CN1305818C - Apparatus for extracting coarse 1,3-butadiene by double baffle plated tower and method thereof - Google Patents
Apparatus for extracting coarse 1,3-butadiene by double baffle plated tower and method thereof Download PDFInfo
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Abstract
The present invention relates to a device and a method thereof for obtaining coarse 1, 3-butadiene by using a double-partition board tower integration process and taking acetonitrile containing water as a solvent for separating butylene from C4 mixtures and removing butyne and recombination parts through extractive distillation. The operation of extractive distillation of the method is carried out in a partition board tower with an upper longitudinal partition board and a lower longitudinal partition board, the inner structure of the partition board tower is divided into a butadiene extractive distillation section, a recombination part removing section, an alkyne extractive distillation section, a middle tower sharing area, a solvent analyzing section, an alkyne distilling section and a lower tower sharing area, wherein liquid phase between the recombination part removing section and the alkyne extractive distillation section is led to a side line tower in order to remove the recombination parts, and the side line tower and relevant components are eliminated when the recombination parts are not removed. The device and the method of the present invention can be used for finishing the operation of traditional twice extractive distillation and partial recombination part removing operation in one tower. The present invention has the advantages of less investment, simple operation and low energy consumption, and thus, the cost of products is reduced.
Description
Technical field:
The present invention relates to a kind of extraction thick 1, the devices and methods therefor of 3-divinyl, specifically make solvent and from C 4 mixture, tell butylene by extracting rectifying and remove butine and the devices and methods therefor of thick 1,3-butadiene is obtained in heavy constituent to contain water-acetonitrile with two partitioned column integrated flows.
Technical background:
Industrial thick 1,3-butadiene obtains from the C 4 mixture cut usually.This mixture main component is 1-butylene, iso-butylene, suitable-2-butylene, anti--2-butylene, 1,3-butadiene and a small amount of ethyl acetylene and vinylacetylene.Can adopt and contain water-acetonitrile and make solvent, obtain thick 1 by twice extracting rectifying (comprising the parsing of extracting rectifying and solvent) back, the 3-divinyl: extracting rectifying separates butylene and divinyl for the first time, extracting rectifying is removed butine and vinylacetylene for the second time, needs 4 towers to finish the extracting rectifying process operation twice usually.If removing heavy constituent also needs one and takes off heavies column.Therefore, there is various, the complicated operation of required equipment in existing method, and energy expenditure is big, the outstanding shortcoming that production cost is high.
Summary of the invention:
In order to overcome the shortcoming of prior art, the present invention adopts two partitioned column integrated flow technology, makes above-mentioned twice extracting rectifying and part take off heavy constituent and operates in the tower and finish.Investment reduces, energy expenditure reduces product cost thereby this method makes.
Extracting rectifying of the present invention operates in the partitioned column with two sections wash plate and carries out, and divider upright is installed, and prevents that the liquid of both sides and vapor generation from laterally mixing.The internal structure of partitioned column is divided into the butadiene extraction rectifying section, take off the reorganization segmentation, alkynes extracting rectifying section, tower zone, shared middle part, solvent are resolved section, the alkynes section of steaming and tower zone, shared bottom; The butadiene extraction rectifying section with take off reorganization segmentation, the alkynes extracting rectifying section wash plate by epimere at interval; Solvent parsing section and the alkynes section of steaming are with the wash plate interval of hypomere, by shared middle part tower interregional separate of the cover plate on the alkynes section of steaming with alkynes section of steaming and top; Be provided with the condenser of raffinating oil on butadiene extraction rectifying section top; Be provided with the crude butadiene condenser taking off reorganization segmentation top, when needs take off heavy constituent, be furnished with the conventional distillation operation that the side line tower realizes taking off heavy constituent taking off reorganization segmentation bottom, the side line tower bottom is provided with and takes off the heavies column reboiler, when not needing to take off heavy constituent, remove side line tower and related accessory; Be provided with intermediate reboiler in tower zone, shared middle part, be provided with the alkynes condenser, to reclaim heat at the entrance of the alkynes section of steaming; Be provided with reboiler in tower zone, shared bottom.
Be equipped with structured packing or tower tray in the tower as internals, the column plate internals without limits.The tower tray of design makes the liquid residence time in the tower be no more than 15 minutes, optimal value 10 minutes.
