CN105906471A - Continuous separation method of m-xylene-ethylene glycol mixture by azeotropic distillation - Google Patents
Continuous separation method of m-xylene-ethylene glycol mixture by azeotropic distillation Download PDFInfo
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- CN105906471A CN105906471A CN201610346563.5A CN201610346563A CN105906471A CN 105906471 A CN105906471 A CN 105906471A CN 201610346563 A CN201610346563 A CN 201610346563A CN 105906471 A CN105906471 A CN 105906471A
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- China
- Prior art keywords
- xylene
- tower
- ethylene glycol
- azeotropic distillation
- 1bar
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- 238000010533 azeotropic distillation Methods 0.000 title claims abstract description 16
- 239000000203 mixture Substances 0.000 title claims abstract description 14
- 238000000926 separation method Methods 0.000 title abstract description 8
- NWMVZMSDIREKNH-UHFFFAOYSA-N ethane-1,2-diol;1,3-xylene Chemical compound OCCO.CC1=CC=CC(C)=C1 NWMVZMSDIREKNH-UHFFFAOYSA-N 0.000 title abstract 3
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005191 phase separation Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 6
- BMWJQXGRRAAJNA-UHFFFAOYSA-N ethane-1,2-diol;1,2-xylene Chemical compound OCCO.CC1=CC=CC=C1C BMWJQXGRRAAJNA-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 33
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- 229920004934 Dacron® Polymers 0.000 description 1
- 240000000233 Melia azedarach Species 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical group O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000003230 hygroscopic agent Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- 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
- C07C7/06—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by azeotropic distillation
-
- 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
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic 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)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a continuous separation method of m-xylene-ethylene glycol mixture by azeotropic distillation, and belongs to the field of m-xylene-ethylene glycol azeotropic mixture separation. According to the method, operation parameters can be optimized, so that energy consumption and investment can be reduced while the product quality is improved; a continuous operation mode can be selected under the condition of a large production scale, so that the product quality can be stabilized, benefits can be increased, and labor cost can be reduced; regarding innovation of azeotrope agents, water is adopted as an azeotrope agent; and the method can be used for preparing high-purity m-xylene and ethylene glycol to ensure the product quality, and drained wastewater can achieve the draining standard in one time.
Description
Technical field
The present invention relates to the separation field of meta-xylene-ethylene glycol mixture, especially relate to the continuous azeotropic distillation separation method of a kind of meta-xylene-ethylene glycol mixture.
Background technology
Solvent that meta-xylene and ethylene glycol all chemical industry and pharmaceutical field are conventional or raw material, and consumption is the hugest.Between two for medicine, spice and dyestuff intermediate raw material and cinecolour solvent-soluble color coupler, also serve as the raw material manufacturing M-phthalic acid.Ethylene glycol is mainly used in polyester dacron processed, polyester resin, hygroscopic agent, plasticizer, surfactant, synthetic fibers, cosmetics and explosive, and it is used as the solvent of dyestuff, ink etc., the antifreeze of preparation electromotor, gas dewatering agent, manufactures resin, can also be used for the wetting agent of cellophane, fiber, leather, binding agent；Can produce synthetic resin PET, fiber level PET i.e. polyster fibre, bottle sheet level PET is used for making mineral water bottle etc.；Also can produce alkyd resin, Biformyl etc., also serve as antifreezing agent.
Substantially azeotropic distillation and extracting rectifying it is divided into currently for azeotropic system separation means, and for azeotropic distillation, the most continuous and two kinds of modes of operation of interval in mode of operation.The operating mode that azeotropic distillation technique under Lian Xucaozuo is big mainly for yield, automatic control level is high, constant product quality is high, intermittently operated mainly uses the highest with output demand, and automatic control level is required low operation operating mode.
Chinese patent CN102952004 A proposes the process of a kind of continuous azeotropic distillation separation glycol monoethyl ether-water, and in this technique, entrainer disposably adds in still, uses universal double tower reflux technique.This invention subject matter is: first patent specification does not mention the compensation problem of entrainer, owing to the continuous operation cycle is longer, partially azeotropic agent can be run off along with the extraction of product, and in causing system, entrainer content constantly reduces, and the difficult quality guarantee causing product is stable；Furthermore this technique is according to traditional reflux type, causes the increase of energy consumption；In addition this technique does not mention whether the discharge of entrainer recovery tower tower reactor water reaches discharge standard.
Currently, with respect to the separation of meta-xylene-ethylene glycol azeotropic mixture, the most relevant document is delivered or reports.
Summary of the invention
The invention aims to overcome present in existing technique not enough, and for meta-xylene-ethylene glycol mixture, propose a kind of to be suitable for major part operating mode, product purity is high, production stability is strong technique.
