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Method for simultaneously separating and purifying racemic optical amyl alcohol, optical active amyl alcohol and isoamyl alcohol from fusel oil or mixed amyl alcohol and its equipment

An optically active and simultaneous separation technology, applied in the field of rectification, can solve the problems of increased investment in automatic control facilities, increased heat required for evaporation, and complicated extraction control process, achieving good separation and purification effects, reducing equipment investment, and improving The effect of separation and purification efficiency

Inactive Publication Date: 2003-09-24
SICHUAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1) Since the amount of extraction agent added is generally 50-100% of the raw material, not only the processing load of the tower will be increased, but also the diameter of the tower will be significantly increased, resulting in an increase in equipment investment
[0010] (2) Due to the addition of more extractants, the heat required for evaporation increases and the operating cost increases
[0011] (3) Due to the complexity of the extraction control process, the investment in its automatic control facilities has increased significantly
[0012] (4) Although high-purity optically active amyl alcohol can be obtained from the top of the tower, to obtain high-concentration isoamyl alcohol, a large amount of isoamyl alcohol and extractant must be rectified in another rectification tower, so that The process flow is lengthened and the operating cost is increased

Method used

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  • Method for simultaneously separating and purifying racemic optical amyl alcohol, optical active amyl alcohol and isoamyl alcohol from fusel oil or mixed amyl alcohol and its equipment
  • Method for simultaneously separating and purifying racemic optical amyl alcohol, optical active amyl alcohol and isoamyl alcohol from fusel oil or mixed amyl alcohol and its equipment
  • Method for simultaneously separating and purifying racemic optical amyl alcohol, optical active amyl alcohol and isoamyl alcohol from fusel oil or mixed amyl alcohol and its equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]In this embodiment, the diameter of the rectifying tower is 30mm, and the filler is stainless steel triangular wire filler of φ3.5×3.5, and the height of the filler layer is 140cm.

[0037] 600 grams of pretreated fusel oil (2-methyl-1-butanol content 10%) is introduced into such as figure 1 In the shown rectification kettle 1 with a certain amount of zeolite, then adjust the stabilized power supply 9 to slowly heat the raw materials in the rectification kettle 1 through the electric heating furnace 10 until the liquid floods, and carry out the liquid flooding operation for 30 minutes, and the liquid flooding Three times, 3 minutes each time, so that the packing layer 3 located on the packing carrying grid 2 in the rectification column 4 is fully wetted. Then adjust the voltage-stabilized power supply 9 to control the heating capacity of the electric heating furnace 10 so as to control the vaporization rate, maintain a constant vaporization rate, and carry out total refl...

Embodiment 2

[0041] In this embodiment, the diameter of the rectifying tower is 20mm, the packing is stainless steel triangular wire packing of φ2.5×2.5, and the packing layer height is 150cm.

[0042] The 2-methyl-1-butanol content obtained in Example 1 is 460 grams of mixed pentanols of 55% introduced figure 1 , 2 . In the device shown in 3 (because embodiment 1 has carried out the description of technological process to the device, so the following embodiments, including this embodiment, are all omitted), the temperature rises to make the raw material boil until liquid flooding, and carry out liquid flooding Operate for 25 minutes, flood three times, each time for 2 minutes; then carry out the first stage of total reflux operation for 0.5 to 1.5 hours; then in the range of controlling the reflux ratio of 5 to 10, distill light components and water from the top of the tower, And remove the water; then carry out the second stage of total reflux operation for 2 hours; after the system is ...

Embodiment 3

[0045] This embodiment adopts the device of embodiment 2. It is worth noting that the main purpose of this example is to pre-concentrate the 2-methyl-1-butanol in the mixed pentanol, so as to be used as a raw material for further rectification, which is beneficial to improve the overall efficiency of the entire separation and purification.

[0046] 570 grams of pretreated fusel oil (2-methyl-1-butanol content is 10%) is introduced figure 1 , 2 , In the device shown in 3, the temperature is raised to make the raw materials boil until they are flooded, and the flooding operation is performed for 40 minutes, and the flooding operation is performed three times, each time for 5 minutes, and then the first full reflux operation is performed for 0.5 to 1 hour, and then the reflux is controlled. The rectification operation is carried out for ratios 4 to 6, and fractions of different temperature sections are collected from the top of the tower. When the 2-methyl-1-butanol in the frac...

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Abstract

The present invention adopts single tower, on the basis of general precision rectification process adds flooding operation, its total reflux is implemented at twice, reflux ratio of 4-80, and betweentwo stages of total reflux the light component can be fractionized out from top of tower and the water content is removed. It provides the equipment for implementing the above-mentioned method. It istechnically characterized by adopting high-effective precision rectification filling material and electromagnetic needle pendulum reflux ratio control instrument, height of filling layer is 140-150 cm, its complete condenser is water-splitting complete condenser, and upper portion of filling layer and its middle portion are respectively equipped with returned liquor distributor and oblique cone ring baffle.

Description

1. Technical field [0001] The invention belongs to the technical field of rectification, and specifically relates to a method and a device for simultaneously separating and purifying from fusel oil or mixed amyl alcohol to obtain racemic optical amyl alcohol, optically active amyl alcohol and isoamyl alcohol. 2. Background technology [0002] Fusel oil is a by-product of alcohol and liquor produced by fermentation, and its main components are 3-methyl-1-butanol (commonly known as isoamyl alcohol), (S)-(-)-2-methyl-1-butanol Alcohol (also known as optically active pentanol, with left-handedness) and racemic 2-methyl-1-butanol (also known as racemic optical pentanol), etc. Among them, isoamyl alcohol is a widely used solvent and an important raw material for synthetic fragrances, and is also a raw material and intermediate for some important drugs. Optically active amyl alcohol is an important intermediate for the synthesis of chiral compounds, especially chiral liquid crysta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/80C07C31/02
Inventor 宋航付超童安渝毛成中刘代科李玉德
Owner SICHUAN UNIV
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