CN104974023A - Method for recovering ethylene glycol monomethyl ether - Google Patents
Method for recovering ethylene glycol monomethyl ether Download PDFInfo
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- CN104974023A CN104974023A CN201510318130.4A CN201510318130A CN104974023A CN 104974023 A CN104974023 A CN 104974023A CN 201510318130 A CN201510318130 A CN 201510318130A CN 104974023 A CN104974023 A CN 104974023A
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- ethylene glycol
- monomethyl ether
- glycol monomethyl
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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
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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
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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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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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for recovering ethylene glycol monomethyl ether from aqueous solution of ethylene glycol monomethyl ether with moisture content of no less than 60% by using isopropyl acetate as an extraction solvent and an extraction separation system. The extraction separation system consists of an azeotropic reactor R1, a stratified tank V1, a condenser, an extraction solvent conveyer pipe L1 and an extraction solvent conveyer pipe L2. The invention utilizes the principle of extraction and azeotropy; the azeotropic reactor R1, stratified tank V1, condenser, extraction solvent conveyer pipe L1 and extraction solvent conveyer pipe L2 consist of an extraction separation system; and water-immiscible isopropyl acetate with specific gravity less than water is selected as the extraction solvent to recover ethylene glycol monomethyl ether from the aqueous solution of ethylene glycol monomethyl ether with high moisture content; and the extraction solvent isopropyl acetate can be reused. The method has the characteristics of high recovery rate of ethylene glycol monomethyl ether, low recycling cost, flexible and easy operation, and no restriction by the composition fluctuation of aqueous solution of ethylene glycol monomethyl ether, and has broad application prospects.
Description
Technical field
The present invention relates to a kind of method reclaiming ethylene glycol monomethyl ether, from the ethylene glycol monomethyl ether aqueous solution of high-moisture percentage, especially reclaim the method for ethylene glycol monomethyl ether.
Background technology
Ethylene glycol monomethyl ether (being abbreviated as MOE), also known as ethylene glycol monomethyl ether, is a kind of colourless transparent liquid, boiling point 124. 6 DEG C (101. 3KPa), fusing point-85 DEG C, and water, alcohol, acetic acid, acetone and DMF are miscible.MOE is widely used in the fields such as lipid, cellulose acetate, nitrocellulose, spirit soluble dyestuffs and synthetic resins as a kind of important solvent, MOE is also more and more for pharmaceutical industry, aviation jet fuel deicing agent, brake solution thinner etc. in recent years, and consumption increases year by year.A large amount of aqueous solution containing MOE often can be produced in MOE use procedure; the mixture formed due to MOE and water belongs to the system that dissolves each other completely; in azeotrope, the massfraction of MOE is only 15.3%; and the boiling point of the boiling point of azeotrope and water is very close; rectifying mode is adopted to be difficult to the two to be effectively separated; these reasons cause the MOE of the high-moisture percentage mode process adopting burning more, add " three wastes " processing cost and risk of environmental pollution.Ethylene glycol monomethyl ether trade effluent as produced the high-moisture percentage produced in benzofuranol and Propoxur process adopts the mode process of burning at present mostly, not only uneconomical but also contaminate environment.
Following methods is mainly contained at present: (a) adds azeotropic entrainment agent in the MOE aqueous solution from containing reclaiming MOE the aqueous solution of MOE, the method of rectifying azeotropic band Water Sproading is adopted to reclaim MOE, but the MOE effect of the method to low-water-content is better, but a large amount of energy consumptions is needed to the aqueous solution of the MOE of water ratio, processing cost is high, and treatment effect is bad; B () adds siccative (as calcium chloride etc.) and dewaters in the MOE aqueous solution, but the method is also only suitable for the MOE of low-water-content, and the slurries regeneration difficulty produced after dehydration, still carry a small amount of MOE secretly in slurries, easily cause some problems to environment.
