CN113354517A - Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene - Google Patents
Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene Download PDFInfo
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- CN113354517A CN113354517A CN202110707033.XA CN202110707033A CN113354517A CN 113354517 A CN113354517 A CN 113354517A CN 202110707033 A CN202110707033 A CN 202110707033A CN 113354517 A CN113354517 A CN 113354517A
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- ethylene glycol
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- isopropanol
- dimethyl ether
- toluene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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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
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
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Abstract
The invention relates to a method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene, which comprises the following steps: and carrying out extractive distillation on the mixed solution and ethylene glycol to obtain a first material containing isopropanol and toluene at the tower top, obtaining a second material containing ethylene glycol dimethyl ether and ethylene glycol at the tower bottom, carrying out extractive distillation on the first material and ethylene glycol to obtain a toluene product at the tower top, obtaining a third material containing isopropanol and ethylene glycol at the tower bottom, rectifying the third material to obtain an isopropanol product at the tower top, rectifying the second material to obtain an ethylene glycol dimethyl ether product at the tower top. The treatment method can separate the ethylene glycol dimethyl ether, the isopropanol and the toluene from the mixed solution of the ethylene glycol dimethyl ether, the isopropanol and the toluene respectively, the ethylene glycol obtained by extraction and rectification can be recycled in the whole system, and the method can be used for treating wastewater containing related components in the fields of various polymer chemistry, electrochemistry and boronization chemical processes.
Description
Technical Field
The present invention relates to a method for treating a mixed liquid containing ethylene glycol dimethyl ether, isopropyl alcohol and toluene.
Background
The glycol dimethyl ether is mainly used in the technical fields of polymer chemistry, electrochemistry and boron chemistry, and also used as a solvent of resin, nitrocellulose and the like, a medical extraction agent and an organic synthesis intermediate. In the waste liquid of glycol dimethyl ether-isopropanol-toluene generated in the bio-pharmaceutical industry, toluene and isopropanol are azeotropic, and the boiling points of the glycol dimethyl ether and the isopropanol are very close to each other, so that the glycol dimethyl ether and the isopropanol cannot be separated by adopting common rectification.
Disclosure of Invention
The invention mainly aims to provide a method capable of treating a mixed liquid of ethylene glycol dimethyl ether, isopropanol and toluene.
In order to achieve the above object, the present invention provides a method for treating a mixed solution containing ethylene glycol dimethyl ether, isopropyl alcohol and toluene, comprising the steps of:
extracting and rectifying the mixed solution and ethylene glycol in a first rectifying tower to obtain a first material containing isopropanol and toluene at the tower top, obtaining a second material containing ethylene glycol dimethyl ether and ethylene glycol at the tower bottom,
the first material and glycol are extracted and rectified in a second rectifying tower to obtain toluene product at the tower top and a third material containing isopropanol and glycol at the tower bottom,
the second material is rectified in a third rectifying tower to obtain ethylene glycol dimethyl ether product at the tower top,
and rectifying the third material in a fourth rectifying tower to obtain an isopropanol product at the tower top.
In some embodiments, the bottom of the third distillation column obtains a fourth material containing ethylene glycol, the bottom of the fourth distillation column obtains a fifth material containing ethylene glycol, and the fourth material and the fifth material are refluxed to the first distillation column for the extractive distillation.
In some embodiments, the operating conditions of the first rectification column are: 20-101kpa, the top temperature of 30-95 ℃, the bottom temperature of 100-160 ℃ and the reflux ratio of 0.2-1.5.
In some embodiments, the operating conditions of the first rectification column are: 101kpa, a top temperature of 88.23 ℃, a bottom temperature of 153.49 ℃ and a reflux ratio of 0.5.
In some embodiments, the operating conditions of the second rectification column are: 20-101kpa, 40-95 ℃ of the top of the tower, 80-140 ℃ of the bottom of the tower and 0.2-1.5 of reflux ratio.
In some embodiments, the operating conditions of the second rectification column are: 101kpa, a top temperature of 87.52 ℃, a bottom temperature of 122.34 ℃ and a reflux ratio of 0.5.
In some embodiments, the operating conditions of the third rectification column are: 5-101kpa, the tower top temperature is 10-50 ℃, the tower bottom temperature is 100-150 ℃, and the reflux ratio is 1-5.
In some embodiments, the operating conditions of the third rectification column are: 101kpa, a top temperature of 26.5 ℃, a bottom temperature of 132.38 ℃ and a reflux ratio of 3.
