CN103449981B - Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water - Google Patents
Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water Download PDFInfo
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- CN103449981B CN103449981B CN201310369761.XA CN201310369761A CN103449981B CN 103449981 B CN103449981 B CN 103449981B CN 201310369761 A CN201310369761 A CN 201310369761A CN 103449981 B CN103449981 B CN 103449981B
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Abstract
The invention discloses an azeotropic rectification device and method for separating propylene glycol monomethyl ether and water. The azeotropic rectification device and method are characterized in that cyclohexane is adopted as an entrainer; waste liquor containing propylene glycol monomethyl ether, water and cyclohexane is added to a rectification kettle once; a rectification column is directly connected with the rectification kettle; a kettle-type reboiler is arranged on the rectification kettle; the waste liquor is heated into steam through the kettle-type reboiler and then enters the rectification column; the material at the top of the column is condensed and then transferred into the a reflux ratio controller; if the material at the top of the column is an azeotrope of cyclohexane and water, the material is fed into a phase splitting tank for phase splitting, a water phase is extracted, and cyclohexane reflows; if the material at the top of the column is cyclohexane, recovered cyclohexane is obtained; if the material at the top of the column is a transition fraction of cyclohexane and propylene glycol monomethyl ether, the material is extracted into a transition fraction storage tank; if the material at the top of the column is propylene glycol monomethyl ether, a propylene glycol monomethyl ether product can be obtained; once materials in the kettle of the column are basically the heavy components of the waste liquor, the extracting at the top of the column is stopped, and the residual materials in the kettle are discharged from the bottom part of the rectification kettle. The device and method for separating propylene glycol monomethyl ether and water are efficient and environment-friendly.
Description
Technical field
The invention belongs to the processing method of chemical separation process, say the device and method relating to azeotropic batch fractionating separating propylene glycol methyl ether and water further.
Background technology
Propylene glycol monomethyl ether (PM) belongs to glycol ether kind solvent, and propylene glycol lower than glycol ether series products, belongs to low toxicity ethers to the toxicity of human body.Propylene glycol monomethyl ether has faint ether taste, but does not have strong and stimulating smell, makes its purposes more extensively safety.Because ether existing in its molecular structure has hydroxyl again, thus its solubility property is very excellent, has again the features such as suitable rate of volatilization and reactive behavior and obtains wide application.Propylene glycol monomethyl ether is mainly used as solvent, dispersion agent, thinner, fuel antifreezing agent, extraction agent, coating and sanitising agent etc.For industry such as coating, ink, printing and dyeing, agricultural chemicals, Mierocrystalline cellulose, acrylate.Embody rule makes the strong solvent of water-based paint; The strong solvent of solvent-based printing inks and coupling agent; The solvent of ballpoint pen and fountain pen ink; The coupling agent of family expenses and industrial cleaners, derust agent and hard surface cleaner and solvent; The solvent of agricultural insecticide; Cleaning glass agent prescription is mixed for propylene glycol n-butyl ether.
The production technique mainly epoxidation of propylene method of propylene glycol monomethyl ether, but containing a large amount of water in the product of propylene ring oxidation reaction technique, so wish to get highly purified propylene glycol monomethyl ether, the moisture in mixture must be removed.And usually water is contained in containing the waste liquid of propylene glycol monomethyl ether, the sepn process of propylene glycol monomethyl ether and water is also had to pass through for obtaining high-purity propylene glycol monomethyl ether from waste liquid.
Propylene glycol monomethyl ether and water can form azeotrope, under azeotropic refers to and is in equilibrium state, mixing solutions when gas phase is identical with liquid phase composition, its azeotropic consists of propylene glycol monomethyl ether 31.5wt%, water 68.5wt%, azeotropic point is 98.41 DEG C, propylene glycol monomethyl ether and water cannot be separated with general rectificating method, now needs to adopt azeotropic distillation to process.Azeotropic distillation, also known as sequence of constant boiling and rectification, is the rectifying that the character utilizing the component in mixture can form azeotrope realizes being separated.Usually in solution to be separated, add entrainer (or claiming entrainment agent), make one or two component in itself and solution form azeotrope, make separation be easy to carry out with the relative volatility increased between component to be separated.
