CN113461476A - Method for treating mixed liquid containing petroleum ether and ethyl acetate - Google Patents
Method for treating mixed liquid containing petroleum ether and ethyl acetate Download PDFInfo
- Publication number
- CN113461476A CN113461476A CN202110706997.2A CN202110706997A CN113461476A CN 113461476 A CN113461476 A CN 113461476A CN 202110706997 A CN202110706997 A CN 202110706997A CN 113461476 A CN113461476 A CN 113461476A
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- Prior art keywords
- ethyl acetate
- phase separation
- petroleum ether
- phase
- temperature
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for treating mixed liquid containing petroleum ether and ethyl acetate, which comprises the following steps: the method comprises the steps of extracting and phase-splitting the mixed solution and ethylene glycol in a phase-splitting tank, obtaining a petroleum ether product in a light phase, obtaining a first material containing ethylene glycol and ethyl acetate in a heavy phase, rectifying the first material in a rectifying tower, and obtaining an ethyl acetate product at the top of the tower.
Description
Technical Field
The invention relates to a separation method of a mixture, in particular to a treatment method of a mixed solution containing petroleum ether and ethyl acetate.
Background
In the pharmaceutical field, petroleum ether/ethyl acetate is largely used as a chromatography developing agent, and a large amount of related mixed solvent mixed liquor is generated. Therefore, the method has important practical significance for effectively separating the mixed waste liquid of petroleum ether and ethyl acetate and realizing recycling.
Disclosure of Invention
The invention mainly aims to provide a recyclable method for separating petroleum ether from ethyl acetate.
In order to achieve the above object, the present invention provides a method for treating a mixed solution containing petroleum ether and ethyl acetate, comprising the steps of:
extracting the mixed solution and glycol in a phase separation tank for phase separation to obtain petroleum ether product in light phase and first material containing glycol and ethyl acetate in heavy phase,
and the first material enters a rectifying tower for rectification, and an ethyl acetate product is obtained at the tower top.
In some embodiments, the bottom of the rectifying tower obtains a second material containing glycol, and the second material reflows to the phase separation tank for extraction phase separation.
In some embodiments, the operating pressure of the phase separation tank is atmospheric and the operating temperature is from 0 to 60 ℃.
In some embodiments, the operating temperature of the phase separation cell is 55 ℃.
In some embodiments, the operating conditions of the rectification column are: 1-101kpa, the temperature at the top of the tower is 15-80 ℃, the temperature at the bottom of the tower is 90-160 ℃, and the reflux ratio is 0.5-3.
In some embodiments, the rectification column has an overhead temperature of 72 ℃, a kettle temperature of 157 ℃ and a reflux ratio of 1.
In some embodiments, the mixed solution further comprises water, and the water is enriched in the heavy phase in the extraction separation phase and enters the rectification column along with the first material for rectification.
On the basis of separating petroleum ether and ethyl acetate, the method can effectively recover the glycol used for extraction phase separation, so that the glycol is recycled, the separation cost is reduced, and the separation process is green and sustainable.
Drawings
FIG. 1 is a schematic diagram of a process for the separation of petroleum ether and ethyl acetate.
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 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 phase separation tank in this embodiment is not limited to a strict tank body, and may be various devices for performing phase separation, such as a phase separation tower and a phase separation tank, and may further include related supporting devices and instrumentation systems, such as a related pump, a pipeline, an invention, and a control system, which are configured for the phase separation tank to perform phase separation.
The contents in the present example are weight percentages unless otherwise specified.
The invention relates to a method for treating mixed liquid containing petroleum ether and ethyl acetate, which mainly comprises the following steps:
extracting the mixed solution and glycol in a phase separation tank for phase separation to obtain petroleum ether product in light phase and first material containing glycol and ethyl acetate in heavy phase,
and the first material enters a rectifying tower for rectification, and an ethyl acetate product is obtained at the tower top.
The invention is further described with reference to the following figures and examples.