For solving above-mentioned technical problem, the technical solution used in the present invention is a kind of method of continuous azeotropic distillation compartment dimethylbenzene-ethylene glycol mixture, and the method uses seriality operation；Meanwhile, in the innovation of entrainer, the present invention adopts and uses water as entrainer；In product quality, the method can obtain high-purity meta-xylene, ethylene glycol product, and the waste water of discharge disposably reaches the standard of discharge.
The method of a kind of continuous azeotropic distillation compartment dimethylbenzene-ethylene glycol mixture described in technique scheme, its capital equipment related to: azeotropy rectification column, phase separation tank, dehydrating tower, reboiler, condenser etc..
This technical scheme equipment with the on-link mode (OLM) of stream stock is: entrainer adds (the 1st block of column plate) from azeotropic distillation top of tower, and raw material adds from the middle and upper part of tower；Overhead vapours enters after condenser (gas phase fraction is 0), enter phase separation tank, phase separation tank upper strata oil reservoir is drawn product meta-xylene, lower aqueous layer enters dehydrating tower top (the 1st block of column plate), dehydration column overhead steam enters condenser, after condensed device, is back to phase separation tank, meta-xylene is reclaimed, at the bottom of tower, discharges pure water.
The equipment of this technical scheme and technological parameter be: the azeotropy rectification column number of plates 20 ~ 40, and entrainer inlet amount and feedstock amount ratio is for 2.44:1 ~ 4:1, tower top operation pressure 1bar(absolute pressure, and hereafter involved pressure is absolute pressure in the case of not having specified otherwise)；It is 1bar that overhead condenser 1 operates pressure, and gas phase fraction is 0；Phase separation tank operation pressure is 1bar；The dehydrating tower number of plates 10 ~ 20, tower top operation pressure is 1bar；It is 1bar that overhead condenser 2 operates pressure, and gas phase fraction is 0.
Preferably, when the azeotropy rectification column number of plates is 25 ~ 30, and the dehydrating tower number of plates reaches 15 ~ 20, this technique can purity higher than 99.99% meta-xylene and ethylene glycol product, and the water of dehydrating tower tower reactor discharge can reach below 100ppm, directly get to the standard of discharge.
The novelty of the present invention is with advantage:
1) meta-xylene separates with ethylene glycol azeotropic system, there is no separating technology report at present or delivers；
2) azeotropy rectification column, dehydrating tower do not have reflux ratio, it is possible to significantly reduce energy consumption；
3) flow process compares traditional technique, and equipment is simpler, and operation easier is less；
4) water selected by entrainer, nontoxic, and waste water can disposably reach the standard of discharge.
Accompanying drawing explanation
Fig. 1 is continuous azeotropic distillation operation chart.
Detailed description of the invention
The invention will be further described to be below embodied as case for combination, but does not limit the scope of protection of the invention.
Embodiment one
A kind of method of continuous azeotropic distillation compartment dimethylbenzene-ethylene glycol mixture, entrainer consumption is 244kg/h；Feed throughput is 100kg/h, and raw material consists of the azeotropic composition of meta-xylene and ethylene glycol.The azeotropy rectification column number of plates is 30, and entrainer feed entrance point is at the 1st block of column plate, and feedstock position is at 5 blocks of column plates.The ethylene glycol of extraction content >=99.99% at the bottom of azeotropy rectification column tower, enters phase separation tank after overhead vapours is condensed, obtains meta-xylene product content >=99.99%；Aqueous phase containing a small amount of meta-xylene enters dehydrating tower, enters the 1st block of column plate of dehydrating tower；The dehydrating tower number of plates is 20, and the water of tower reactor extraction is almost pure water；And overhead vapours condensed after enter phase separation tank, meta-xylene is reclaimed.
Claims (4)
1. the method for continuous azeotropic distillation compartment dimethylbenzene-alcohol mixture, it is characterized in that: the method for described a kind of continuous azeotropic distillation compartment dimethylbenzene-ethylene glycol mixture, use green non-pollution entrainer, its capital equipment related to: azeotropy rectification column, phase separation tank, dehydrating tower, reboiler, condenser etc..
Method the most according to claim 1, it is characterised in that this technical scheme main flow is: entrainer adds (the 1st block of column plate) from azeotropic distillation top of tower, raw material adds from the middle and upper part of tower；After overhead vapours enters condenser condensation, enter phase separation tank, phase separation tank upper strata oil reservoir is drawn product meta-xylene, lower aqueous layer enters dehydrating tower top (the 1st block of column plate), dehydration column overhead steam enters condenser, after condensed device, is back to phase separation tank, meta-xylene is reclaimed, at the bottom of tower, discharges pure water.
