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Method for producing high-purity optical isoamylol through decompression and rectification and technical process thereof

A technology of vacuum distillation and isoamyl alcohol, which is applied in the fields of chemical instruments and methods, organic chemistry, and the preparation of organic compounds, can solve the problems of complicated process, low separation efficiency, and high processing cost, so as to improve the purity and effect , The effect of reducing processing costs

Active Publication Date: 2013-11-13
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The present invention overcomes the deficiencies of the prior art, and proposes a method for producing high-purity optical isoamyl alcohol by vacuum distillation and its process flow. The production of high-purity optical isoamyl alcohol fundamentally solves the technical problems of low separation efficiency, complicated process and high processing cost in traditional separation methods by changing the relative volatility of the material to be separated.

Method used

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  • Method for producing high-purity optical isoamylol through decompression and rectification and technical process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Implementation Example 1: The optical isoamyl alcohol accounts for 10.42% in the raw material mixed isoamyl alcohol, and the isoamyl alcohol accounts for 89.53%. The other contents are impurities, and the temperature is 20°C. Carry out rectification under vacuum in the described rectification under vacuum according to the steps described above, the operating pressure of rectification under vacuum is an optimal pressure after optimization in the scope of 0.05-0.5atm, and the reflux ratio is 20:1, preheated to 60°C before entering the tower, the feed position is at 6 / 10 of the tower, the residence time of the raw material in the top condenser is 5s, and the residence time of the material in the vacuum distillation tower is 20s, The recovery percentage at the bottom of the tower is 25%, and the quality of the obtained product has an optical purity of isoamyl alcohol of 99.95%, and a purity of isoamyl alcohol of 99.98%.

Embodiment 2

[0046] Implementation example 2: The optical isoamyl alcohol accounts for 19.30% in the raw material mixed isoamyl alcohol, and the isoamyl alcohol accounts for 80.62%. The other contents are impurities, and the temperature is 20°C. Carry out rectification under vacuum in the described rectification under vacuum according to the steps described above, the operating pressure of rectification under vacuum is an optimal pressure after optimization in the scope of 0.05-0.5atm, and the reflux ratio is 18:1, preheated to 60°C before entering the tower, the feed position is at 6 / 10 of the tower, the residence time of the raw material in the top condenser is 5s, and the residence time of the material in the vacuum distillation tower is 22s, The recovery percentage at the bottom of the tower is 28%, and the quality of the product obtained has an optical purity of isoamyl alcohol of 99.96%, and a purity of isoamyl alcohol of 99.97%.

Embodiment 3

[0047] Implementation example 3: The optical isoamyl alcohol accounts for 30.11% in the raw material mixed isoamyl alcohol, and the isoamyl alcohol accounts for 69.85%. The other contents are impurities, and the temperature is 20°C. Carry out rectification under vacuum in the described rectification under vacuum according to the steps described above, the operating pressure of rectification under vacuum is an optimal pressure after optimization in the scope of 0.05-0.5atm, and the reflux ratio is 18:1, preheated to 65°C before entering the tower, the feed position is at 6 / 10 of the tower, the residence time of the raw material in the top condenser is 5s, and the residence time of the material in the vacuum distillation tower is 22s, The recovery percentage at the bottom of the tower is 30%, the quality of the obtained product is optical isoamyl alcohol purity 99.97%, and the purity of isoamyl alcohol is 99.97%.

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Abstract

The invention relates to a method for producing high-purity optical isoamylol through decompression and rectification. The method comprises the following steps of: lowering the operating pressure of input materials to be separated through a vacuum system by using a decompression and rectification tower and a tower-top condenser; increasing the relative volatility of optical isoamylol and isoamylol; dividing the optical isoamylol and isoamylol passed through the decompression and rectification tower into a gas-phase substance at the tower top and a liquid-phase substance at the tower bottom under the heat and mass transferring function; and setting a thermosyphon reboiler at the bottom of the decompression and rectification tower so that the gas-phase substance and liquid-phase substance flow back and are in reverse multistage contact. The invention solves the technical problems of low separation efficiency, complex process, high processing cost, and the like in the traditional separation method.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to a method for producing high-purity optical isoamyl alcohol through vacuum distillation and a process flow thereof. Background technique [0002] When alcohol is produced by fermentation, about 0.2-1.1% fusel oil is produced by-product, and the content of mixed amyl alcohol is 45-70%. The annual production of fermented alcohol in my country is about 2 million tons, so the annual production of fusel oil is nearly 10,000 tons. The recycling of fusel oil can not only be used as a high-quality raw material for high value-added fine chemical products, but also reduce environmental pollution, thereby achieving sustainable development. [0003] Fusel oil can now be easily processed into a high concentration of mixed pentanols containing 15-30% 2-methyl-1-butanol (commonly known as optical isoamyl alcohol) and the rest being 3-methyl Base-1-butanol (commonly know...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/125C07C29/80
Inventor 王英龙朱兆友杨晶巍
Owner QINGDAO UNIV OF SCI & TECH
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