In this example, a mixed solution containing 65.2% of petroleum ether, 32.6% of ethyl acetate and 2.17% of water was treated, and the mixed solution was fed into a phase separation tank together with an ethylene glycol extractant to perform extraction and phase separation, wherein the feed rate of the mixed solution was 1000kg/h, the feed rate of ethylene glycol was 2500kg/h, the pressure in the phase separation tank was atmospheric pressure, the operation temperature was 55 ℃, the light phase discharge in the phase separation tank was a first stream containing 99.8% of petroleum ether and 0.2% of ethyl acetate, the flow rate was 641kg/h, and the heavy phase discharge was a first stream containing 11.4% of ethyl acetate, greater than 87.4% of ethylene glycol, 0.76% of water and less than 0.5% of petroleum ether, the flow rate was 2859 kg/h.
Feeding the first material into a rectifying tower to regenerate and recover the glycol extractant, wherein the feeding flow of the first material is 2859kg/h, and the operating conditions of the rectifying tower are as follows: normal pressure, tower top temperature of 72 ℃, tower bottom temperature of 157 ℃ and reflux ratio of 1. The top discharge of the rectifying tower is an ethyl acetate product containing 94.7% of ethyl acetate and 5.3% of water, and the bottom discharge of the rectifying tower is a second material containing 0.5% of petroleum ether, 0.1% of water and 99% of glycol. The second material can directly flow back to the phase separation tank to be used as an extractant.
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 (7)
1. A method for treating a mixed solution containing petroleum ether and ethyl acetate is characterized by comprising the following steps:
extracting the mixed solution and glycol in a phase separation tank for phase separation to obtain petroleum ether product in light phase and first material containing glycol and ethyl acetate in heavy phase,
and the first material enters a rectifying tower for rectification, and an ethyl acetate product is obtained at the tower top.
2. The method according to claim 1, wherein the second material containing ethylene glycol is obtained from the bottom of the rectifying column, and the second material is refluxed to the phase separation tank for extractive phase separation.
3. The method according to claim 1, wherein the operating pressure of the phase separation tank is normal pressure and the operating temperature is 0 to 60 ℃.
4. The method according to claim 3, wherein the operation temperature of the phase separation tank is 55 ℃.
5. The method according to claim 1, wherein the distillation column is operated under the following conditions: 1-101kpa, the temperature at the top of the tower is 15-80 ℃, the temperature at the bottom of the tower is 90-160 ℃, and the reflux ratio is 0.5-3.
6. The method according to claim 5, wherein the distillation column has a top temperature of 72 ℃ and a bottom temperature of 157 ℃ and a reflux ratio of 1.
7. The method according to claim 1, wherein the mixed solution further comprises water, and the water is concentrated in the heavy phase and enters the rectifying tower along with the first material for rectification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110706997.2A CN113461476A (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing petroleum ether and ethyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110706997.2A CN113461476A (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing petroleum ether and ethyl acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113461476A true CN113461476A (en) | 2021-10-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110706997.2A Pending CN113461476A (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing petroleum ether and ethyl acetate |
Country Status (1)
| Country | Link |
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| CN (1) | CN113461476A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4379028A (en) * | 1982-03-30 | 1983-04-05 | Lloyd Berg | Separation of ethyl acetate from ethanol and water by extractive distillation |
| CN101955427A (en) * | 2010-08-25 | 2011-01-26 | 南京师范大学 | Method for separating methyl acetate and methanol water solution through multistage cross flow liquid-liquid extraction |
-
2021
- 2021-06-24 CN CN202110706997.2A patent/CN113461476A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4379028A (en) * | 1982-03-30 | 1983-04-05 | Lloyd Berg | Separation of ethyl acetate from ethanol and water by extractive distillation |
| CN101955427A (en) * | 2010-08-25 | 2011-01-26 | 南京师范大学 | Method for separating methyl acetate and methanol water solution through multistage cross flow liquid-liquid extraction |
Non-Patent Citations (1)
| Title |
|---|
| 黄丽红等: "萃取精馏分离乙酸乙酯和正己烷的过程模拟", 《广东化工》 * |
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Application publication date: 20211001 |
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| RJ01 | Rejection of invention patent application after publication |