Entrainer at least should form azeotrope with one of component in original solution, and the boiling point of this azeotrope should be significantly lower than the boiling point of original solution component, in general, in azeotropic distillation, heterogeneous azeotrope can be formed better, the now recovery of entrainer only need use the method for layering just, the entrainer selected when containing propylene glycol monomethyl ether waste water based on our process of mentioned above principle is hexanaphthene, hexanaphthene and water can form the lower azeotrope of boiling point, its azeotropic consists of hexanaphthene 91.6wt%, water 8.4wt%, azeotropic point is 68.95 DEG C, so utilize hexanaphthene to make entrainer can remove water in former waste liquid, and the azeotrope of hexanaphthene and water formation is heterogeneous azeotrope, hexanaphthene can be reclaimed by the method for layering.
The entrainer being generally used for separating propylene glycol methyl ether and water is benzene, but benzene is very serious to the pollution of environment, and also can produce serious influence for the health of the personnel of operation of equipment.
Therefore the present invention proposes one utilizes cyclohexane give for entrainer, the technique of intermittent azeotropic rectifying coupling phase-splitting operation processes the waste water containing propylene glycol monomethyl ether, this technique can propylene glycol monomethyl ether product in efficient recovery waste water, and technical process is simple, entrainer is easy to reclaim, recycle, not only creates good social benefit and also creates good economic benefit.
Summary of the invention
The object of this invention is to provide the device and method of a kind of intermittent azeotropic rectifying separating propylene glycol methyl ether and water, adopt this technique can propylene glycol monomethyl ether effectively in Recycling of waste liquid, highly purified propylene glycol monomethyl ether product can not only be obtained, and the waste water after processing can be made to reach the standard of discharge, thus decrease environmental pollution.
Technical scheme of the present invention is as follows:
First the waste liquid adding hexanaphthene enters in rectifying still, be heated into after steam through kettle-type reboiler and rise to rectifying tower tower top, top gaseous phase enters reflux ratio controller after being condensed into liquid phase, when overhead extraction material is the azeotrope of hexanaphthene and water, tower top material enters phase separation tank, hexanaphthene and water stratification in phase separation tank, water enters water pot, and upper strata hexanaphthene refluxes; When overhead extraction material is hexanaphthene, enter entrainer storage tank; When overhead extraction material is the interim fraction between hexanaphthene and propylene glycol monomethyl ether, enter interim fraction storage tank; When overhead extraction material is propylene glycol monomethyl ether product, enter propylene glycol monomethyl ether product storage tank.Still is residual discharges bottom rectifying still.
Described separating propylene glycol methyl ether and the device of water are batch rectification device.
Described extraction pipeline connects entrainer storage tank, interim fraction storage tank, propylene glycol monomethyl ether product storage tank.
The installation site of described reflux ratio controller refluxing opening should higher than the installation site of the refluxing opening of rectifying tower and phase separation tank material inlet.
The installation site of described phase separation tank bottoms material outlet should higher than water pot, entrainer storage tank, the installation site of interim fraction storage tank and propylene glycol monomethyl ether product storage tank material inlet.
Consider that hexanaphthene and water belong to heterogeneous azeotrope, so utilize phase separation tank to carry out phase-splitting operation, just can realize the recycle of hexanaphthene, such consumption that can reduce hexanaphthene, reduce energy consumption, so at the intermittent azeotropic rectifying operation initial stage, overhead extraction material is the azeotrope of hexanaphthene and water, the not extraction of tower top material, all enter phase separation tank, hexanaphthene and water stratification in phase separation tank, lower floor's aqueous phase is exported by phase separation tank bottoms material and enters water pot, extraction is exported from bottoms material for preventing hexanaphthene, phase separation tank bottoms material extraction pipeline arranges inverted U curved, the backflow of rectifying column top return mouth got back to by upper strata hexanaphthene, water in waste liquid can be removed by the operation in this stage, the waste water obtained can reach emission standard.
