CN102584576A - Method and device for purifying tert-butyl acetate by using partition wall column - Google Patents
Method and device for purifying tert-butyl acetate by using partition wall column Download PDFInfo
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- CN102584576A CN102584576A CN2012100023396A CN201210002339A CN102584576A CN 102584576 A CN102584576 A CN 102584576A CN 2012100023396 A CN2012100023396 A CN 2012100023396A CN 201210002339 A CN201210002339 A CN 201210002339A CN 102584576 A CN102584576 A CN 102584576A
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Abstract
The invention belongs to the technical field of compound separation, and relates to a method for purifying tert-butyl acetate by using a partition wall column, and a separation device. The method is particularly suitable for purification that tert-butyl acetate is prepared from acetic acid and isobutene by a direct conversion method; the method is characterized in that tert-butyl acetate inlet materials enter the partition wall column from an area II and are separated; recovered gas phase on the top of an area I is condensed into liquid by a condenser, and the liquid enters a return tank, the liquid phase is boosted by a pump, a part of the boosted liquid phase, which is used as a light component is recovered, and the residual boosted liquid phase which is used as returned flow is returned to the top of the area I; and a part of liquid phase at the bottom of an area IV is used as an acetic acid component and is recovered, a part of liquid phase at the bottom of an area IV is heated by a reboiler and then is returned to the column, and the tert-butyl acetate is recovered in the middle of an area III. The purity of tert-butyl acetate after separation can reach over 99 weight percent, even over 99.5 weight percent, and the energy consumption and equipment number of the method are greatly reduced compared with those of the dealcoholization column and refining column schemes in the conventional process.
Description
Technical field
The invention belongs to the compound separation technical field, relate to and utilize the method for dividing wall column purification tert-butyl acetate to relate to tripping device, being specially adapted to acetic acid and iso-butylene is raw material, adopts direct conversion method to produce the purification of tert-butyl acetate.
Background technology
Mixture separation is the committed step of Chemical Manufacture, and facility investment and operation energy consumption are the key indexs of extensive sepn process.At present, along with the energy and price of steel product rise steadily, seek the minimum separation method of investment and energy consumption and seem particularly important.
Tert-butyl acetate is extensive day by day in the application in fields such as coating, solvent and medicine intermediate, and its demand also significantly improves.At present, tert-butyl acetate is a raw material with acetic acid and iso-butylene usually, adopts direct conversion method production, and in this method, tert-butyl acetate is purified to be needed can meet the demands through extracting tower, dealcoholize column with after treating tower separates, and its energy consumption is higher, and flow process is longer, and equipment is more.
Summary of the invention
The objective of the invention is to improve, a kind of economical and practical tert-butyl acetate method of purification and device of rationally holding concurrently is provided to the shortcoming and the problem that exist in the background technology.
Technical scheme of the present invention:
1. tert-butyl acetate purifying plant
In the vertical direction of common rectifying tower one partition wall is installed, tower is divided into four parts.Wherein the I zone is positioned at partition wall top, and 1 gaseous phase outlet and 1 reflux inlet are arranged, and 1 liquid phase distributor is arranged at the bottom, is used to control II zone and III zone backflow ratio; The II zone is positioned at partition wall one side, and 1 opening for feed is arranged; The III zone is positioned at the partition wall opposite side, has 1 to extract mouth out; The IV zone is positioned at the partition wall bottom, has 1 liquid phase to extract mouth and 1 gas phase return port out, and 1 gas phase sparger is arranged at the top, is used to control II zone and III zone rising gas phase ratio.
2.
The technical scheme of purification tert-butyl acetate:
The tert-butyl acetate charging is sent into dividing wall column II zone by opening for feed and is carried out prefrationation, and wherein required gas phase of stripping section and the required liquid phase of rectifying section are provided by I zone bottom liquid phases and top, IV zone gas phase respectively; Top, II zone gas phase gets into the further rectifying of I zone, with separating of realization light constituent and tert-butyl acetate component, wherein; The I zone is a rectifying section, and the top gas phase gets into return tank by the gaseous phase outlet extraction after condenser condenses is liquid; Its liquid phase is after pump boosts; A part is as the light constituent extraction, and all the other return top, I zone as refluxing by reflux inlet, and it is stripping section that III extracts mouthful top out in the zone; Its required gas phase provides by rising gas phase on the extraction mouthful bottom, and the tert-butyl acetate component is by extracting a mouthful extraction out; II zone bottom liquid phases gets into the further rectifying of IV zone, with separating of realization tert-butyl acetate component and acetic acid component, wherein; The IV zone is a stripping section; Required rising gas phase is provided by reboiler, and acetic acid component is extracted a mouthful extraction out by IV zone bottom liquid phases, and it is rectifying section that III extracts a mouthful bottom out in the zone; Its required backflow provides by extracting a mouthful top decline liquid phase out, and the tert-butyl acetate component is by extracting a mouthful extraction out.
