053] In this process, the circulating mass flow rate of the solvent divided by the raw material feed mass flow rate is set to 3;

[0054] Reactive distillation column start-up test

[0055] The first step: under normal pressure, add cyclohexane from the first feed port, establish the liquid level of the tower kettle to 60%, raise the temperature of the tower kettle, set up the top reflux tank 5 cyclohexane liquid level 50%, start the top reflux pump 6. The cyclohexane pumped back by the tower top reflux pump 6 enters the rectification section 3 through the second interface 12 and establishes a total reflux of the reactive distillation column with a reflux rate of 10kg / h;

[0056] The second step: add acetic acid from the feed port (10) at a flow rate of 5kg / h, gradually increase the temperature of the tower kettle to 118°C, the temperature of the stripping section is 85°C, and the temperature of the reaction section and rectifying section is 79-81°C.

[0057] The 3rd step: ...

Embodiment 3

[0059] Using n-hexane instead of cyclohexane, the test process is the same as in Example 1. When the device is running stably, in step 3, the temperature of the tower kettle is 125°C, the temperature of the stripping section is 78°C, the temperature of the reaction section is 73-75°C, and the temperature of the rectifying section is 65°C. ~66°C, continuous operation for 240 hours, the yield of cyclohexyl acetate is greater than 99.8%.

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Abstract

The invention relates to a method for producing cyclohexyl acetate through reaction rectification, and belongs to the field of petrochemical technology development. According to the present invention,cyclohexene and acetic acid are used as raw materials, alkane or cycloalkane with a boiling point of A DEG C is used as a solvent, the raw materials and the solvent are added to a reaction rectification tower, the circulation mass of the solvent and the feed mass flow of the raw materials are controlled, a reaction is performed at a temperature of B DEG C to obtain cyclohexyl acetate, the value of A is 50-110, the value of B is greater than or equal to A and less than or equal to 110, and a ratio of the circulation mass flow of the solvent to the feed mass flow of the raw materials is more than or equal to 0.5; and the method has advantages of simple process, strong parameter controllability, easy separation of the obtained product, less by-products and long service life of the catalyst,and is suitable for large-scale industrial application.

Description

technical field [0001] The invention relates to a method for preparing cyclohexyl acetate by reactive distillation, belonging 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 for large-scale industrial production; with ...

Claims

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Application Information

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IPC IPC(8): C07C67/04C07C67/54C07C69/14
CPCC07C67/04C07C67/54C07C69/14
Inventor 吴明旷志刚狄金凤管健王卉谯荣
Owner CHINA PETROLEUM & CHEM CORP
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