Method the most according to claim 1, it is characterised in that equipment and operating parameter be: the azeotropy rectification column number of plates 20 ~ 40, entrainer inlet amount is 2.44:1 ~ 4:1 with the ratio of feedstock amount, tower top operation pressure 1bar(absolute pressure)；It is 1bar(absolute pressure that overhead condenser 1 operates pressure), gas phase fraction is 0；Phase separation tank operation pressure is 1bar(absolute pressure)；The dehydrating tower number of plates 10 ~ 20, tower top operation pressure is 1bar(absolute pressure)；It is 1bar(absolute pressure that overhead condenser 2 operates pressure), gas phase fraction is 0.
Method the most according to claim 1, the green non-pollution entrainer of selection is water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610346563.5A CN105906471B (en) | 2016-05-24 | 2016-05-24 | A kind of method of continuous azeotropic distillation separation meta-xylene-ethylene glycol mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610346563.5A CN105906471B (en) | 2016-05-24 | 2016-05-24 | A kind of method of continuous azeotropic distillation separation meta-xylene-ethylene glycol mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105906471A true CN105906471A (en) | 2016-08-31 |
| CN105906471B CN105906471B (en) | 2018-11-09 |
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| CN201610346563.5A Active CN105906471B (en) | 2016-05-24 | 2016-05-24 | A kind of method of continuous azeotropic distillation separation meta-xylene-ethylene glycol mixture |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044281A (en) * | 1989-11-06 | 1990-08-01 | 肖藻生 | The synthetic method of diphosphonate ester and application |
| CN1022568C (en) * | 1985-08-09 | 1993-10-27 | 伊莱利利公司 | Synthesis of tricyclazole |
| JP2000034250A (en) * | 1998-07-15 | 2000-02-02 | Nippon Refine Kk | Azeotropic distillation of mixed solution of methyl ethyl ketone, glycol ether and water, and recovery of methyl ethyl ketone and glycol ether using the same |
| CN104313789A (en) * | 2014-03-24 | 2015-01-28 | 长春工业大学 | Method for enhancing mechanical properties of electric spinning membrane |
| CN104326477A (en) * | 2014-10-10 | 2015-02-04 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of ultra-high pure silica sol for capacitor |
| CN105130755A (en) * | 2015-07-24 | 2015-12-09 | 常州大学 | Method of separating mixture of neopentyl glycol and ethylene glycol |
-
2016
- 2016-05-24 CN CN201610346563.5A patent/CN105906471B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1022568C (en) * | 1985-08-09 | 1993-10-27 | 伊莱利利公司 | Synthesis of tricyclazole |
| CN1044281A (en) * | 1989-11-06 | 1990-08-01 | 肖藻生 | The synthetic method of diphosphonate ester and application |
| JP2000034250A (en) * | 1998-07-15 | 2000-02-02 | Nippon Refine Kk | Azeotropic distillation of mixed solution of methyl ethyl ketone, glycol ether and water, and recovery of methyl ethyl ketone and glycol ether using the same |
| CN104313789A (en) * | 2014-03-24 | 2015-01-28 | 长春工业大学 | Method for enhancing mechanical properties of electric spinning membrane |
| CN104326477A (en) * | 2014-10-10 | 2015-02-04 | 东莞市长安东阳光铝业研发有限公司 | Preparation method of ultra-high pure silica sol for capacitor |
| CN105130755A (en) * | 2015-07-24 | 2015-12-09 | 常州大学 | Method of separating mixture of neopentyl glycol and ethylene glycol |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778087A (en) * | 2021-01-14 | 2021-05-11 | 山东科技大学 | Method for separating methanol-toluene azeotrope through continuous extractive distillation |
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| CN105906471B (en) | 2018-11-09 |
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Effective date of registration: 20210528 Address after: 272000 middle section of Wanda West Road, coatings industrial park, Yangying Town, Liangshan County, Jining City, Shandong Province Patentee after: Tongchuang chemical (Shandong) Co.,Ltd. Address before: College of chemistry and chemical engineering, Jinan University, no.336, nanxinzhuang West Road, Shizhong District, Jinan City, Shandong Province, 250022 Patentee before: University of Jinan |
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Denomination of invention: A method for continuous azeotropic distillation separation of xylene ethylene glycol mixture Effective date of registration: 20231221 Granted publication date: 20181109 Pledgee: Shandong Liangshan Rural Commercial Bank Co.,Ltd. Pledgor: Tongchuang chemical (Shandong) Co.,Ltd. Registration number: Y2023980073157 |