In some embodiments, the operating conditions of the fourth rectification column are: 5-101kpa, the temperature at the top of the tower is 20-85 ℃, the temperature at the bottom of the tower is 100-.
In some embodiments, the operating conditions of the fourth rectification column are: 101kpa, top temperature 81.96 ℃, bottom temperature 197.09 ℃ and reflux ratio of 1.
The treatment method can separate the ethylene glycol dimethyl ether, the isopropanol and the toluene from the mixed solution of the ethylene glycol dimethyl ether, the isopropanol and the toluene respectively, the ethylene glycol obtained by extraction and rectification can be recycled in the whole system, and the method can be used for treating wastewater containing related components in the fields of various polymer chemistry, electrochemistry and boronization chemical processes.
Drawings
FIG. 1 is a schematic view showing a process flow of a mixed solution of ethylene glycol dimethyl ether, isopropyl alcohol and toluene.
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 contents in the present example are weight percentages unless otherwise specified.
The invention relates to a method for treating mixed liquid containing glycol dimethyl ether, isopropanol and toluene, which comprises the following steps:
extracting and rectifying the mixed solution and ethylene glycol in a first rectifying tower to obtain a first material containing isopropanol and toluene at the tower top, obtaining a second material containing ethylene glycol dimethyl ether and ethylene glycol at the tower bottom,
the first material and glycol are extracted and rectified in a second rectifying tower to obtain toluene product at the tower top and a third material containing isopropanol and glycol at the tower bottom,
the second material is rectified in a third rectifying tower to obtain ethylene glycol dimethyl ether product at the tower top,
and rectifying the third material in a fourth rectifying tower to obtain an isopropanol product at the tower top.
The invention is further described with reference to the following figures and examples.
The mixed liquid of this embodiment contains 65% of ethylene glycol dimethyl ether, 5% of isopropanol and 30% of toluene, the mixed liquid and ethylene glycol enter a first rectification tower for extractive rectification, the feed flow rate of the mixed liquid is 1000kg/h, the feed flow rate of the ethylene glycol is 3000kg/h, so as to perform preliminary separation on each component, and the operating conditions of the first rectification tower are as follows: the tower top temperature is 88.23 ℃, the tower bottom temperature is 153.49 ℃, the first material containing 85.22% of methylbenzene, 14.12% of isopropanol and 0.66% of glycol is discharged from the tower top, the flow rate is 352kg/h, and the second material containing 82.18% of glycol and 17.82% of glycol dimethyl ether is discharged from the tower bottom, the flow rate is 3648 kg/h.
Respectively carrying out the following treatment on the first material and the second material:
the first material and ethylene glycol enter a second rectifying tower together for extraction and rectification, the feeding flow of the first material is 352kg/h, the feeding flow of the ethylene glycol is 1000kg/h, and the operating conditions of the second rectifying tower are as follows: the normal pressure, the top temperature of 87.52 ℃ and the bottom temperature of 122.34 ℃ and the reflux ratio of 0.5, wherein the top discharge is a toluene product containing 99.65 percent of toluene and 0.35 percent of ethylene glycol, the flow rate is 301kg/h, and the bottom discharge is a third material containing 95.27 percent of ethylene glycol and 4.73 percent of isopropanol, the flow rate is 1051 kg/h.
The second material enters a third rectifying tower for rectification, the feeding flow of the second material is 3648kg/h, and the operating conditions of the third rectifying tower are as follows: the tower top temperature is 26.5 ℃, the tower bottom temperature is 132.38 ℃, the reflux ratio is 3, the material discharged from the tower top is glycol dimethyl ether product containing 99.95 percent of glycol dimethyl ether and 0.05 percent of isopropanol, the flow rate is 650kg/h, the material discharged from the tower bottom is fourth material containing 99.989 percent of glycol and 0.011 percent of glycol dimethyl ether, and the flow rate is 2998 kg/h.
The third material enters a fourth rectifying tower for rectification, the feed flow of the third material is 1051kg/h, and the operating conditions of the fourth rectifying tower are as follows: the tower top temperature is 81.96 ℃, the tower bottom temperature is 197.09 ℃, the reflux ratio is 1, the tower top discharge is an isopropanol product containing 99.91 percent of isopropanol and 0.09 percent of methylbenzene, the flow rate is 49.7kg/h, and the tower bottom discharge is a fifth material containing 99.997 percent of glycol and 0.003 percent of isopropanol, the flow rate is 1001.3 kg/h.