Summary of the invention
The object of this invention is to provide a kind of method reclaiming ethylene glycol monomethyl ether, is take isopropyl acetate as extraction agent, by extracting and separating system recoveries ethylene glycol monomethyl ether from the ethylene glycol monomethyl ether aqueous solution of high-moisture percentage.Extracting and separating system is made up of azeotropic still R1, layering tank V1, condenser, extraction agent transfer lime L1 and extraction liquid transfer lime L2.The ethylene glycol monomethyl ether aqueous solution enters in layering tank V1, by the extraction agent isopropyl acetate in extraction agent storage tank V2 by connecting layering tank V1 the extraction agent transfer lime L1 be inserted into bottom layering tank V1 enters bottom layering tank V1, proportion due to extraction agent isopropyl acetate is less than water and does not dissolve each other with water, the extraction agent isopropyl acetate entered into bottom layering tank V1 rises toward V1 tank top bottom layering tank V1, extracts in extraction agent uphill process to the ethylene glycol monomethyl ether in the ethylene glycol monomethyl ether aqueous solution.Ethylene glycol monomethyl ether extraction liquid is that organic phase floats over V1 tank top, extraction liquid organic phase flows in azeotropic still R1 by the extraction liquid transfer lime L2 on V1 tank top, ethylene glycol monomethyl ether extraction liquid organic phase carries out adding thermal distillation in azeotropic still R1, extraction agent isopropyl acetate is constantly steamed, and is reentered bottom layering tank V1 extract ethylene glycol monomethyl ether again after condenser condenses by pipeline L1.When recording ethylene glycol monomethyl ether content≤0.1% in layering tank V1 lower floor aqueous phase, stopping azeotropic still R1 distillation, releasing layering tank V1 lower floor aqueous phase and entering Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit simultaneously and carry out rectifying, namely obtain the ethylene glycol monomethyl ether of water ratio≤0.1%.Ethylene glycol monomethyl ether rate of recovery > 90%.
The consumption of extraction agent isopropyl acetate of the present invention is 0.02 ~ 5 times of ethylene glycol monomethyl ether aqueous solution weight.The ethylene glycol monomethyl ether aqueous solution of high-moisture percentage refers to water ratio >=60%(mass percent) the ethylene glycol monomethyl ether aqueous solution.
The present invention can install many take-off pipes to expand area when extraction agent isopropyl acetate passes into, to improve extraction efficiency in described extraction agent transfer lime L1 exit according to actual needs.
The present invention utilizes extraction and azeotropic principles, extracting and separating system is formed by azeotropic still R1, layering tank V1, condenser, extraction agent transfer lime L1 and extraction liquid transfer lime L2, choose proportion to be less than water and to be extraction agent with the immiscible isopropyl acetate of water, from the ethylene glycol monomethyl ether aqueous solution of high-moisture percentage, reclaim ethylene glycol monomethyl ether.And extraction agent isopropyl acetate is capable of circulation to be applied mechanically.The ethylene glycol monomethyl ether rate of recovery of the present invention is high, and cost recovery is low, and flexible operation is easy, not by features such as ethylene glycol monomethyl ether aqueous solution composition fluctuation restrictions, has broad application prospects.
Accompanying drawing explanation
Fig. 1 is that extracting and separating reclaims ethylene glycol monomethyl ether process flow sheet.
In Fig. 1, R1 is azeotropic still, and V1 is layering tank, and V2 is extraction agent storage tank, and E1 is condenser, and L1 is extraction agent transfer lime, and L2 is extraction liquid transfer lime.
Embodiment
The specific embodiment of the present invention is described in detail as follows with reference to accompanying drawing, but is not only restriction the present invention as explanation.
Embodiment 1
In layering tank V1, add water ratio is 80%(mass percent) the ethylene glycol monomethyl ether aqueous solution 500 kg, then the isopropyl acetate in extraction agent storage tank V2 is added 50 kg isopropyl acetates by extraction agent transfer lime L1 in layering tank V1, the organic phase on aqueous solution upper strata is flow in azeotropic still R1 by pipeline L2.After having added, heating azeotropic still R1 distills, cooled cut extraction agent directly enters bottom layering tank V1 by extraction agent transfer lime L1, the process that extraction agent rises to liquid level bottom the ethylene glycol monomethyl ether aqueous solution is extraction process, the extraction liquid organic phase on layering tank V1 upper strata constantly returns in azeotropic still R1 by extraction liquid transfer lime L2, when in layering tank V1 lower floor aqueous phase, ethylene glycol monomethyl ether content is less than 0.1%(mass percent) time stop the distillation of azeotropic still R1.Release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit and carries out conventional rectification, namely obtain ethylene glycol monomethyl ether 96.9 kg, record water ratio≤0.1%.
The isopropyl acetate reclaimed directly can be applied mechanically to next batch as extraction agent and test.
Embodiment 2
In layering tank V1, add water ratio is 80%(mass percent) the ethylene glycol monomethyl ether aqueous solution 500 kg, then in layering tank V1, added extraction agent 48 kg of embodiment 1 recovery by extraction agent transfer lime L1, the organic phase on aqueous solution upper strata is flow in azeotropic still R1 by pipeline L2.After having added, heating azeotropic still R1 distills, cooled cut (extraction agent) directly enters bottom layering tank V1 by extraction agent transfer lime L1, the process that extraction agent rises to liquid level bottom the ethylene glycol monomethyl ether aqueous solution is extraction process, the extraction liquid organic phase on layering tank V1 upper strata constantly returns in azeotropic still R1 by extraction liquid transfer lime L2, when in layering tank V1 lower floor aqueous phase, ethylene glycol monomethyl ether content is less than 0.1%(mass percent) time stop the distillation of azeotropic still R1.Release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit and carries out conventional rectification, namely obtain ethylene glycol monomethyl ether 98.7 kg, record water ratio≤0.1%.