Advantage of the present invention and beneficial effect:
The purity that the present invention separates the back tert-butyl acetate can reach more than the 99wt%, even can surpass 99.5wt%, and energy consumption and number of devices all have bigger reduction respectively than dealcoholize column in the traditional process and treating tower scheme.
Its processing condition are seen table 1
Description of drawings
The purify process flow sheet of tert-butyl acetate of Fig. 1.
Fig. 2 tert-butyl acetate device synoptic diagram of purifying.
The process flow sheet of Fig. 3 Comparative Examples.
Identify among Fig. 1:
1-1 dividing wall column 1-2 condensing surface 1-3 return tank 1-4 reflux pump 1-5 reboiler 1-6 tert-butyl acetate charging 1-7 light constituent 1-8 tert-butyl acetate component 1-9 acetic acid component.
Identify among Fig. 2:
2-1 gaseous phase outlet 2-2 reflux inlet 2-3 opening for feed 2-4 extracts a mouthful 2-5 liquid phase out and extracts mouthful 2-12 IV zone, 2-11 III zone, 2-10 II zone, a 2-6 gas phase return port 2-7 liquid phase distributor 2-8 gas phase sparger 2-9 I zone 2-13 partition wall out.
Identify among Fig. 3:
3-1 dealcoholize column 3-2 dealcoholize column condensing surface 3-3 dealcoholize column return tank 3-4 dealcoholize column reflux pump 3-5 dealcoholize column reboiler 3-6 dealcoholysis column bottoms pump 3-7 treating tower 3-8 treating tower condensing surface 3-9 treating tower return tank 3-10 treating tower reflux pump 3-11 treating tower reboiler 3-12 tert-butyl acetate charging 3-13 light constituent 3-14 tert-butyl acetate component 3-15 acetic acid component.
Embodiment
As shown in Figure 1, purification tert-butyl acetate device of the present invention is installed a partition wall in the vertical direction of common rectifying tower, and tower is divided into four parts.Wherein the I zone is positioned at partition wall top, and 1 gaseous phase outlet and 1 reflux inlet are arranged, and 1 liquid phase distributor is arranged at the bottom, is used to control II zone and III zone backflow ratio; The II zone is positioned at partition wall one side, and 1 opening for feed is arranged; The III zone is positioned at the partition wall opposite side, has 1 to extract mouth out; The IV zone is positioned at the partition wall bottom, has 1 liquid phase to extract mouth and 1 gas phase return port out, and 1 gas phase sparger is arranged at the top, is used to control II zone and III zone rising gas phase ratio.
The tert-butyl acetate charging gets into dividing wall column by the II zone and separates; I district top extraction gas phase gets into return tank after condenser condenses is liquid, its liquid phase is after pump boosts, and a part is as the light constituent extraction; All the other return top, I zone as backflow; An IV zone bottom liquid phases part is as the acetic acid component extraction, and a part is returned tower after the reboiler heating, III zone middle part extraction tert-butyl acetate component.