The present invention is similar to the conventional rectification tower, is provided with overhead condenser and tower still reboiler, can move continuously usually.With theoretical plate number hereinafter for to calculate downwards from cat head.
Extracting method of the present invention is: add moisture acetonitrile solvent logistics on partitioned column butadiene extraction rectifying section top, the middle part adds the mixed c 4 logistics, and gaseous stream, condensing reflux are arranged at the top, and obtain the logistics of raffinating oil based on butylene; The material logistics of drawing of coming out at the bottom of the butadiene extraction rectifying section forms the feed back logistics through intermediate reboiler and enters tower zone, shared middle part, in this section realization heat energy recycle, and has gaseous stream to go alkynes extracting rectifying section; Add moisture acetonitrile solvent logistics on the top of alkynes extracting rectifying section, realize the operation of alkynes extracting rectifying; Gaseous stream, condensing reflux are arranged taking off reorganization segmentation top, and obtain product stream based on divinyl; When needs took off heavy constituent, taking off reorganization segmentation lower end had liquid phase stream to introduce the side line tower, has gaseous stream to return and takes off heavies column, obtains the heavy constituent logistics at the bottom of the side line tower; When not needing to take off heavy constituent, can be without the side line tower; Resolve the operation that section realizes steaming divinyl at solvent; Realize steaming the operation of butine and vinylacetylene in the alkynes section of steaming, gaseous stream, condensing reflux are arranged at the top, carbon four alkynes and the vinylacetylene logistics of liquid phase extraction safety content; Realize steaming of alkynes obtaining the pure solvent logistics in shared bottom tower zone, through recovery of heat and modified after recycling.
According to the present invention, finish the butadiene extraction distillation operation at the butadiene extraction rectifying section, from then on the C 4 mixture cut adds at the section middle part, and moisture acetonitrile solvent adds from top, and four streams are arranged at the top.Moisture acetonitrile solvent add-on is adjusted to 4.1～8.9, optimal value 5.2～7.5 with the ratio of C 4 mixture amount.The trim the top of column amount is adjusted to 2.0～5.2, optimal value 2.3～4.0 with the ratio of produced quantity.Butadiene extraction theoretical number of plates of rectifying section 50～110, optimal value 70～100.The solvent feed plate is positioned at theoretical stage 2～8, optimal value 3～6.C 4 mixture fraction charging theoretical stage 25～60, optimal value 35～50.The cat head working pressure is adjusted to 0.42～0.58MPa (A), optimal value 0.45～0.52MPa (A).The cat head service temperature is adjusted to 35～50 ℃, 40～45 ℃ of optimal values.
According to the present invention, finish the extracting rectifying operation of carbon four alkynes and vinylacetylene in alkynes extracting rectifying section: from then on the butadiene stream of carbon containing four alkynes and vinylacetylene enters this section in the section lower end, and moisture acetonitrile solvent adds from top, and backflow is arranged at the top.Solvent adding amount is adjusted to 1.2～3.3, optimal value 1.5～2.8 with the ratio of crude butadiene amount.Quantity of reflux is adjusted to 2.8～5.4, optimal value 3.0～4.8 with the ratio of cat head produced quantity.This pars infrasegmentalis rising tolerance is adjusted to 0.32～0.65, optimal value 0.39～0.58 with the ratio of shared middle part tower district rising tolerance.The setting of this ratio realizes by column internals or cat head vapor phase stream variable valve.This section number of theoretical plate 50～80, optimal value 40～60.The solvent feed plate is positioned at the side line tower and draws theoretical stage 5～20 under the flitch, optimal value 7～12.
According to the present invention, take off the reorganization segmentation finish heavy constituent 1,2-butylene and the carbon five etc. that remove in the crude butadiene product; Backflow is arranged at this section top, and reflux ratio is adjusted to 3.0～6.2, optimal value 4.0～5.8.This section number of theoretical plate 30～60, optimal value 45～55.The cat head working pressure is adjusted to 0.42～0.58MPa (A), optimal value 0.45～0.52MPa (A).The cat head service temperature is adjusted to 35～50 ℃, 38～43 ℃ of optimal values.
