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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
ethylene glycol
tower
isopropanol
dimethyl ether
toluene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110707033.XA
Other languages
Chinese (zh)
Other versions
CN113354517B (en
Inventor
许兆华
章乐琦
邵峰
王帅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Solvent Environmental Protection Technology Shanghai Co ltd
Original Assignee
Solvent Environmental Protection Technology Shanghai Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Solvent Environmental Protection Technology Shanghai Co ltd filed Critical Solvent Environmental Protection Technology Shanghai Co ltd
Priority to CN202110707033.XA priority Critical patent/CN113354517B/en
Publication of CN113354517A publication Critical patent/CN113354517A/en
Application granted granted Critical
Publication of CN113354517B publication Critical patent/CN113354517B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01Preparation of ethers
    • C07C41/34Separation; Purification; Stabilisation; Use of additives
    • C07C41/40Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
    • C07C41/42Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • C07C7/05Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation

Landscapes

  • 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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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

Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene
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.
CN202110707033.XA 2021-06-24 2021-06-24 Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene Active CN113354517B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110707033.XA CN113354517B (en) 2021-06-24 2021-06-24 Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110707033.XA CN113354517B (en) 2021-06-24 2021-06-24 Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene

Publications (2)

Publication Number Publication Date
CN113354517A true CN113354517A (en) 2021-09-07
CN113354517B CN113354517B (en) 2022-10-14

Family

ID=77536323

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110707033.XA Active CN113354517B (en) 2021-06-24 2021-06-24 Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene

Country Status (1)

Country Link
CN (1) CN113354517B (en)

Citations (4)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Also Published As

Publication number Publication date
CN113354517B (en) 2022-10-14

Similar Documents

Publication Publication Date Title
CN103449981B (en) Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water
CN101898952A (en) Method and device for treating low-concentration acetic acid wastewater
CN100548972C (en) A kind of method of separation of methanol acetonitrile azeotrope
CN103055530B (en) Solvent reinforced transformation thermal coupling rectification system for separating cyclohexanone and phenol
CN112239434B (en) Epoxy chloropropane production device and technology
CN104628522A (en) Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture
CN112237749A (en) Device and method for synthesizing trioxymethylene by rectifying through salt effect reaction
CN106008186A (en) Method for separating acetone, isopropanol and water mixed solution
CN105693466A (en) Reactive distillation method and device for efficient hydrolysis of glycol acetal/ketone product
CN113354517B (en) Method for treating mixed liquid containing ethylene glycol dimethyl ether, isopropanol and toluene
CN112125802B (en) Extractive distillation separation system and method for ethyl acetate-isopropanol-water mixture
CN106349188B (en) A kind of de- propylene, deoxidization technique
CN1145901A (en) Method for separating trioxane from aqueous mixture
CN113461544B (en) Method for treating mixed liquid containing acetonitrile, triethylamine and water
CN108467330B (en) Method and device for efficiently separating cyclohexane and benzene mixture
CN113461570A (en) Method for treating mixed liquid containing isopropanol, acetonitrile, triethylamine and water
CN106431880A (en) Novel method for rectifying and separating acetone and isopropyl ether systems under variable pressures
CN113461571A (en) Treatment method of mixed liquid containing triethylamine, acetonitrile and water
EP1981833A2 (en) Azeotropic distillation method
CN113372297B (en) Method for treating mixed liquid containing ethanol, piperazine, n-hexanol and water
CN105272808A (en) Propylene recovery device
CN113321597A (en) Method for treating mixed liquid containing isopropanol, acetonitrile, triethylamine and water
CN113354571B (en) Method for treating mixed liquid containing piperidine and water
CN203494193U (en) Azeotropic rectifying device for separating propylene glycol monomethyl ether from water
CN105712953A (en) Method of pre-purifying epoxy propane

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant