CN113372242A - Purification method of water-containing acetonitrile - Google Patents
Purification method of water-containing acetonitrile Download PDFInfo
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- CN113372242A CN113372242A CN202110706965.2A CN202110706965A CN113372242A CN 113372242 A CN113372242 A CN 113372242A CN 202110706965 A CN202110706965 A CN 202110706965A CN 113372242 A CN113372242 A CN 113372242A
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- acetonitrile
- water
- tower
- stripping
- containing acetonitrile
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
The invention relates to a purification method of water-containing acetonitrile, wherein the water-containing acetonitrile is subjected to steam stripping in a stripping tower, a first material containing acetonitrile with higher concentration is obtained at the top of the tower, and the first material is subjected to water removal through a vaporization film to obtain an acetonitrile product. The purification method of the invention can purify the water-containing acetonitrile containing only a small amount of acetonitrile to obtain the acetonitrile product with high purity.
Description
Technical Field
The invention relates to a method for purifying water-containing acetonitrile.
Background
Acetonitrile is typically nitrile-reactive and is used to prepare many typical nitrogen-containing compounds, an important organic intermediate. Acetonitrile can be used for synthesizing solvents of vitamin A, cortisone, carbon amine drugs and intermediates thereof, and also can be used for preparing active medium solvents of vitamin B1 and amino acid.
The low-energy acetonitrile wastewater generated in the production process contains high-concentration water, so that the acetonitrile is recovered by a rectification evaporation process, the steam consumption is high, and the treatment cost is high; the waste water is concentrated and purified by a liquid-liquid extraction process, so that the steam consumption can be reduced, but a third-party solvent is introduced as an extracting agent, so that potential danger of third-party material pollution exists, and the application range of the recovered acetonitrile is limited.
Disclosure of Invention
The invention mainly aims to overcome the defects of the acetonitrile recovery process and provide an economic and technically mature method for purifying low-concentration water-containing acetonitrile.
In order to achieve the above object, the present invention provides a method for purifying aqueous acetonitrile, comprising the steps of:
steam stripping the water-containing acetonitrile in a stripping tower to obtain a first material containing acetonitrile with higher concentration at the top of the tower,
and (3) dehydrating the first material through a vaporization film to obtain an acetonitrile product.
In some embodiments, the operating conditions of the stripping column are: the operation pressure is normal pressure, the tower top temperature is 80-90 ℃, the tower bottom temperature is 90-100 ℃, the number of tower plates is 5-20, and the steam pressure is 1-101 kPa.
In some embodiments, the stripper column has an overhead temperature of 86.6 deg.C, a kettle temperature of 100 deg.C, a tray number of 10, and a steam pressure of 5 kPa.
In some embodiments, permeate condensate after water removal by the vaporization membrane is refluxed to a stripping column for stripping.
The purification method of the invention can purify the water-containing acetonitrile containing only a small amount of acetonitrile to obtain the acetonitrile product with high purity.
Drawings
FIG. 1 is a schematic flow diagram of aqueous acetonitrile purification.
Detailed Description
The stripping tower in the embodiment comprises a tower body, and also comprises related corollary equipment and instrument systems such as related pumps, pipelines, valves and control systems which are configured for the stripping tower body to realize rectification.
In this embodiment, the transportation of each material may be controlled by a pipeline, a pump, a valve, and a control system, and the temperature of the material may be adjusted by various heaters, heat exchangers, and other devices.
The contents in the present example are weight percentages unless otherwise specified.
The invention relates to a method for purifying water-containing acetonitrile, which mainly comprises the following steps:
steam stripping the water-containing acetonitrile in a stripping tower to obtain a first material containing acetonitrile with higher concentration at the top of the tower,
and (3) dehydrating the first material through a vaporization film to obtain an acetonitrile product.
The invention is further described with reference to the following figures and examples.
The aqueous acetonitrile treated in this example contains 3% acetonitrile and 97% water, and is fed into a stripping tower for stripping to increase the concentration of acetonitrile in water, wherein the feed flow rate of the aqueous acetonitrile is 1000kg/h, the steam pressure for stripping is 5kPaG, the feed flow rate is 160kg/h, and the operating conditions of the stripping tower are as follows: the operation pressure is normal pressure, the top temperature of the tower is 86.6 ℃, the bottom temperature of the tower is 100 ℃, the number of plates is 10, the top discharge of the stripping tower is a first material containing 61.99% of acetonitrile and 38.01% of water, the bottom discharge of the tower is wastewater containing 0.0039% of acetonitrile and 99.9961% of water, the flow rate is 1111.67kg/h, the first material can be subjected to water removal through a vaporization membrane to obtain an acetonitrile product, and the permeate condensate of the vaporization membrane can flow back to the stripping tower to be stripped together with the water-containing acetonitrile.
The embodiments of the present invention are merely illustrative, and not restrictive, of the scope of the claims, and other substantially equivalent alternatives may occur to those skilled in the art and are within the scope of the present invention.
Claims (4)
1. A method for purifying water-containing acetonitrile is characterized by comprising the following steps:
steam stripping the water-containing acetonitrile in a stripping tower to obtain a first material containing acetonitrile with higher concentration at the top of the tower,
and (3) dehydrating the first material through a vaporization film to obtain an acetonitrile product.
2. The purification process of claim 1, wherein the stripping column is operated under the following conditions: the operation pressure is normal pressure, the tower top temperature is 80-90 ℃, the tower bottom temperature is 90-100 ℃, the number of tower plates is 5-20, and the steam pressure is 1-101 kPa.
3. The purification process according to claim 2, wherein the temperature at the top of the stripping column is 86.6 ℃, the temperature at the bottom of the stripping column is 100 ℃, the number of plates is 10, and the steam pressure is 5 kPa.
4. The purification process of claim 1, wherein permeate condensate after water removal from the vaporization membrane is returned to the stripping column for stripping.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110706965.2A CN113372242A (en) | 2021-06-24 | 2021-06-24 | Purification method of water-containing acetonitrile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110706965.2A CN113372242A (en) | 2021-06-24 | 2021-06-24 | Purification method of water-containing acetonitrile |
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| Publication Number | Publication Date |
|---|---|
| CN113372242A true CN113372242A (en) | 2021-09-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110706965.2A Pending CN113372242A (en) | 2021-06-24 | 2021-06-24 | Purification method of water-containing acetonitrile |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180756A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Acetonitrile waste liquid purification and recovery device and method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4294665A (en) * | 1979-02-02 | 1981-10-13 | Asahi Kasei Kogyo Kabushiki Kaisha | Separation of acetonitrile from crude olefinically unsaturated nitrile |
| US4404064A (en) * | 1982-12-30 | 1983-09-13 | Monsanto Company | Water extractive distillation of olefinically unsaturated nitriles |
| US4444571A (en) * | 1983-03-07 | 1984-04-24 | Bend Research, Inc. | Energy-efficient process for the stripping of gases from liquids |
| CN103224456A (en) * | 2013-04-08 | 2013-07-31 | 江苏九天高科技股份有限公司 | Process and device for refining acetonitrile with a pervaporation method |
| CN112159337A (en) * | 2020-10-30 | 2021-01-01 | 广西科伦制药有限公司 | System and method for recycling acetonitrile from cephalosporin medicine intermediate |
-
2021
- 2021-06-24 CN CN202110706965.2A patent/CN113372242A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4294665A (en) * | 1979-02-02 | 1981-10-13 | Asahi Kasei Kogyo Kabushiki Kaisha | Separation of acetonitrile from crude olefinically unsaturated nitrile |
| US4404064A (en) * | 1982-12-30 | 1983-09-13 | Monsanto Company | Water extractive distillation of olefinically unsaturated nitriles |
| US4444571A (en) * | 1983-03-07 | 1984-04-24 | Bend Research, Inc. | Energy-efficient process for the stripping of gases from liquids |
| CN103224456A (en) * | 2013-04-08 | 2013-07-31 | 江苏九天高科技股份有限公司 | Process and device for refining acetonitrile with a pervaporation method |
| CN112159337A (en) * | 2020-10-30 | 2021-01-01 | 广西科伦制药有限公司 | System and method for recycling acetonitrile from cephalosporin medicine intermediate |
Non-Patent Citations (2)
| Title |
|---|
| 崔明珍: "《废弃物化学组分的毒理和处理技术》", 30 November 1993, 中国环境科学出版社 * |
| 王彦斌等: "《化工环境污染与防治》", 31 July 2000, 民族出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180756A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Acetonitrile waste liquid purification and recovery device and method |
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