Embodiment 3
In layering tank V1, add water ratio is 97%(mass percent) the ethylene glycol monomethyl ether aqueous solution 500 kg, then the isopropyl acetate in extraction agent storage tank V2 is added 10 kg isopropyl acetates by extraction agent transfer lime L1 in layering tank V1, the extraction liquid organic phase on aqueous solution upper strata is flow in azeotropic still R1 by extraction liquid transfer lime L2.After having added, heating azeotropic still R1 distills, cooled cut extraction agent directly enters bottom layering tank V1 by extraction agent transfer lime L1, the process that extraction agent rises to liquid level bottom the ethylene glycol monomethyl ether aqueous solution is extraction process, the organic phase on layering tank V1 upper strata constantly returns in azeotropic still R1 by pipeline L2, when in layering tank V1 lower floor aqueous phase, ethylene glycol monomethyl ether content is less than 0.1%(mass percent) time stop the distillation of azeotropic still R1.Release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit and carries out conventional rectification, namely obtain ethylene glycol monomethyl ether 14.25kg, record water ratio≤0.1%.
Embodiment 4
In layering tank V1, add water ratio is 90%(mass percent) the ethylene glycol monomethyl ether aqueous solution 500 kg, then the isopropyl acetate in extraction agent storage tank V2 is added 30 kg isopropyl acetates by pipeline L1 in layering tank V1, the organic phase on aqueous solution upper strata is flow in azeotropic still R1 by pipeline L2.After having added, heating azeotropic still R1 distills, cooled cut (extraction agent) directly enters bottom layering tank V1 by extraction agent transfer lime L1, the process that extraction agent rises to liquid level bottom the ethylene glycol monomethyl ether aqueous solution is extraction process, the extraction liquid organic phase on layering tank V1 upper strata constantly returns in azeotropic still R1 by extraction liquid transfer lime L2, when in layering tank V1 lower floor aqueous phase, ethylene glycol monomethyl ether content is less than 0.1%(mass percent) time stop the distillation of azeotropic still R1.Release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit and carries out conventional rectification, namely obtain ethylene glycol monomethyl ether 48.3kg, record water ratio≤0.1%.
Embodiment 5
In layering tank V1, add water ratio is 60%(mass percent) ethylene glycol monomethyl ether aqueous solution liquid 200 kg, then the isopropyl acetate in extraction agent storage tank V2 is added 1000 kg isopropyl acetates by extraction agent transfer lime L1 in layering tank V1, the organic phase on aqueous solution upper strata is flow in azeotropic still R1 by pipeline L2.After having added, heating azeotropic still R1 distills, cooled cut (extraction agent) directly enters bottom layering tank V1 by extraction agent transfer lime L1, the process that extraction agent rises to liquid level bottom the ethylene glycol monomethyl ether aqueous solution is extraction process, the extraction liquid organic phase on layering tank V1 upper strata constantly returns in azeotropic still R1 by extraction liquid transfer lime L2, when in layering tank V1 lower floor aqueous phase, ethylene glycol monomethyl ether content is less than 0.1%(mass percent) time stop the distillation of azeotropic still R1.Release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment.Still liquid in azeotropic still R1 is imported rectifier unit and carries out conventional rectification, namely obtain ethylene glycol monomethyl ether 75.2kg, record water ratio≤0.1%.
Claims (4)
1. one kind is reclaimed the method for ethylene glycol monomethyl ether, it is characterized in that taking isopropyl acetate as extraction agent, by extracting and separating system recoveries ethylene glycol monomethyl ether from the ethylene glycol monomethyl ether aqueous solution, extracting and separating system is made up of azeotropic still R1, layering tank V1, condenser, extraction agent transfer lime L1, extraction liquid transfer lime L2.