According to the present invention, in the time of need taking off heavy constituent, draw material between reorganization segmentation and the alkynes extracting rectifying section and remove the side line tower taking off, this side line tower is finished the operation of extraction heavy constituent, this tower number of theoretical plate 15～35, optimal value 25～32, the feed liquid phasor of drawing of side line tower accounts for 20%～40% of its upper tray decline amount of liquid phase, optimal value 25%～32%.
According to the present invention, realize operations such as heat recuperation and shunting steam flow in shared middle part tower zone, this section number of theoretical plate 3～10, optimal value 4～8.
According to the present invention, resolve section at solvent and finish the solvent parse operation, promptly from solvent, steam divinyl.This section number of theoretical plate 6～20, optimal value 8～15.
According to the present invention, finish the operation that from solvent, steams butine and vinylacetylene in the alkynes section of steaming.From then on the solvent stream of carbon containing four alkynes and vinylacetylene enters the section lower end, and backflow is arranged at the top, and reflux ratio is adjusted to 3.1～6.5, optimal value 3.5～5.3.The ratio that rises tolerance and shared bottom tower zone rising tolerance on the bottom is adjusted to 0.11～0.25, optimal value 0.12～0.20.The setting of this ratio realizes by column internals or section top vapor phase stream variable valve.This section number of theoretical plate 6～16, optimal value 7～13.
According to the present invention, finish the operation that from solvent, steams butine and vinylacetylene in tower zone, shared bottom, make and obtain qualified circulating solvent at the bottom of the tower.This tower section number of theoretical plate 5～13, optimal value 6～10.
Description of drawings:
Fig. 1 is apparatus of the present invention structural principle synoptic diagram.
Fig. 2 is the structural principle synoptic diagram behind apparatus of the present invention remodeling, the i.e. rough schematic view of device when not needing to be temporarily released from one's regular work the product heavy constituent.
Specific embodiments:
Below by embodiment apparatus of the present invention and method are described further.
Embodiment 1:
Apparatus of the present invention partitioned column 1 internal structure is divided into butadiene extraction rectifying section 5, take off reorganization segmentation 32, alkynes extracting rectifying section 6, tower zone, shared middle part 7, solvent are resolved section 8, the alkynes section of steaming 9 and tower zone, shared bottom 10; Butadiene extraction rectifying section 5 with take off reorganization segmentation 32, alkynes extracting rectifying section 6 wash plate 2 by epimere at interval; Solvent is resolved wash plate 3 intervals of section 8 and the alkynes section of steaming 9 usefulness hypomeres, by upper end cover plate 4 the shared middle part tower zone 7 of the alkynes section of steaming 9 with top is separated; Be provided with the condenser 11 of raffinating oil on butadiene extraction rectifying section 5 tops; Be provided with crude butadiene condenser 12 taking off reorganization segmentation 32 tops, when needs take off heavy constituent, be furnished with the conventional distillation operation that side line tower 33 realizes taking off heavy constituent taking off reorganization segmentation 32 bottoms, side line tower 33 bottoms are provided with takes off heavies column reboiler 37; Be provided with intermediate reboiler 15 in tower zone, shared middle part 10, be provided with alkynes condenser 14 at the entrance of the alkynes section of steaming 9; Be provided with reboiler 15 in tower zone, shared bottom 10.
Be on the 49th theoretical stage of the C 4 mixture stream 17 of 54 ℃ the 12248.87kg/h butadiene extraction rectifying section 5 that adds the partitioned column 1 that has 140 theoretical stages altogether with gaseous form with temperature, moisture acetonitrile solvent logistics 16 joins on the 4th theoretical stage, moisture acetonitrile solvent and C 4 mixture weight ratio are 5.8: 1.0, product considers to remove heavy constituent, adopt Fig. 1 flow process, C 4 mixture has the weight percentage of following composition:
Propane 0.43
Propine 0.38
Normal butane 2.00
Trimethylmethane 0.75
Iso-butylene 18.51
1-butylene 15.53
Instead-2-butylene 4.71
Suitable-2-butylene 3.78
1,3-butadiene 52.04
1 0.01
Ethyl acetylene 0.40
Vinylacetylene 0.59
According to Fig. 1, butadiene extraction rectifying section 5 number of theoretical plates 100, take off reorganization segmentation 32 number of theoretical plates 50, alkynes extracting rectifying section 6 number of theoretical plates 50, tower zone, shared middle part 7 number of theoretical plates 16, solvent is resolved section 8 number of theoretical plates 14, the alkynes section of steaming 9 number of theoretical plates 14, shared bottom tower zone 10 number of theoretical plates 10.Moisture acetonitrile solvent logistics 31 joins on the 67th block of plate, and its amount is 1.9: 1.0 with the ratio of cymogene alkene.The amount of liquid of introducing the side line tower accounts for 27% of dropping liq amount.Butadiene extraction rectifying section 5 tops are all 0.495MPa (A) with the working pressure that takes off reorganization segmentation 32 tops.