According to said apparatus, can proceed as follows:
The waste liquid 1 adding hexanaphthene all joins in rectifying still 2 according to every still treatment capacity is disposable, material in rectifying still 2 is heated into after steam through kettle-type reboiler 3 and rises to rectifying tower 5 tower top, rectifying tower 5 top gaseous phase is condensed into after liquid phase through overhead condenser 6 and enters reflux ratio controller 7, in intermittent azeotropic rectifying process, overhead extraction is divided into four-stage, is followed successively by chronological order:
First stage: overhead extraction material is the azeotrope of hexanaphthene and water, the now extraction closedown of pipeline of reflux ratio controller 7, reflux line valve 8 is also closed, phase separation tank pipeline valve 9 is opened, overhead extraction material all enters phase separation tank 10, hexanaphthene and water stratification in phase separation tank 10, hexanaphthene is on upper strata, water is in lower floor, water 11 enters water pot 12 from phase separation tank 10 bottoms material extraction pipeline, extraction is exported from bottoms material for preventing hexanaphthene, phase separation tank bottoms material extraction pipeline arranges inverted U curved, upper strata hexanaphthene is got back to rectifying tower 5 trim the top of column mouth and is refluxed,
Subordinate phase: overhead extraction material is hexanaphthene, and now reflux line valve 8 is opened, and phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, and entrainer 13 enters entrainer storage tank 14;
Phase III: overhead extraction material is the interim fraction between hexanaphthene and propylene glycol monomethyl ether, and now reflux line valve 8 is opened, and phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, and interim fraction 15 enters interim fraction storage tank 16;
Fourth stage: overhead extraction material is propylene glycol monomethyl ether product, and now reflux line valve 8 is opened, and phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, and propylene glycol monomethyl ether product 17 enters propylene glycol monomethyl ether product storage tank 18.
After fourth stage completes, the remaining material of tower reactor is the heavy constituent in waste liquid substantially, and stop overhead extraction, still residual 4 is discharged bottom rectifying still.
The device of intermittent azeotropic rectifying separating propylene glycol methyl ether and water, rectifying tower generally adopts atmospheric operation, utilizes this device can realize satisfied recovery separating effect.
The theoretical plate number of batch fractionating tower is 70 ~ 80, and reflux ratio is 2 ~ 8, and tower top temperature is 65 DEG C ~ 125 DEG C, and bottom temperature is 90 DEG C ~ 140 DEG C.
During atmospheric operation, reflux ratio is 2 ~ 8, and tower top temperature is 65 DEG C ~ 125 DEG C, and bottom temperature is 90 DEG C ~ 140 DEG C, and be 65 DEG C ~ 75 DEG C from tower top service temperature during the azeotrope of overhead extraction hexanaphthene and water, reflux ratio is 8; Be 75 DEG C ~ 85 DEG C from tower top service temperature during overhead extraction hexanaphthene, reflux ratio is 4; Be 85 DEG C ~ 115 DEG C from tower top service temperature during interim fraction between overhead extraction hexanaphthene and propylene glycol monomethyl ether, reflux ratio is 4; Be 115 DEG C ~ 125 DEG C from tower top service temperature during overhead extraction propylene glycol monomethyl ether product, reflux ratio is 2.
The invention has the advantages that the technique of described intermittent azeotropic rectifying separating propylene glycol methyl ether and water can propylene glycol monomethyl ether effectively in Recycling of waste liquid, and the waste water after process can reach emission standard, be coupled the operation of phase-splitting in the technique of intermittent azeotropic rectifying, can by the azeotrope phase-splitting of hexanaphthene and water, being separated of hexanaphthene and water is realized in phase separation tank, effectively can reduce the consumption of hexanaphthene like this, reduce energy consumption, improve the market competitiveness, also creating good social benefit, is a kind of recovery separating technology of high-efficiency environment friendly.
Accompanying drawing explanation
Accompanying drawing is the azeotropic distillation device of the waste water containing propylene glycol monomethyl ether of the present invention.
Wherein: 1-add the waste liquid of hexanaphthene, 2-rectifying still, 3-kettle-type reboiler, 4-still is residual, 5-rectifying tower, 6-overhead condenser, 7-reflux ratio controller, 8-reflux line valve, 9-phase separation tank pipeline valve, 10-phase separation tank, 11-water, 12-water pot, 13-entrainer, 14-entrainer storage tank, 15-interim fraction, 16-interim fraction storage tank, 17-propylene glycol monomethyl ether product, 18-propylene glycol monomethyl ether product storage tank
Embodiment
Below in conjunction with embodiment, further illustrate the present invention, but the present invention is not limited to embodiment.
