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Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture

An azeotrope, extractive distillation technology, applied in extractive distillation, chemical instruments and methods, carboxylic acid nitrile purification/separation and other directions, to achieve the effect of reducing equipment cost, easy control, and short process flow

Inactive Publication Date: 2012-11-21
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 3) The extraction and rectification solvent cannot chemically react with the separated components;

Method used

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  • Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Such as figure 1 The diagram of the device is shown. according to figure 1 Install the extractive distillation tower, the height of the effective packing tower is 200cm, the methanol content is 75% acetonitrile-methanol mixed solution 1000ml is added to the tower kettle, measure 1000ml extraction agent N, N-dimethylformamide is added in the head tank; Total reflux operation without extractant: the top condenser is fed with cooling water, the tower kettle is heated, and when the liquid in the tower kettle starts to boil, the heating input power is slowly increased. Maintain normal operating conditions. Total reflux operation, until the whole tower is in a stable state, keep the pressure drop at the top and bottom of the tower at 300Pa, and continue the total reflux for 1h. Total reflux operation with extraction agent added: After the total reflux is stable, add the extractant N,N-dimethylformamide into the tower at a solvent ratio of 1:1, and perform total reflux oper...

Embodiment 2

[0038] Such as figure 1 The diagram of the device is shown. according to figure 1Install the extractive distillation tower, the height of the effective packing tower is 200cm, the methanol content is 75% acetonitrile-methanol mixed solution 1000ml is added to the tower kettle, measure 1000ml extraction agent N, N-dimethylformamide is added in the head tank; Total reflux operation without extractant: the top condenser is fed with cooling water, the tower kettle is heated, and when the liquid in the tower kettle starts to boil, the heating input power is slowly increased. Maintain normal operating conditions. Total reflux operation, until the whole tower is in a stable state, keep the pressure drop at the top and bottom of the tower at 300Pa, and continue the total reflux for 1h. Total reflux operation with extraction agent added: After the total reflux is stable, add the extractant N, N-dimethylformamide into the tower at a solvent ratio of 2:1, and perform total reflux oper...

Embodiment 3

[0040] Such as figure 1 The diagram of the device is shown. according to figure 1 Install the extractive distillation tower, the height of the effective packing tower is 200cm, the methanol content is 75% acetonitrile-methanol mixed solution 1000ml is added to the tower kettle, measure 1000ml extraction agent N, N-dimethylformamide is added in the head tank; Total reflux operation without extractant: the top condenser is fed with cooling water, the tower kettle is heated, and when the liquid in the tower kettle starts to boil, the heating input power is slowly increased. Maintain normal operating conditions. Total reflux operation, until the whole tower is in a stable state, keep the pressure drop at the top and bottom of the tower at 300Pa, and continue the total reflux for 1h. Total reflux operation with extractant added: After the total reflux is stable, add the extractant N,N-dimethylformamide into the tower at a solvent ratio of 3:1, and perform total reflux operation ...

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PUM

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Abstract

The invention discloses a batch extractive distillation device and separation method for an acetonitrile-methanol azeotropic mixture. The device disclosed by the invention comprises an electrical heating sleeve, a tower kettle, a temperature thermocouple, an extractive distillation tower, a condenser, a head tank, a product collection tank, a rotameter and a U-shaped differential pressure gauge. The method is implemented through the following steps: carrying out extractive distillation operation in the extractive distillation tower; carrying out total-reflux operation in the absence of an extracting agent; carrying out total-reflux operation in the presence of the extracting agent; and carrying out product extraction and solvent recovery operations in a constant reflux ratio. The product purities of separated acetonitrile and methanol are high, and the process flow is short, the equipment investment is less, and the operation method is simple and convenient to control, therefore, the batch extractive distillation device and separation method disclosed by the invention are suitable for acetonitrile-methanol azeotropic mixtures mixed in any proportion. Because extractive distillation is utilized to replace varying-voltage distillation, on one hand, the equipment cost is reduced, and on the other hand, the energy consumption is effectively reduced.

Description

technical field [0001] The invention relates to a batch extraction and rectification device and separation method for acetonitrile-methanol azeotropic mixture. Background technique [0002] Acetonitrile and methanol are two important organic solvents, which are widely used in chemical, pharmaceutical and other fields. But the two form an azeotrope under normal pressure, the azeotropic composition is 79%-80% (wt) containing methanol, and the azeotropic temperature is 63.4-63.7 ° C, so it is difficult to effectively separate it by ordinary rectification methods. [0003] At present, the separation method of acetonitrile-methanol azeotrope is mainly the method of pressure swing rectification. Chinese patent CN101134736A proposes separation of acetonitrile-methanol azeotrope by pressure swing rectification. However, the cost of pressure swing rectification equipment is high, and the temperature of the vacuum column bottom is too low, so the energy consumption is huge. [0004...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/40C07C255/03C07C253/34C07C31/04C07C29/84
Inventor 白鹏于洋张锦威肖颖
Owner TIANJIN UNIV