Take off the divinyl 6386.68kg/h that reorganization segmentation 32 top obtains not contain heavy constituent, purity 98.88% (wt), the rate of recovery 99.0%, carbon containing four alkynes≤20ppm wherein, vinylacetylene≤5ppm.Butadiene extraction rectifying section 5 tops obtain to raffinate oil 5497.44kg/h, wherein contain divinyl≤100ppm.Obtain to contain water-acetonitrile, hydrocarbon content≤50ppm at the bottom of the tower.Meet the requirement of the refining divinyl of postorder workshop section fully.Tower still reboiler thermal load 2.4755 * 10
4MJ/h.Be equivalent to product crude butadiene per ton (having taken off heavy constituent) and consume steam 1.6129t.
Embodiment 2:
Product does not consider to take off heavy constituent, and the partitioned column structure has been removed side line tower 33 and related accessory, adopts Fig. 2 flow process, and all the other are identical with embodiment 1.
Be on the 36th theoretical stage of the C 4 mixture stream 17 of 54.0 ℃ the 13498.4kg/h butadiene extraction rectifying section 5 that adds the partitioned column that has 100 theoretical stages altogether with gaseous form with temperature, moisture acetonitrile solvent logistics 16 joins on the 4th theoretical stage, moisture acetonitrile solvent and C 4 mixture weight ratio are 5.4: 1.0, and C 4 mixture has the weight percentage of following composition:
Propane 0.5047
Propine 0.1019
Normal butane 1.3094
Trimethylmethane 0.3802
Iso-butylene 23.3535
1-butylene 16.6869
Instead-2-butylene 5.1783
Suitable-2-butylene 3.8939
1,3-butadiene 47.5445
1 0.3046
1-acetylene 0.1278
Vinylacetylene 0.5488
According to Fig. 2, butadiene extraction rectifying section 5 number of theoretical plates 60, alkynes extracting rectifying section 6 number of theoretical plates 50, tower zone, shared middle part 7 number of theoretical plates 16, solvent is resolved section 8 number of theoretical plates 14, the alkynes section of steaming 9 number of theoretical plates 14, shared bottom tower zone 10 number of theoretical plates 10.Moisture acetonitrile solvent logistics 31 joins on the 8th theoretical stage, and its amount is 1.6: 1 with the ratio of cymogene alkene.Butadiene extraction rectifying section 5 tops are all 0.52MPa (A) with the working pressure on alkynes extracting rectifying section 6 tops.Alkynes extracting rectifying section 6 tops obtain crude butadiene 7045.30kg/h, purity 94.24% (wt), the rate of recovery 99.0%.Wherein carbon containing four alkynes≤20ppm, vinylacetylene≤5ppm.Butadiene extraction rectifying section 5 tops obtain to raffinate oil 6652.33kg/h, wherein contain divinyl≤100ppm.Obtain the pure water-acetonitrile that contains, alkynes content≤50ppm at the bottom of the tower.Meet the requirement of the refining divinyl of postorder workshop section fully.Tower still reboiler thermal load 2.780 * 10
4MJ/h.Thick product divinyl quite per ton consumes steam 1.6416t.
The present invention compares with the conventional tower flow process owing to adopt highly integrated partitioned column technology, and investment saves 35%, and cost of energy saves 28%.