Equipment of the present invention as shown in the figure, by rectifying tower 5, rectifying still 2, kettle-type reboiler 3, overhead condenser 6, reflux ratio controller 7, reflux line valve 8, phase separation tank pipeline valve 9, phase separation tank 10, water pot 12, entrainer storage tank 14, interim fraction storage tank 16, propylene glycol monomethyl ether product storage tank 18 forms, distillation operation adopts intermittent azeotropic rectifying operation, directly rectifying still 2 is connected bottom rectifying tower 5, rectifying still 2 is arranged kettle-type reboiler 3, the water back level of kettle-type reboiler 3 is inserted into bottom rectifying still 2, rectifying tower tower top arranges overhead condenser 6, overhead condenser 6 exports and connects reflux ratio controller 7, reflux ratio controller 7 refluxing opening connects two pipelines, , an install pipeline reflux line valve 8, connect rectifying tower 5 trim the top of column mouth, another install pipeline phase separation tank pipeline valve 9, connect phase separation tank 10, phase separation tank 10 outlet at bottom connects water pot 12, upper outlet connects rectifying tower 5 trim the top of column mouth, reflux ratio controller 7 extraction mouth connects extraction pipeline, extraction pipeline connects entrainer storage tank 14, interim fraction storage tank 16 and propylene glycol monomethyl ether product storage tank 18.The installation site of reflux ratio controller refluxing opening should higher than the installation site of the refluxing opening of rectifying tower and phase separation tank material inlet.The installation site of phase separation tank bottoms material outlet should higher than water pot, entrainer storage tank, the installation site of interim fraction storage tank and propylene glycol monomethyl ether product storage tank material inlet.
Technology and equipment of the present invention can be applicable to the process of intermittent azeotropic rectifying separating propylene glycol methyl ether and water, in order to the advantage of the present invention in separating propylene glycol methyl ether and water is better described, choose application example to be illustrated, but therefore do not limit the scope of application of this technology and equipment.
Embodiment 1
Feed composition:
| Composition | Propylene glycol monomethyl ether | Heavy constituent | Water |
| Content (wt%) | 35%～40% | 5% | 55%～60% |
Batch fractionating operates, process a still waste liquid every day, the treatment capacity of every still is 5 tons, and every still treatment time is 20 hours, all joins in rectifying still 2 by the waste liquid 1 adding hexanaphthene according to every still treatment capacity is disposable, material in rectifying still 2 is heated into after steam through kettle-type reboiler 3 and rises to rectifying tower 5 tower top, the number of theoretical plate of rectifying tower is 75, and working pressure is normal pressure, reflux ratio 2 ~ 8, tower top temperature is 65 DEG C ~ 125 DEG C, and bottom temperature is 90 DEG C ~ 140 DEG C.Rectifying tower 5 top gaseous phase is condensed into after liquid phase through rectifying tower overhead condenser 6 and enters reflux ratio controller 7, and in intermittent azeotropic rectifying process, overhead extraction is divided into four-stage, is followed successively by chronological order:
First stage: overhead extraction material is the azeotrope of hexanaphthene and water, the now extraction closedown of pipeline of reflux ratio controller 7, reflux line valve 8 is also closed, phase separation tank pipeline valve 9 is opened, overhead extraction material all enters phase separation tank 10, hexanaphthene and water stratification in phase separation tank 10, hexanaphthene is on upper strata, water is in lower floor, water 11 enters water pot 12 from phase separation tank 10 bottoms material extraction pipeline, extraction is exported from bottoms material for preventing hexanaphthene, phase separation tank bottoms material extraction pipeline arranges inverted U curved, upper strata hexanaphthene is got back to rectifying tower 5 trim the top of column mouth and is refluxed, now tower top service temperature is 65 DEG C ~ 75 DEG C, reflux ratio is 8,
Subordinate phase: overhead extraction material is hexanaphthene, and now reflux line valve 8 is opened, and phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, entrainer 13 enters entrainer storage tank 14, and now tower top service temperature is 75 DEG C ~ 85 DEG C, and reflux ratio is 4;
Phase III: overhead extraction material is the interim fraction between hexanaphthene and propylene glycol monomethyl ether, now reflux line valve 8 is opened, phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, interim fraction 15 enters interim fraction storage tank 16, now tower top service temperature is 85 DEG C ~ 115 DEG C, and reflux ratio is 4;
Fourth stage: overhead extraction material is propylene glycol monomethyl ether product, now reflux line valve 8 is opened, phase separation tank pipeline valve 9 is closed, reflux ratio controller 7 extraction pipeline is opened, propylene glycol monomethyl ether product 17 enters propylene glycol monomethyl ether product storage tank 18, now tower top service temperature is 115 DEG C ~ 125 DEG C, and reflux ratio is 2.
After fourth stage completes, the remaining material of tower reactor is the heavy constituent in waste liquid substantially, and stop overhead extraction, still residual 4 is discharged bottom rectifying still.
Can propylene glycol monomethyl ether effectively in Recycling of waste liquid through intermittent azeotropic rectifying process, and the waste water after process can reach emission standard, not only reduce environmental pollution, also for enterprise creates good economic benefit and social benefit, by above-mentioned disposition, can obtain propylene glycol monomethyl ether product 1.75 tons/still, the purity of the propylene glycol monomethyl ether obtained can reach more than 99%.
