Unlock instant, AI-driven research and patent intelligence for your innovation.

Device and method for separating acetonitrile-water-methanol mixture

A separation device and mixture technology, which are used in the purification/separation of carboxylic acid nitrile, the preparation of organic compounds, chemical instruments and methods, etc. problem, to achieve the effect of high safety performance, simple structure and low energy consumption

Active Publication Date: 2013-11-13
SUN YAT SEN UNIV +1
View PDF4 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to prevent these mixtures from causing damage to the environment, recovery is usually carried out, and the recovery of the mixture after recovery can be applied here; however, no matter whether it is a two-component mixture or a three-component mixture, it is easy to form an azeotrope under normal pressure, so Difficult to separate by ordinary rectification methods
[0005] The separation of the two-component mixture of methanol and acetonitrile is mainly separated by pressure swing rectification. The separation effect of pressure swing rectification is better, but the cost of pressure swing rectification is high, and the temperature of the vacuum tower is too low. consumes a lot of energy
Chinese patent application CN102068831A discloses a batch extraction and rectification separation method of acetonitrile-methanol azeotropic mixture. The extraction and rectification method of adding DMF is used to separate acetonitrile-methanol azeotropic mixture. Although the problem of energy consumption is solved, DMF has relatively High toxicity, potential safety hazard, unfavorable for industrial promotion and application
[0006] For the separation of methanol, acetonitrile and water three-component mixture, it is difficult to achieve the separation effect by pressure swing rectification; since water, methanol and DMF are all miscible, the above method cannot be used to separate the three-component mixture
So far, there is no method for separating the mixture of methanol, acetonitrile and water, so a large part is sold to waste reagent recycling companies for incineration, but acetonitrile incineration is prone to produce highly toxic hydrogen cyanide, which is harmful to environmental damage

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Device and method for separating acetonitrile-water-methanol mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Using the above separation device, add 20kg of waste liquid and 5kg of dichloromethane into the still of the rectification column, close the first control valve, the second control valve and the liquid stop valve at the same time, start stirring, and slowly raise the temperature; Reflux for 0.5 hours, the top temperature is 38°C, start discharging, after being condensed by the condensation tower, separate layers at the bottom of the condensation tower, open the first control valve and the second control valve to recover methanol, and reflux dichloromethane, and control the reflux ratio to 1.2; After the methanol phase is discharged, close the first control valve and the second control valve, raise the temperature to 70°C again, take a fraction at 50-51°C, open the liquid stop valve to recover additives, after the recovery is completed, cool down to room temperature, close the liquid stop valve, Add 0.1 kg of NaCl to the still tower, raise the temperature to 90°C, top tem...

Embodiment 2

[0038]Using the above separation device, add 20kg of waste liquid and 6.5kg of dichloromethane to the still of the rectification column, close the first control valve, the second control valve and the liquid stop valve at the same time, start stirring, and slowly raise the temperature; it starts boiling at 50°C, Total reflux for 0.5 hours, the top temperature is 38°C, start to discharge the material, after condensing through the condensation tower, stratify at the bottom of the condensation tower, open the first control valve and the second control valve to recover methanol, and reflux dichloromethane, control the reflux ratio of 1.2 ; After the methanol phase is discharged, close the first control valve and the second control valve, heat up to 70°C again, take a fraction of 50-51°C, open the liquid stop valve to recover additives, after the recovery is completed, cool down to room temperature, and close the liquid stop valve , add 0.1kg of NaCl to the still tower, raise the te...

Embodiment 3

[0040] Using the above separation device, add 20kg of waste liquid and 4kg of dichloromethane into the still of the rectification column, close the first control valve, the second control valve and the liquid stop valve at the same time, start stirring, and slowly raise the temperature; Reflux for 0.5 hours, the top temperature is 38°C, start discharging, after being condensed by the condensation tower, separate layers at the bottom of the condensation tower, open the first control valve and the second control valve to recover methanol, and reflux dichloromethane, and control the reflux ratio to 1.2; After the methanol phase is discharged, close the first control valve and the second control valve, raise the temperature to 70°C again, take a fraction at 50-51°C, open the liquid stop valve to recover additives, after the recovery is completed, cool down to room temperature, close the liquid stop valve, Add 0.1 kg of NaCl to the still tower, raise the temperature to 90°C, top tem...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a device and a method for separating an acetonitrile-water-methanol mixture. The separating device comprises a heating device, a temperature measurement couple, a rectification tower and a product collection tank. The rectification tower, which is located in the heating device, comprises a tower bottom, in which the temperature measurement couple is arranged, a rectification section connected to the tower bottom, a condensing tower above the rectification section, and a liquid transfer tube. The separating method utilizes the device and the differences of solubilities of all components of the mixture in dichloromethane to remove methanol first, the dichloromethane in the lower layer flows back into the rectification tower, and sodium chloride is added into the remaining mixture of acetonitrile and water for breaking and separating the azeotrope to obtain the acetonitrile and the water. The separating device is simple in structure, easy to operate, low in energy consumption, and suitable for industrial production. The device and the method achieve separation of acetonitrile, water and methanol with low costs and energy consumption, and are environmentally friendly and convenient for applications.

Description

[0001] technical field [0002] The invention relates to a separation process of a mixture, in particular to a separation device and a separation method of an acetonitrile-water-methanol mixture. [0003] Background technique [0004] Methanol and acetonitrile are important chemical raw materials and solvents, and they are also important mobile phases in liquid chromatography detection. Therefore, it is easy to produce a mixture of methanol and acetonitrile or a mixture of methanol, acetonitrile and water in the process of chemical production and detection. mixture of components. In order to prevent these mixtures from causing damage to the environment, recovery is usually carried out, and the recovery of the mixture after recovery can be applied here; however, no matter whether it is a two-component mixture or a three-component mixture, it is easy to form an azeotrope under normal pressure, so It is difficult to separate by ordinary distillation methods. [0005] The sep...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): B01D3/36C07C31/04C07C29/82C07C255/03C07C253/34
Inventor 王崇晓朱龙平黄世亮王永理
Owner SUN YAT SEN UNIV
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More