Claims (12)
1, a kind of pair of partitioned column extracts thick 1, the device of 3-divinyl is characterized in that the internal structure of partitioned column is divided into the butadiene extraction rectifying section, takes off the reorganization segmentation, alkynes extracting rectifying section, tower zone, shared middle part, solvent resolve section, the alkynes section of steaming and tower zone, shared bottom; The butadiene extraction rectifying section with take off reorganization segmentation, the alkynes extracting rectifying section wash plate by epimere at interval; Solvent parsing section and the alkynes section of steaming separate by the shared middle part tower zone of the cover plate on the alkynes section of steaming with alkynes section of steaming and top with the wash plate interval of hypomere; Be provided with the condenser of raffinating oil on butadiene extraction rectifying section top; Be provided with the crude butadiene condenser taking off reorganization segmentation top, when needs take off heavy constituent, be furnished with the conventional distillation operation that the side line tower realizes taking off heavy constituent taking off reorganization segmentation bottom, the side line tower bottom is provided with and takes off the heavies column reboiler, when not needing to take off heavy constituent, remove side line tower and related accessory; Be provided with intermediate reboiler in tower zone, shared middle part, be provided with the alkynes condenser at the entrance of the alkynes section of steaming; Be provided with reboiler in tower zone, shared bottom.
2, the according to claim 1 pair of partitioned column extracts the device of thick 1,3-butadiene, it is characterized in that divider upright installs, and prevents that the liquid of both sides and vapor generation from laterally mixing.
3, the according to claim 1 pair of partitioned column extracts the device of thick 1,3-butadiene, it is characterized in that being equipped with in the tower structured packing or tower tray as internals, and the tower tray of design makes the liquid residence time in the tower be no more than 15 minutes.
4, a kind of pair of partitioned column extracts thick 1, the method of 3-divinyl is characterized in that adding moisture acetonitrile solvent logistics on partitioned column butadiene extraction rectifying section top, and the middle part adds the mixed c 4 logistics, gaseous stream, condensing reflux are arranged at the top, and obtain the logistics of raffinating oil based on butylene; The material logistics of drawing of coming out at the bottom of the butadiene extraction rectifying section forms the feed back logistics through intermediate reboiler and enters tower zone, shared middle part, in this section realization heat energy recycle, and has gaseous stream to go alkynes extracting rectifying section; Add moisture acetonitrile solvent logistics on the top of alkynes extracting rectifying section, realize the operation of alkynes extracting rectifying; Gaseous stream, condensing reflux are arranged taking off reorganization segmentation top, and obtain product stream based on divinyl; When needs took off heavy constituent, taking off reorganization segmentation lower end had liquid phase stream to introduce the side line tower, has gaseous stream to return and takes off heavies column, obtains the heavy constituent logistics at the bottom of the side line tower; When not needing to take off heavy constituent, without the side line tower; Resolve the operation that section realizes steaming divinyl at solvent; Realize steaming the operation of butine and vinylacetylene in the alkynes section of steaming, gaseous stream, condensing reflux are arranged at the top, carbon four alkynes and the vinylacetylene logistics of liquid phase extraction safety content; Realize steaming of alkynes obtaining the pure solvent logistics in shared bottom tower zone, through recovery of heat and modified after recycling.
5, according to claim 4 pair of partitioned column extracts thick 1, the method of 3-divinyl, it is characterized in that finishing the butadiene extraction distillation operation at the butadiene extraction rectifying section, moisture acetonitrile solvent add-on is adjusted to 4.1～8.9 with the ratio of C 4 mixture amount, the trim the top of column amount is adjusted to 2.0～5.2 with the ratio of produced quantity, butadiene extraction theoretical number of plates of rectifying section 50～110, the solvent feed plate is positioned at theoretical stage 2～8, C 4 mixture fraction charging theoretical stage 25～60, the cat head working pressure is adjusted to 0.42～0.58MPa (A), and the cat head service temperature is adjusted to 35～50 ℃.
6, according to claim 4 pair of partitioned column extracts thick 1, the method of 3-divinyl, it is characterized in that finishing the extracting rectifying operation of carbon four alkynes and vinylacetylene in alkynes extracting rectifying section, from then on the butadiene stream of carbon containing four alkynes and vinylacetylene enters this section in the section lower end, moisture acetonitrile solvent adds from top, and backflow is arranged at the top; Solvent adding amount is adjusted to 1.2～3.3 with the ratio of crude butadiene amount, quantity of reflux is adjusted to 2.8～5.4 with the ratio of cat head produced quantity, this pars infrasegmentalis rising tolerance is adjusted to 0.32～0.65 with the ratio of shared middle part tower district rising tolerance, this section number of theoretical plate 50～80, solvent feed plate are positioned at the side line tower and draw theoretical stage 5～20 under the flitch.