The fourth material and the fifth material can directly flow back to the first rectifying tower, the high-purity ethylene glycol can be used as an extracting agent for extractive rectification, and the ethylene glycol is recovered and recycled in the process.
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 (10)
1. A treatment method of mixed liquid containing glycol dimethyl ether, isopropanol and toluene is characterized by comprising the following steps:
extracting and rectifying the mixed solution and ethylene glycol in a first rectifying tower to obtain a first material containing isopropanol and toluene at the tower top, obtaining a second material containing ethylene glycol dimethyl ether and ethylene glycol at the tower bottom,
the first material and glycol are extracted and rectified in a second rectifying tower to obtain toluene product at the tower top and a third material containing isopropanol and glycol at the tower bottom,
the second material is rectified in a third rectifying tower to obtain ethylene glycol dimethyl ether product at the tower top,
and rectifying the third material in a fourth rectifying tower to obtain an isopropanol product at the tower top.
2. The process according to claim 1, wherein the fourth material containing ethylene glycol is obtained from the bottom of the third distillation column, the fifth material containing ethylene glycol is obtained from the bottom of the fourth distillation column, and the fourth material and the fifth material are refluxed to the first distillation column for the extractive distillation.
3. The process according to claim 1, characterized in that the operating conditions of the first rectification column are: 20-101kpa, the top temperature of 30-95 ℃, the bottom temperature of 100-160 ℃ and the reflux ratio of 0.2-1.5.
4. The process according to claim 3, characterized in that the operating conditions of the first rectification column are: 101kpa, a top temperature of 88.23 ℃, a bottom temperature of 153.49 ℃ and a reflux ratio of 0.5.
5. The process according to claim 1, characterized in that the operating conditions of the second rectification column are: 20-101kpa, 40-95 ℃ of the top of the tower, 80-140 ℃ of the bottom of the tower and 0.2-1.5 of reflux ratio.
6. The process according to claim 6, characterized in that the operating conditions of the second rectification column are: 101kpa, a top temperature of 87.52 ℃, a bottom temperature of 122.34 ℃ and a reflux ratio of 0.5.
7. The process according to claim 1, characterized in that the operating conditions of the third rectification column are: 5-101kpa, the tower top temperature is 10-50 ℃, the tower bottom temperature is 100-150 ℃, and the reflux ratio is 1-5.
8. The process according to claim 7, characterized in that the operating conditions of the third rectification column are: 101kpa, a top temperature of 26.5 ℃, a bottom temperature of 132.38 ℃ and a reflux ratio of 3.
9. The process according to claim 1, characterized in that the operating conditions of the fourth rectification column are: 5-101kpa, the temperature at the top of the tower is 20-85 ℃, the temperature at the bottom of the tower is 100-.
10. The process according to claim 9, characterized in that the operating conditions of the fourth rectification column are: 101kpa, top temperature 81.96 ℃, bottom temperature 197.09 ℃ and reflux ratio of 1.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4514262A (en) * | 1982-08-02 | 1985-04-30 | Lloyd Berg | Separation of benzene from non-aromatic hydrocarbons by extractive distillation |
US5897750A (en) * | 1997-08-28 | 1999-04-27 | Berg; Lloyd | Separation of acetone from isopropanol-water mixtures by extractive distillation |
CN107253901A (en) * | 2017-07-26 | 2017-10-17 | 四川天采科技有限责任公司 | A kind of separation of high-purity isopropanol and purification method |
CN107311833A (en) * | 2017-07-04 | 2017-11-03 | 中国科学院过程工程研究所 | Application for the eutectic solvent of aromatics seperation and its in extracting rectifying |
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- 2021-06-24 CN CN202110707033.XA patent/CN113354517B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4514262A (en) * | 1982-08-02 | 1985-04-30 | Lloyd Berg | Separation of benzene from non-aromatic hydrocarbons by extractive distillation |
US5897750A (en) * | 1997-08-28 | 1999-04-27 | Berg; Lloyd | Separation of acetone from isopropanol-water mixtures by extractive distillation |
CN107311833A (en) * | 2017-07-04 | 2017-11-03 | 中国科学院过程工程研究所 | Application for the eutectic solvent of aromatics seperation and its in extracting rectifying |
CN107253901A (en) * | 2017-07-26 | 2017-10-17 | 四川天采科技有限责任公司 | A kind of separation of high-purity isopropanol and purification method |
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