CN103396290A - Novel process for separating ethylene glycol and 1,2-butanediol - Google Patents
Novel process for separating ethylene glycol and 1,2-butanediol Download PDFInfo
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- CN103396290A CN103396290A CN2013102836969A CN201310283696A CN103396290A CN 103396290 A CN103396290 A CN 103396290A CN 2013102836969 A CN2013102836969 A CN 2013102836969A CN 201310283696 A CN201310283696 A CN 201310283696A CN 103396290 A CN103396290 A CN 103396290A
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Abstract
The invention discloses a method for separating an azeotropic mixture of ethylene glycol and 1,2-butanediol through azeotropic distillation. Through ASPEN modeling and simulation, an entrainer is selected and a rectification condition is determined. The whole separating process comprises the following step of: adding a polyhydric alcohol mixture and the entrainer into an azeotropic rectification tower to obtain the ethylene glycol and the entrainer at the top of the tower and the 1,2-butanediol at the bottom of the tower. The entrainer is incompatible with polyhydric alcohols, thus high-purity ethylene glycol can be obtained after the entrainer and the polyhydric alcohols are layered. When the entrainer is used for rectifying, the amount of tower plates of the azeotropic rectification tower is 30-120; and through normal pressure or reduced pressure rectification operation under the rectification condition that the reflux ratio is 5-30, the mixture of the ethylene glycol and the 1,2-butanediol can be well separated, and the purity of a butanediol separating product can be up to over 98%.
Description
Technical field
A kind of method that the present invention relates to azeotropic distillation is separated ethylene glycol and 1,2-mixture of butanediols, obtains the novel method of ethylene glycol product, belongs to the separation field in chemical engineering.
Background technology
Along with destruction and the exhaustion of global environment and the energy, we can open from this way of heat recovery the new gate of Economic development, not only can protection of the environment and the energy, and can newly increase some newborn enterprises.It is promising that the biological fermentation treatment solution separates alcohol, it is the production technique of necessity of following chemical industry, both at home and abroad also in the project of Gong the suitability for industrialized production of the similar energy cycling and reutilization of research, be ethylene glycol as corn fermentation liquid through the thick product of dehydration, cracking and initial gross separation, 1, the mixture of 2-butyleneglycol, wherein ethylene glycol, for the production of vibrin, Synolac, softening agent, frostproofer, also is used for makeup and explosive; As analytical reagent, stratographic analysis reagent and capacitor dielectric.Also can be used for producing its minute synthetic resins, solvent, lubricant, tensio-active agent, tenderizer, moistening agent, explosive etc.And butyleneglycol also has higher economic worth.Therefrom isolate the method for heavy constituent ethylene glycol, have important economic worth and realistic meaning.
Summary of the invention
, for the deficiencies in the prior art, the object of the present invention is to provide the novel method of the ethylene glycol in a kind of azeotropic distillation separating ethylene glycol and 1,2-mixture of butanediols.
The present invention is achieved by the following scheme: adopt azeotropic distillation, select suitable entrainer to come ethylene glycol and 1,2-butyleneglycol are separated., to azeotropic distillation, can select to be rich in entrainer backflow or entrainer and stock blend and jointly form backflow with definite composition, so reflux ratio and form affects change in concentration at the bottom of liquid phase distribution and tower top in tower, tower to a great extent., by the adjusting to the heterogeneous azeotropic rectification reflux ratio, can obtain desirable separating effect.It is simple that heterogeneous azeotropic rectification has equipment, can separate multicomponent mixture by single tower, and highly versatile, have reflux ratio operation strategy more flexibly, and the very large advantages such as turndown ratio are arranged.
The present invention is used one or more in toluene, ethylbenzene, dimethylbenzene, diethylbenzene, many carbon alkanes, ether compound, ketone compounds as extraction agent, has tentatively determined azeotrope composition, azeotropic point and the separation sequence of experiment system by ASPENPLUS.Azeotropy rectification column is by following conditional operation, and in overhead mixture, the content of ethylene glycol is 64.8001%-93.6590% under normal pressure or decompression, and reflux ratio is set in 5-30, and by overhead extraction ethylene glycol and the entrainer of rectifying tower, at the bottom of tower, extraction 1, the 2-butyleneglycol.Because entrainer and ethylene glycol do not dissolve each other, directly recycling use of entrainer.