7, the according to claim 4 pair of partitioned column extracts the method for thick 1,3-butadiene, it is characterized in that finishing heavy constituent 1,2-butylene and the carbon five that removes in the crude butadiene product taking off the reorganization segmentation; Backflow is arranged at this section top, and reflux ratio is adjusted to 3.0～6.2, and this section number of theoretical plate 30～60, cat head working pressure are adjusted to 0.42～0.58MPa (A), and the cat head service temperature is adjusted to 35～50 ℃.
8, according to claim 4 pair of partitioned column extracts thick 1, the method of 3-divinyl, when it is characterized in that to take off heavy constituent, draw material between reorganization segmentation and the alkynes extracting rectifying section and remove the side line tower taking off, this tower is finished the operation of extraction heavy constituent, this tower number of theoretical plate 15～35, the feed liquid phasor of drawing of side line tower accounts for 20%～40% of its upper tray decline amount of liquid phase.
9, the according to claim 4 pair of partitioned column extracts the method for thick 1,3-butadiene, it is characterized in that realizing in shared middle part tower zone heat recuperation and the operation of shunting steam flow, this section number of theoretical plate 3～10.
10, the according to claim 4 pair of partitioned column extracts the method for thick 1,3-butadiene, it is characterized in that resolving section at solvent finishes the solvent parse operation, promptly steams divinyl, this section number of theoretical plate 6～20 from solvent.
11, according to claim 4 pair of partitioned column extracts thick 1, the method of 3-divinyl, it is characterized in that finishing the operation that from solvent, steams butine and vinylacetylene in the alkynes section of steaming, from then on the solvent stream of carbon containing four alkynes and vinylacetylene enters the section lower end, backflow is arranged at the top, reflux ratio is adjusted to 3.1～6.5, and the ratio that rises tolerance and shared bottom tower zone rising tolerance on the bottom is adjusted to 0.11～0.25, this section number of theoretical plate 6～16.
12, the according to claim 4 pair of partitioned column extracts the method for thick 1,3-butadiene, it is characterized in that finishing the operation that steams butine and vinylacetylene from solvent in tower zone, shared bottom this tower section number of theoretical plate 5～13.
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| CN100453587C (en) * | 2007-04-13 | 2009-01-21 | 青岛伊科思新材料股份有限公司 | Recovery and using method of solution and unreaction monomer in process of producting polymer by solution polymerization process |
| CN102188837B (en) * | 2010-03-03 | 2013-08-21 | 中国石油化工股份有限公司 | Extractive distillation method |
| CN103420756B (en) * | 2012-05-16 | 2016-05-18 | 中国石油化工股份有限公司 | The method of preparing propylene from C 4 olefins |
| CN103570486A (en) * | 2012-07-27 | 2014-02-12 | 抚顺伊科思新材料有限公司 | Method for obtaining isoprene from C5 fraction |
| MY175112A (en) * | 2012-10-30 | 2020-06-08 | Lummus Technology Inc | Butadiene extraction process |
| US10689313B2 (en) * | 2015-10-23 | 2020-06-23 | Sabic Global Technologies B.V. | Processes and systems for purification of 1,3-butadiene |
| CN109593022B (en) * | 2017-09-30 | 2021-11-02 | 中国石油天然气股份有限公司 | Composite extracting agent for extracting butadiene and application thereof |
| CN112403015A (en) * | 2020-11-03 | 2021-02-26 | 汇智工程科技股份有限公司 | Device and method for separating acetone-n-heptane mixture by extractive distillation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2002062733A1 (en) * | 2001-02-08 | 2002-08-15 | Basf Aktiengesellschaft | Method for recovering crude 1,3-butadiene by extractive distillation from a c4 cut |
| CN1474794A (en) * | 2000-11-16 | 2004-02-11 | �����ɷ� | Method and device for obtaining 1,3-butadiene from 1,3-raw butadiene by distilation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1474794A (en) * | 2000-11-16 | 2004-02-11 | �����ɷ� | Method and device for obtaining 1,3-butadiene from 1,3-raw butadiene by distilation |
| WO2002062733A1 (en) * | 2001-02-08 | 2002-08-15 | Basf Aktiengesellschaft | Method for recovering crude 1,3-butadiene by extractive distillation from a c4 cut |
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