Embodiment
Tert-butyl acetate charging (iso-butylene 0.02wt%, C
8Alkene 2.9wt%; Trimethyl carbinol 15.3wt%, tert-butyl acetate 73.4wt%, acetic acid 8.38wt%) 270kg/h; 60 ℃ get into dividing wall column II zone and carry out prefrationation; II zone top gas phase and bottom liquid phases get into bottom, I zone and the IV zone further rectifying in top, light constituent (iso-butylene 0.1wt%, C respectively
8Alkene 13.9wt%, trimethyl carbinol 75.2wt%, tert-butyl acetate 10.8wt%) 54.5kg/h is by the return tank extraction; Acetic acid component (tert-butyl acetate 9.1wt%; Acetic acid 90.9wt%) 24.5kg/h is by the bottom extraction of IV zone, tert-butyl acetate component (tert-butyl acetate 99.6wt%, acetic acid 0.1wt%; Trimethyl carbinol 0.2wt%, C
8Alkene 0.1wt%) 191kg/h extracts a mouthful extraction out by the III zone.Wherein the overhead condensation load is 80972kcal/h, and the load that boils again at the bottom of the tower is 86703kcal/h, and tower diameter is DN400mm.Its processing condition are as shown in table 2.
Comparative Examples
As comparing; Adopt dealcoholize column and treating tower flow process to carry out the tert-butyl acetate purification, flow process is as shown in Figure 2, and the tert-butyl acetate charging is introduced into dealcoholize column and carries out separating of light constituent and tert-butyl acetate component and acetic acid component; Return tank of top of the tower extraction light constituent, the liquid phase extraction gets into treating tower at the bottom of the tower.Treating tower carries out separating of tert-butyl acetate component and acetic acid component, its cat head extraction tert-butyl acetate component, extraction acetic acid component at the bottom of the tower.Under identical feed conditions and separation requirement, dealcoholize column overhead condensation load is 60262kcal/h, and the load that boils again at the bottom of the tower is 66340kcal/h, and tower diameter is DN350mm, and number of theoretical plate is 24.Treating tower overhead condensation load is 37022kcal/h, and the load that boils again at the bottom of the tower is 35959kcal/h, and tower diameter is DN250mm, and number of theoretical plate is 24.Obviously again under the same terms, utilize dividing wall column to carry out the method and apparatus energy consumption low 15% that tert-butyl acetate is purified.See table 3 for details.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; Be not that design of the present invention and scope are limited; Under the prerequisite that does not break away from design philosophy of the present invention, engineering technical personnel make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention; The technology contents that the present invention asks for protection all is documented in claims.
Claims (4)
1. a method of utilizing dividing wall column purification tert-butyl acetate is characterized in that the tert-butyl acetate charging gets into dividing wall column by the II zone and separates, and I district top extraction gas phase gets into return tank after condenser condenses is liquid; Its liquid phase is after pump boosts; A part is as the light constituent extraction, and all the other return top, I zone as backflow, and an IV zone bottom liquid phases part is as the acetic acid component extraction; A part is returned tower after the reboiler heating, III zone middle part extraction tert-butyl acetate component
Implement the described dividing wall column purification tert-butyl acetate device that utilizes of claim 1, it is characterized by in the vertical direction of common rectifying tower one partition wall is installed, tower is divided into four parts.
2. wherein the I zone is positioned at partition wall top, and 1 gaseous phase outlet and 1 reflux inlet are arranged, and 1 liquid phase distributor is arranged at the bottom; The II zone is positioned at partition wall one side, and 1 opening for feed is arranged; The III zone is positioned at the partition wall opposite side, has 1 to extract mouth out; The IV zone is positioned at the partition wall bottom, has 1 liquid phase to extract mouth and 1 gas phase return port out, and 1 gas phase sparger is arranged at the top.
3. the 1 described method of utilizing dividing wall column purification tert-butyl acetate as requested is characterized in that the composition requirement of described tert-butyl acetate charging, light constituent, acetic acid component and tert-butyl acetate component is:
The tert-butyl acetate charging comprises iso-butylene, C
8Alkene, the trimethyl carbinol, tert-butyl acetate and acetic acid, its composition requirement is following:
(1) tert-butyl acetate content>60wt%,
(2) iso-butylene+C
8Alkene+trimethyl carbinol total content<30%, and iso-butylene content<1wt%, C
8Olefin(e) centent<5wt%,
(3) acetic acid content < 30wt%;
Light constituent comprises iso-butylene, C
8Alkene, the trimethyl carbinol and the little acetic acid tert-butyl ester, its composition requirement are tert-butyl acetate content<c
8Olefin(e) centent;
Acetic acid component mainly comprises acetic acid and tert-butyl acetate, and its composition requirement is tert-butyl acetate content < 10wt%;
The tert-butyl acetate composition requirement is a tert-butyl acetate content>99wt%.