Idiographic flow (seeing accompanying drawing 1): ethylene glycol-1,2-butyleneglycol-entrainer mixture enters rectifying tower, the tower top azeotrope is after condenser is cooling, the extraction of partial reflux part, reflux ratio is 5-30, collect azeotropic mixture after extraction, by quantizer, isolate ethylene glycol and entrainer, entrainer can continue to use.It is qualified 1 finally to obtain at the bottom of tower, 2-butyleneglycol product.Rectifying tower operation under normal pressure or decompression can obtain good separating effect.
The invention has the advantages that and adopt entrainer and ethylene glycol to form azeotrope, relative volatility and the boiling-point difference of azeotrope and 1,2-butyleneglycol are larger, thereby isolate highly purified ethylene glycol and 1,2-butyleneglycol product.It is simple that azeotropic distillation has equipment, can separate multicomponent mixture by single tower, and highly versatile, have reflux ratio operation strategy more flexibly, and the very large advantages such as turndown ratio are arranged.
Description of drawings
Fig. 1 is the rectifier unit schematic diagram
Embodiment
Experiment is made tower reactor with the 1000mL there-necked flask, with electric heating cover, heats.The intermittent azeotropic rectifying tower that adopts is that internal diameter is the glass column of 30mm, inner stainless steel Dixon ring filler of filling 3mm * 3mm, and the packing layer total height is 0.95m, and being equivalent to stage number is 38, and tower top dress spherical condensation tube, use water cooling.At first from disposable charging at the bottom of tower, raw material is ethylene glycol-1, and the mixture of 2-butyleneglycol-entrainer (wherein contains ethylene glycol: 1, the 2-butyleneglycol: entrainer=6:1:12), the normal temperature charging, start heating, the tower reactor temperature maintains 170 degrees centigrade of left and right, material steam after overhead condenser is cooling, total reflux 20min, then partial reflux, the part extraction, reflux ratio is 10:1, slips out in thing and does not contain 1,2-butyleneglycol.Obtain product ethylene glycol after the effluent layering, its content is 99.9257%.
The inventive method is not subjected to the restriction of above-mentioned concrete device, according to this patent, carries out concrete adjustment of technology or conversion, by treatment capacity, amplifies, carries out lab scale, pilot scale and suitability for industrialized production according to this patent requirement and all belong to the behavior of the infringement of patent.
Claims (8)
1. a heterogeneous azeotropic rectification separating ethylene glycol and 1, the method of 2-mixture of butanediols, step is as follows: polyol blends and extraction agent add in azeotropy rectification column, the azeotrope that overhead extraction ethylene glycol and extraction agent form, isolated entrainer and ethylene glycol layering, entrainer can be reused, and contains ethylene glycol more than 93% in the azeotrope that finally obtains.
2., according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, it is characterized in that: described polyol blends ethylene glycol and 1,2-butyleneglycol massfraction are than being 3:1-8:1.
3. according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, it is characterized in that the extraction agent that uses is one or more in toluene, ethylbenzene, dimethylbenzene, diethylbenzene, many carbon alkanes, ether compound, ketone compounds, its addition is 1-5 times of ethylene glycol.
4. according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, the reflux ratio that it is characterized in that the overhead extraction mixture is 5-30.
5. according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, the stage number that it is characterized in that azeotropy rectification column is the 30-120 piece.
6., according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, it is characterized in that azeotropy rectification column is operating as normal pressure or rectification under vacuum.
7., according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, it is characterized in that tower top obtains ethylene glycol and entrainer, entrainer and polyvalent alcohol are incompatible, can obtain highly purified ethylene glycol after layering.
8., according to the method for heterogeneous azeotropic rectification separating ethylene glycol claimed in claim 1, it is characterized in that utilizing the method to carry out lab scale, pilot scale and suitability for industrialized production.
