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Method for extracting, distilling and separating acetonitrile-phenylmethane by utilizing dividing-wall rectifying tower

A separation wall rectification column and extractive rectification technology are applied in the field of separation of acetonitrile-toluene azeotrope mixture, which can solve the problems of difficult separation, many transition fractions and high cost, and reduce energy consumption, equipment investment and equipment investment. and the effect of reducing energy consumption

Active Publication Date: 2010-09-15
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Acetonitrile and toluene are commonly used extraction agents in the pharmaceutical industry. The acetonitrile-toluene mixture produced in the production process is difficult to separate due to the azeotrope formed by acetonitrile-toluene. If it is not recovered, it will not only pollute the environment, but also increase production costs. Therefore It is of great significance to develop a separation method for acetonitrile-toluene azeotrope
[0003] ZL200510014635.8 and ZL200510014636.2 use batch extractive distillation and continuous extractive distillation to separate acetonitrile-toluene azeotropic mixture respectively, using propylbenzene, n-butylbenzene, isobutylbenzene, sec-butylbenzene, tert-butyl phenylbenzene, p-diethylbenzene or p-tert-butyltoluene, among these extractants, propylbenzene and acetonitrile are difficult to separate in the high-concentration section, so the energy consumption for obtaining high-purity acetonitrile products will be very high, except for p-diethyl Except for benzene, the rest of the extractants are mainly from the synthesis process, and the cost is very high
The batch extraction and rectification process is flexible in operation and low in equipment costs. It can realize the separation of acetonitrile and toluene and the recovery of the extractant in a batch rectification tower. However, there are many transitional fractions, the energy consumption is very large, and the purity of the obtained product is not high.
The product obtained by the continuous extraction and rectification process has high purity and relatively low energy consumption, but the investment in equipment is high

Method used

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  • Method for extracting, distilling and separating acetonitrile-phenylmethane by utilizing dividing-wall rectifying tower
  • Method for extracting, distilling and separating acetonitrile-phenylmethane by utilizing dividing-wall rectifying tower

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Raw materials (mass ratio: acetonitrile 80%, toluene 20%), extractant durene (99.9m%)

[0014] like figure 1 As shown, there are 50 theoretical plates in area I, 30 theoretical plates in area II, and 10 theoretical plates in area IV. After heating, the raw materials enter area I of the dividing wall rectification column, and the feeding position is the 30th theoretical plate , the extractant durene enters the sixth theoretical plate after being heated, high-purity acetonitrile is extracted from the top of the first area, toluene is extracted from the top of the second area, and the extractant is extracted from the bottom of the tower for recycling.

[0015] The operating conditions are as follows:

[0016] Pressure: 0.1MPa

[0017] The reflux ratio of zone I: 1.5:1

[0018] The reflux ratio of zone II: 2:1

[0019] Solvent ratio: 1:1

[0020] Acetonitrile toluene feed temperature: 60°C

[0021] Durene feed temperature: 90°C

[0022] The chromatographic analysis o...

Embodiment 2

[0039] Raw material (mass ratio: acetonitrile 80%, toluene 20%), extractant is propylbenzene (99.9m%)

[0040] like figure 1 As shown, there are 50 theoretical plates in area I, 30 theoretical plates in area II, and 10 theoretical plates in area IV. After heating, the raw materials enter area I of the dividing wall rectification column, and the feeding position is the 30th theoretical plate , the extractant propylbenzene enters the sixth theoretical plate after being heated, high-purity acetonitrile is extracted from the top of the first area, toluene is extracted from the top of the second area, and the extractant is extracted from the bottom of the tower for recycling.

[0041] The operating conditions are as follows:

[0042] Pressure: 0.1MPa

[0043] The reflux ratio of zone I: 3:1

[0044] The reflux ratio of zone II: 5:1

[0045] Solvent ratio: 3:1

[0046] Acetonitrile toluene feed temperature: 50°C

[0047] Propylene feed temperature: 80°C

[0048] Tower top pro...

Embodiment 3

[0065] Raw materials (mass ratio: acetonitrile 50%, toluene 50%), extractant durene (99.9m%)

[0066] like figure 1 As shown, there are 40 theoretical plates in area I, 20 theoretical plates in area II, and 10 theoretical plates in area IV. After heating, the raw materials enter area I of the dividing wall rectification column, and the feeding position is the 25th theoretical plate , the extractant durene enters the fifth theoretical plate after being heated, high-purity acetonitrile is extracted from the top of the I area, toluene is extracted from the top of the II area, and the extractant is extracted from the bottom of the tower for recycling.

[0067] The operating conditions are as follows:

[0068] Pressure: 0.1MPa

[0069] The reflux ratio of zone I: 0.5:1

[0070] The reflux ratio of zone II: 0.6:1

[0071] Solvent ratio: 0.8:1

[0072] Acetonitrile toluene feed temperature: 60°C

[0073] Durene feed temperature: 90°C

[0074] The chromatographic analysis of th...

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Abstract

The invention discloses a method for extracting, distilling and separating acetonitrile-phenylmethane by utilizing dividing-wall rectifying tower, which belongs to separation techniques for an acetonitrile-phenylmethane azeotropic mixture. In the method, durene (1,2,4,5-durene) is preferably used as an extracting agent, the adopted device is an extractive rectifying tower provided with a dividingwall, and a dividing wall is installed in the vertical direction of a common rectifying tower to divide the tower into four parts. Region I is an extractive rectifying region, and the main body of the region I is provided with a tower tray and a filler; a sealing plate is arranged between region II and region III; the region II is an extracting agent recovery region; and since the extracting agent can be more easily separated in general and the extracting agent recovery region requires a smaller number of theoretical plates as compared with the extractive rectifying region, the position of the sealing plate can be adjusted by controlling the quantity of the tower trays or the filler. Region III is not additionally provided with any tower tray or filler. Region IV is the common stripping section of the region I and the region II. The invention can separate out high-purity acetonitrile and phenylmethane by using accessible, cheap and efficient extracting agent through extractive rectification with a dividing wall. The method reduces the equipment investment and energy consumption by more than 20% as compared with the conventional continuous extractive rectification.

Description

technical field [0001] The invention relates to a partition wall extraction and rectification separation method of an acetonitrile-toluene azeotrope mixture, which belongs to the separation technology of the acetonitrile-toluene azeotrope mixture. Background technique [0002] Extractive distillation is a special distillation separation technology, which is suitable for the separation of azeotropic and near-boiling systems. The purpose of separation is achieved by continuously adding extractant to the top of the rectification tower to change the relative volatility between the original components. The selection of extractant is the key to extractive distillation. The dividing wall rectification column is a new type of column, which can realize the combination of extractive distillation and extractant recovery in one column. Acetonitrile and toluene are commonly used extraction agents in the pharmaceutical industry. The acetonitrile-toluene mixture produced in the production...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34C07C15/06C07C7/08B01D3/40
Inventor 周金波任海鸥王玫董炳利王小强王艳飞程中克苟文甲倪岩刘飞黄剑锋宋帮勇孔祥冰马应海张松显
Owner PETROCHINA CO LTD
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