4. according to the described method of utilizing dividing wall column purification tert-butyl acetate of claim 1; It is characterized in that described tert-butyl acetate charging is between the 4th ~ 14 theoretical stage in II zone; Tert-butyl acetate is extracted out between the 6th ~ 13 theoretical stage in III zone, and reflux ratio is 12 ~ 18, and tower top temperature is 80 ~ 90 ℃; 117 ~ 137 ℃ of column bottom temperatures, tower top pressure are 0 ~ 0.1MPa; Several 8 ~ 14 of I Region Theory plate, several 14 ~ 18 of II Region Theory plate, several 14 ~ 18 of III Region Theory plate, several 8 ~ 14 of IV Region Theory plate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104797551A (en) * | 2012-09-28 | 2015-07-22 | 陶氏环球技术有限公司 | Process for the production of high purity glycol esters |
| CN107438470A (en) * | 2015-04-03 | 2017-12-05 | 株式会社Lg化学 | Distilling apparatus |
| CN110114335A (en) * | 2016-12-21 | 2019-08-09 | 巴斯夫欧洲公司 | The method of pure (methyl) tert-butyl acrylate is separated by distillation out from thick (methyl) tert-butyl acrylate |
| CN111375219A (en) * | 2018-12-31 | 2020-07-07 | 中国石油化工股份有限公司 | Dividing wall tower and dividing wall rectification method |
| CN112552174A (en) * | 2020-12-23 | 2021-03-26 | 江门谦信化工发展有限公司 | Device and method for rectifying acetic ester |
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| JP2003080002A (en) * | 2001-09-11 | 2003-03-18 | Sumitomo Heavy Ind Ltd | Distillation apparatus and distilling method |
| CN1467202A (en) * | 2002-06-14 | 2004-01-14 | Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column | |
| JP2004089873A (en) * | 2002-08-30 | 2004-03-25 | Sumitomo Heavy Ind Ltd | Distillation apparatus and method |
| CN101417930A (en) * | 2008-11-28 | 2009-04-29 | 湖南阿斯达生化科技有限公司 | Method and apparatus for separating and purifying ethyl vanillin by decompression and continuous distillation in dividing wall column |
| CN101675022A (en) * | 2007-03-23 | 2010-03-17 | 巴斯夫欧洲公司 | Method for the recovery of maleic anhydride by distillation |
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2012
- 2012-01-06 CN CN2012100023396A patent/CN102584576A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003080002A (en) * | 2001-09-11 | 2003-03-18 | Sumitomo Heavy Ind Ltd | Distillation apparatus and distilling method |
| CN1467202A (en) * | 2002-06-14 | 2004-01-14 | Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column | |
| JP2004089873A (en) * | 2002-08-30 | 2004-03-25 | Sumitomo Heavy Ind Ltd | Distillation apparatus and method |
| CN101675022A (en) * | 2007-03-23 | 2010-03-17 | 巴斯夫欧洲公司 | Method for the recovery of maleic anhydride by distillation |
| CN101417930A (en) * | 2008-11-28 | 2009-04-29 | 湖南阿斯达生化科技有限公司 | Method and apparatus for separating and purifying ethyl vanillin by decompression and continuous distillation in dividing wall column |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104797551A (en) * | 2012-09-28 | 2015-07-22 | 陶氏环球技术有限公司 | Process for the production of high purity glycol esters |
| CN107438470A (en) * | 2015-04-03 | 2017-12-05 | 株式会社Lg化学 | Distilling apparatus |
| CN110114335A (en) * | 2016-12-21 | 2019-08-09 | 巴斯夫欧洲公司 | The method of pure (methyl) tert-butyl acrylate is separated by distillation out from thick (methyl) tert-butyl acrylate |
| CN111375219A (en) * | 2018-12-31 | 2020-07-07 | 中国石油化工股份有限公司 | Dividing wall tower and dividing wall rectification method |
| CN111375219B (en) * | 2018-12-31 | 2022-02-08 | 中国石油化工股份有限公司 | Dividing wall tower and dividing wall rectification method |
| CN112552174A (en) * | 2020-12-23 | 2021-03-26 | 江门谦信化工发展有限公司 | Device and method for rectifying acetic ester |
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Application publication date: 20120718 |