The device and method of the intermittent azeotropic rectifying separating propylene glycol methyl ether that the present invention proposes and water, be described by preferred embodiment, person skilled obviously can not depart from content of the present invention, in spirit and scope, equipment as herein described and method are changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, all similar replacements and to change be apparent concerning those skilled in the art, they are deemed to be included in spirit of the present invention, in scope and content.
Claims (1)
1. the azeotropic distillation method of a separating propylene glycol methyl ether and water, first the waste liquid adding hexanaphthene enters in rectifying still, be heated into after steam through kettle-type reboiler and rise to rectifying tower tower top, top gaseous phase enters reflux ratio controller after being condensed into liquid phase, when overhead extraction material is the azeotrope of hexanaphthene and water, tower top material enters phase separation tank, hexanaphthene and water stratification in phase separation tank, water enters water pot, and upper strata hexanaphthene refluxes; When overhead extraction material is hexanaphthene, enter entrainer storage tank; When overhead extraction material is the interim fraction between hexanaphthene and propylene glycol monomethyl ether, enter interim fraction storage tank; When overhead extraction material is propylene glycol monomethyl ether product, enter propylene glycol monomethyl ether product storage tank; Still is residual discharges bottom rectifying still; During atmospheric operation, reflux ratio is 2 ~ 8, and tower top temperature is 65 DEG C ~ 125 DEG C, and bottom temperature is 90 DEG C ~ 140 DEG C, and be 65 DEG C ~ 75 DEG C from tower top service temperature during the azeotrope of overhead extraction hexanaphthene and water, reflux ratio is 8; Be 75 DEG C ~ 85 DEG C from tower top service temperature during overhead extraction hexanaphthene, reflux ratio is 4; Be 85 DEG C ~ 115 DEG C from tower top service temperature during interim fraction between overhead extraction hexanaphthene and propylene glycol monomethyl ether, reflux ratio is 4; Be 115 DEG C ~ 125 DEG C from tower top service temperature during overhead extraction propylene glycol monomethyl ether product, reflux ratio is 2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106178571B (en) * | 2016-08-31 | 2023-07-14 | 烟台国邦化工机械科技有限公司 | Azeotrope separation process |
| CN107032966B (en) * | 2017-06-14 | 2020-06-12 | 青岛科技大学 | Method for separating propylene glycol methyl ether and water by liquid-liquid extraction-extractive distillation |
| CN107998678B (en) * | 2017-10-30 | 2023-08-18 | 烟台国邦化工机械科技有限公司 | Environment-friendly cleaning device and process method for separating organic azeotrope |
| CN108299203A (en) * | 2018-01-29 | 2018-07-20 | 淄博高新技术产业开发区精细化工和高分子材料研究院 | A method of PGMEA being recycled from PGMEA/ aqueous solutions using intermittent azeotropic rectifying |
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| CN110272333B (en) * | 2019-07-31 | 2022-08-09 | 惠生工程（中国）有限公司 | Method for recovering propylene glycol monomethyl ether |
| CN110681173A (en) * | 2019-10-23 | 2020-01-14 | 广州首联环境工程有限公司 | Multifunctional waste organic solvent recovery device and application thereof |
| CN111056930B (en) * | 2019-12-12 | 2022-05-03 | 山东天汉生物科技有限公司 | Methyl cyclopentenolone rearrangement optimization production device and method |
| CN113185390A (en) * | 2021-04-07 | 2021-07-30 | 厦门中坤化学有限公司 | Method for continuously separating propylene glycol methyl ether, cyclopentanone and propylene glycol methyl ether acetate |
| CN114315546B (en) * | 2021-12-18 | 2024-01-23 | 张家港市飞翔环保科技有限公司 | Method for treating waste electronic solvent containing water, propylene glycol methyl ether and cyclopentanone |
| CN114369013B (en) * | 2022-01-25 | 2024-08-02 | 福建钰融科技有限公司 | Method for recovering propylene glycol methyl ether from water-containing waste liquid |
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| CN102617299A (en) * | 2012-03-17 | 2012-08-01 | 江苏怡达化工有限公司 | Continuous production method of electronic-grade propylene glycol monomethyl ether |
| CN203494193U (en) * | 2013-08-22 | 2014-03-26 | 无锡中天固废处置有限公司 | Azeotropic rectifying device for separating propylene glycol monomethyl ether from water |
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