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| CN2013102836969A CN103396290A (en) | 2013-07-08 | 2013-07-08 | Novel process for separating ethylene glycol and 1,2-butanediol |
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| CN2013102836969A CN103396290A (en) | 2013-07-08 | 2013-07-08 | Novel process for separating ethylene glycol and 1,2-butanediol |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664516A (en) * | 2013-11-29 | 2014-03-26 | 中国五环工程有限公司 | Ethanediol separation process for preparing ethanediol from synthetic gas |
| CN104370696A (en) * | 2014-10-21 | 2015-02-25 | 吉林化工学院 | Novel method for separating ethylene glycol and 1,2-pentanediol |
| CN104926608A (en) * | 2014-03-17 | 2015-09-23 | 中国石油化工股份有限公司 | Method for separating ethylene glycol and 1,2-butanediol |
| WO2016097064A1 (en) * | 2014-12-18 | 2016-06-23 | Shell Internationale Research Maatschappij B.V. | Process for the separation of glycols |
| CN106132912A (en) * | 2014-04-02 | 2016-11-16 | 国际壳牌研究有限公司 | For separating monoethylene glycol and the method for 1,2 butanediols |
| CN106938973A (en) * | 2017-03-28 | 2017-07-11 | 青岛科技大学 | A kind of method of single column heterogeneous azeotropic rectification separation aniline and ethylene glycol azeotropic mixture |
| US9718752B2 (en) | 2013-05-31 | 2017-08-01 | Shell Oil Company | Process for the separation of an alkylene glycol |
| US9932284B2 (en) | 2013-05-31 | 2018-04-03 | Shell Oil Company | Process for the separation of 1,4-butanediol and co-products |
| US10099980B2 (en) | 2013-05-31 | 2018-10-16 | Shell Oil Company | Glycol recovery with solvent extraction |
| CN112538002A (en) * | 2020-12-08 | 2021-03-23 | 天津天南同创科技发展有限公司 | Process method for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
| CN114591145A (en) * | 2022-03-25 | 2022-06-07 | 广西科技大学 | Method for separating dihydric fusel from ethylene glycol by double-solvent synergistic extraction |
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| CN102372596A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing glycol product by separating synthetic gas |
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2013
- 2013-07-08 CN CN2013102836969A patent/CN103396290A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102372596A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing glycol product by separating synthetic gas |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10099980B2 (en) | 2013-05-31 | 2018-10-16 | Shell Oil Company | Glycol recovery with solvent extraction |
| US9718752B2 (en) | 2013-05-31 | 2017-08-01 | Shell Oil Company | Process for the separation of an alkylene glycol |
| US9932284B2 (en) | 2013-05-31 | 2018-04-03 | Shell Oil Company | Process for the separation of 1,4-butanediol and co-products |
| CN103664516B (en) * | 2013-11-29 | 2015-08-05 | 中国五环工程有限公司 | The ethylene glycol separating technology of synthetic gas preparing ethylene glycol |
| CN103664516A (en) * | 2013-11-29 | 2014-03-26 | 中国五环工程有限公司 | Ethanediol separation process for preparing ethanediol from synthetic gas |
| CN104926608A (en) * | 2014-03-17 | 2015-09-23 | 中国石油化工股份有限公司 | Method for separating ethylene glycol and 1,2-butanediol |
| CN104926608B (en) * | 2014-03-17 | 2017-04-12 | 中国石油化工股份有限公司 | Method for separating ethylene glycol and 1,2-butanediol |
| CN106132912B (en) * | 2014-04-02 | 2018-05-11 | 国际壳牌研究有限公司 | Method for separating monoethylene glycol and 1,2- butanediols |
| CN106132912A (en) * | 2014-04-02 | 2016-11-16 | 国际壳牌研究有限公司 | For separating monoethylene glycol and the method for 1,2 butanediols |
| US10221116B2 (en) | 2014-04-02 | 2019-03-05 | Shell Oil Company | Process for the separation of monoethylene glycol and 1,2-butanediol |
| CN104370696A (en) * | 2014-10-21 | 2015-02-25 | 吉林化工学院 | Novel method for separating ethylene glycol and 1,2-pentanediol |
| WO2016097064A1 (en) * | 2014-12-18 | 2016-06-23 | Shell Internationale Research Maatschappij B.V. | Process for the separation of glycols |
| CN107001206A (en) * | 2014-12-18 | 2017-08-01 | 国际壳牌研究有限公司 | Method for separating glycol |
| CN107001206B (en) * | 2014-12-18 | 2021-04-23 | 国际壳牌研究有限公司 | Process for separating diols |
| CN106938973A (en) * | 2017-03-28 | 2017-07-11 | 青岛科技大学 | A kind of method of single column heterogeneous azeotropic rectification separation aniline and ethylene glycol azeotropic mixture |
| CN112538002A (en) * | 2020-12-08 | 2021-03-23 | 天津天南同创科技发展有限公司 | Process method for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
| CN112538002B (en) * | 2020-12-08 | 2023-03-21 | 天津天南同创科技发展有限公司 | Process method for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
| CN114591145A (en) * | 2022-03-25 | 2022-06-07 | 广西科技大学 | Method for separating dihydric fusel from ethylene glycol by double-solvent synergistic extraction |
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Application publication date: 20131120 |