2. method according to claim 1, it is characterized in that the ethylene glycol monomethyl ether aqueous solution enters in layering tank V1, extraction agent isopropyl acetate is by connection layering tank V1 and the extraction agent transfer lime L1 be inserted into bottom layering tank V1 enters bottom layering tank V1, proportion due to extraction agent isopropyl acetate is less than water and does not dissolve each other with water, the extraction agent isopropyl acetate entered into bottom layering tank V1 rises toward V1 tank top bottom layering tank V1, extracts in extraction agent uphill process to the ethylene glycol monomethyl ether in the ethylene glycol monomethyl ether aqueous solution, ethylene glycol monomethyl ether extraction liquid is that organic phase floats over V1 tank top, ethylene glycol monomethyl ether extraction liquid organic phase flows in azeotropic still R1 by the extraction liquid transfer lime L2 on V1 tank top, ethylene glycol monomethyl ether extraction liquid organic phase carries out adding thermal distillation in azeotropic still R1, extraction agent isopropyl acetate is constantly steamed, reentered bottom layering tank V1 by extraction agent transfer lime L1 after condenser condenses and ethylene glycol monomethyl ether is extracted again, when recording ethylene glycol monomethyl ether content≤0.1% in layering tank V1 lower floor aqueous phase, stop azeotropic still R1 distillation, release layering tank V1 lower floor aqueous phase and enter Waste Water Treatment, still liquid in azeotropic still R1 is imported rectifier unit simultaneously and carry out rectifying, namely the ethylene glycol monomethyl ether of water ratio≤0.1% is obtained, ethylene glycol monomethyl ether rate of recovery > 90%.
3. the method according to claim 1 and 2, is characterized in that the consumption of extraction agent isopropyl acetate is 0.02 ~ 5 times of ethylene glycol monomethyl ether aqueous solution weight.
4. the method according to claim 1 and 2, is characterized in that the ethylene glycol monomethyl ether aqueous solution refers to the ethylene glycol monomethyl ether aqueous solution of water ratio >=60%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510318130.4A CN104974023A (en) | 2015-06-11 | 2015-06-11 | Method for recovering ethylene glycol monomethyl ether |
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| CN201510318130.4A CN104974023A (en) | 2015-06-11 | 2015-06-11 | Method for recovering ethylene glycol monomethyl ether |
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| CN104974023A true CN104974023A (en) | 2015-10-14 |
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| CN201510318130.4A Pending CN104974023A (en) | 2015-06-11 | 2015-06-11 | Method for recovering ethylene glycol monomethyl ether |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032966A (en) * | 2017-06-14 | 2017-08-11 | 青岛科技大学 | A kind of method of liquid-liquid extraction separation of extractive distillation methyl proxitol and water |
| CN110330413A (en) * | 2019-07-31 | 2019-10-15 | 惠生工程（中国）有限公司 | A method of propylene glycol monomethyl ether in recycling alcohol ether aqueous solution logistics |
| CN114212941A (en) * | 2021-12-21 | 2022-03-22 | 江苏三吉利化工股份有限公司 | System and method for recovering MOE (metal oxide organic ether) in ethylene glycol monomethyl ether wastewater |
| CN114307217A (en) * | 2021-12-30 | 2022-04-12 | 江苏三吉利化工股份有限公司 | Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63307836A (en) * | 1987-06-09 | 1988-12-15 | Daicel Chem Ind Ltd | Recovery of dipropylene glycol monomethyl ether |
| CN102952004A (en) * | 2012-01-11 | 2013-03-06 | 河北工业大学 | Technology for separating ethylene glycol monomethyl ether and water by use of continuous azeotropic distillation method |
-
2015
- 2015-06-11 CN CN201510318130.4A patent/CN104974023A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63307836A (en) * | 1987-06-09 | 1988-12-15 | Daicel Chem Ind Ltd | Recovery of dipropylene glycol monomethyl ether |
| CN102952004A (en) * | 2012-01-11 | 2013-03-06 | 河北工业大学 | Technology for separating ethylene glycol monomethyl ether and water by use of continuous azeotropic distillation method |
Non-Patent Citations (1)
| Title |
|---|
| 李春利等: "间歇共沸精馏分离乙二醇单甲醚-水物系", 《化工进展》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032966A (en) * | 2017-06-14 | 2017-08-11 | 青岛科技大学 | A kind of method of liquid-liquid extraction separation of extractive distillation methyl proxitol and water |
| CN110330413A (en) * | 2019-07-31 | 2019-10-15 | 惠生工程（中国）有限公司 | A method of propylene glycol monomethyl ether in recycling alcohol ether aqueous solution logistics |
| CN110330413B (en) * | 2019-07-31 | 2022-08-09 | 惠生工程（中国）有限公司 | Method for recovering propylene glycol monomethyl ether in alcohol ether aqueous solution material flow |
| CN114212941A (en) * | 2021-12-21 | 2022-03-22 | 江苏三吉利化工股份有限公司 | System and method for recovering MOE (metal oxide organic ether) in ethylene glycol monomethyl ether wastewater |
| CN114307217A (en) * | 2021-12-30 | 2022-04-12 | 江苏三吉利化工股份有限公司 | Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol |
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