CN113372297B - Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water - Google Patents
Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water Download PDFInfo
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- CN113372297B CN113372297B CN202110707055.6A CN202110707055A CN113372297B CN 113372297 B CN113372297 B CN 113372297B CN 202110707055 A CN202110707055 A CN 202110707055A CN 113372297 B CN113372297 B CN 113372297B
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- hexanol
- piperazine
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- water
- ethanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/023—Preparation; Separation; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/027—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for treating mixed liquor containing ethanol, piperazine, n-hexanol and water, which comprises the following steps: and (2) carrying out rectification separation on the mixed solution in a first rectification tower to obtain a first material containing ethanol and water at the tower top, obtaining a second material containing piperazine and n-hexanol at the tower bottom, extracting the second material, carrying out reduced pressure rectification in a second rectification tower to obtain a piperazine product at the tower top, and obtaining an n-hexanol product at the tower bottom. The treatment process can be used for respectively extracting and recovering the ethanol, the piperazine, the n-hexanol and the water from the mixed solution of the ethanol, the piperazine, the n-hexanol and the water, and the obtained product has high purity and can be used for treating the wastewater containing the substances in the pharmaceutical industry.
Description
Technical Field
The invention relates to a method for treating a mixed solution containing ethanol, piperazine, n-hexanol and water.
Background
Piperazine in ethanol-piperazine-n-hexanol-water waste liquid generated in the pharmaceutical industry is easy to dissolve in water, water-ethanol and water-n-hexanol are azeotropic, and can not be separated by common rectification. Therefore, the separation can not be realized by adopting the common rectification.
Disclosure of Invention
The invention mainly aims to provide a method for treating a mixed solution which can contain ethanol, piperazine, n-hexanol and water.
In order to achieve the above object, the present invention provides a method for treating a mixed solution containing ethanol, piperazine, n-hexanol and water, comprising the steps of:
rectifying and separating the mixed solution in a first rectifying tower to obtain a first material containing ethanol and water at the tower top and a second material containing piperazine and n-hexanol at the tower bottom,
and performing reduced pressure rectification on the extracted second material in a second rectification tower to obtain a piperazine product at the tower top and obtain a n-hexanol product at the tower bottom.
In some embodiments, the first material is purified to obtain a higher purity ethanol product.
In some embodiments, the first rectification column is operated at atmospheric pressure, an overhead temperature of 78.3 ℃, a kettle temperature of 150.4 ℃, and a reflux ratio of 1.
In some embodiments, the operating conditions of the second rectification column are: the pressure is 5kpa, the overhead temperature is 66.56 ℃, the bottom temperature is 80.09 ℃, and the reflux ratio is 3.
The treatment process can be used for respectively extracting and recovering the ethanol, the piperazine, the n-hexanol and the water from the mixed solution of the ethanol, the piperazine, the n-hexanol and the water, and the obtained product has high purity and can be used for treating the wastewater containing the substances in the pharmaceutical industry.
Drawings
FIG. 1 is a schematic process flow diagram of the mixed solution of ethanol, piperazine, n-hexanol and water in the example.
Detailed Description
The rectifying tower in this embodiment includes not only the tower body, but also relevant corollary equipment and instrumentation systems, such as a relevant pump, a pipeline, a valve, a control system, etc., configured for the rectifying tower body to achieve rectification.
In the embodiment, the conveying of each material can be controlled by adopting pipelines, pumps, valves and control systems, and the temperature of the material can be adjusted by various heaters, heat exchangers and other equipment.
The contents in the present example are weight percentages unless otherwise specified.
The invention relates to a method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water, which mainly comprises the following steps:
rectifying and separating the mixed solution in a first rectifying tower to obtain a first material containing ethanol and water at the tower top and a second material containing piperazine and n-hexanol at the tower bottom,
and performing reduced pressure rectification on the extracted second material in a second rectification tower to obtain a piperazine product at the tower top and obtain a n-hexanol product at the tower bottom.
The invention is further described with reference to the following figures and examples.
The mixed liquor treated in the embodiment contains 62% of ethanol, 20% of piperazine, 15% of n-hexanol and 3% of water, the mixed liquor enters a first rectifying tower for primary separation, the flow rate of the fed mixed liquor is 1000kg/h, the operating conditions of the first rectifying tower are normal pressure, the tower top temperature is 78.3 ℃, the tower bottom temperature is 150.4 ℃, the reflux ratio is 1, the tower top discharge of the first rectifying tower is a first material containing 95.37% of ethanol, 4.615% of water and 0.015% of piperazine, the flow rate is 650.1kg/h, the tower bottom discharge is a second material containing 57.13% of piperazine and 42.87% of n-hexanol, and the flow rate is 349.9 kg/h.
And (2) feeding the second material into a second rectifying tower for further rectification under reduced pressure, wherein the flow rate of the second material is 349.9kg/h, and the operating conditions of the second rectifying tower are as follows: the pressure is 5kpa, the overhead temperature is 66.56 ℃, the temperature of a tower bottom is 80.09 ℃, the reflux ratio is 3, the material discharged from the tower top of the second rectifying tower is piperazine with the content of 99.9998%, the impurity is trace n-hexanol, the flow is 199.9kg/h, the material discharged from the tower bottom of the second rectifying tower is n-hexanol with the content of 99.9994%, the impurity is trace piperidine, and the flow is 150kg/h.
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 treatment method of mixed liquid containing ethanol, piperazine, n-hexanol and water is characterized by comprising the following steps:
rectifying and separating the mixed solution in a first rectifying tower to obtain a first material containing ethanol and water at the tower top and a second material containing piperazine and n-hexanol at the tower bottom,
and performing reduced pressure rectification on the extracted second material in a second rectification tower to obtain a piperazine product at the tower top and obtain a n-hexanol product at the tower bottom.
2. The method according to claim 1, wherein the first material is purified to obtain a higher purity ethanol product.
3. The method according to claim 1, wherein the first distillation column is operated under normal pressure, at an overhead temperature of 78.3 ℃, at a bottom temperature of 150.4 ℃ and at a reflux ratio of 1.
4. The method according to claim 1, wherein the second distillation column is operated under the following conditions: the pressure is 5kpa, the overhead temperature is 66.56 ℃, the bottom temperature is 80.09 ℃, and the reflux ratio is 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110707055.6A CN113372297B (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110707055.6A CN113372297B (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113372297A CN113372297A (en) | 2021-09-10 |
| CN113372297B true CN113372297B (en) | 2023-01-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110707055.6A Active CN113372297B (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332727A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Recovery and purification method of ethanol-n-hexanol-piperazine aqueous solution |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5897750A (en) * | 1997-08-28 | 1999-04-27 | Berg; Lloyd | Separation of acetone from isopropanol-water mixtures by extractive distillation |
| DE10101942A1 (en) * | 2001-01-17 | 2002-07-18 | Basf Ag | Separating azeotropic mixtures, e.g. of butanol and perchloroethylene from ascorbic acid production, involves distillation with substance which forms lower-boiling azeotropes to give fractions rich in each component |
| CN102977055B (en) * | 2012-11-21 | 2015-10-28 | 西安近代化学研究所 | A kind of separation method of piperazine |
| CN104230850B (en) * | 2013-06-17 | 2016-04-13 | 中国石油化工股份有限公司 | The separation method of piperazine |
| CN107970632A (en) * | 2016-10-21 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of azeotropic distillation separator and n-hexyl alcohol azeotropic distillation separation method and its application |
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