WO2005037396A1 - Butadiene recovery process - Google Patents
Butadiene recovery process Download PDFInfo
- Publication number
- WO2005037396A1 WO2005037396A1 PCT/PL2004/000083 PL2004000083W WO2005037396A1 WO 2005037396 A1 WO2005037396 A1 WO 2005037396A1 PL 2004000083 W PL2004000083 W PL 2004000083W WO 2005037396 A1 WO2005037396 A1 WO 2005037396A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- butadiene
- distillation column
- extractive distillation
- column
- stream
- Prior art date
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/28—Evaporating with vapour compression
- B01D1/284—Special features relating to the compressed vapour
- B01D1/2856—The compressed vapour is used for heating a reboiler or a heat exchanger outside an evaporator
-
- 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
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/343—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
Definitions
- BUTADIENE RECOVERY PROCESS This invention relates to a process of 1 ,3-butadiene recovery from C 4 hydrocarbon mixtures by means of extractive distillation with a selective solvent.
- N° 3 798 132 process of recovery 1 ,3-butadiene from its mixtures with other four-carbon molecule hydrocarbons. Accordingly to this process the C 4 hydrocarbon mixture is introduced into the intermediate zone of the extractive distillation column and the selective solvent is introduced into the upper section of the column.
- olefin and paraffin hydrocarbons are separated from the C 4 hydrocarbon mixture, and are withdrawn from the column overhead, while 1 -3-butadiene and acetylenes are withdrawn from the column bottoms and transferred to the upper part of the stripping column.
- the stripping column operated at lower pressure than the extractive distillation column, the feed flashes and butadiene rich vapour is withdrawn overhead.
- the vapour is compressed in a compressor to higher pressure than that in the extractive distillation column and directed partly to the second stripping column, and partly to the extractive distillation column, whereas acetylenes are separated and recovered in an intermediate portion of the first stripping column.
- Butadiene vapours from the second stripping column overhead are condensed and the finished butadiene product is obtained from there.
- the solvent is stripped off in the bottom section of the first stripping column and recycled to the extractive distillation column and to the second stripping column, while the selective solvent from the second column bottoms is recycled to the first stripping column to recover butadiene.
- the process consists in that C4 hydrocarbon mixture is introduced to one or more trays of the extractive distillation column and a selective solvent to its upper zone. Olefin and paraffin hydrocarbons are withdrawn from the extractive distillation column top.
- the bottoms product from this column is sent to a flash (expansion) drum in which due to intermediate flashing at reduced pressure partial butadiene vaporization and vapour/liquid separation takes place.
- the separated vapour enters a distillation column operating at lower pressure than the pressure in the extractive distillation column.
- the distillate from the distillation column being concentrated butadiene and condensed in a water cooled condenser is the first butadiene stream.
- the liquid phase from the flash drum enters to the stripper operating at almost atmospheric pressure. Concentrated butadiene vapour from the stripper after compression is the second butadiene stream partly recycled to the extractive distillation column.
- the selective solvent recovered from the bottoms of the stripping column is transferred to the extractive distillation column and can be introduced to one or more trays of this column.
- the extractive distillation column consists of two bottom section columns and one common upper section column, whereas vapour streams from the bottom section columns enter the bottom of the upper section column and the bottoms product from the upper section column is introduced to the top of both lower section columns.
- the bottoms product from the extractive distillation column can be expanded in a flash drum or in a distillation column operating at a pressure that is lower than the extractive distillation column pressure but high enough to enable vapour condensing in a condenser cooled with water at 5-35°C.
- the slops expanded in a flash drum or in a column are heated up if necessary.
- the subject invention enables a substantial increase of butadiene recovery plant capacity, because due to the application of an intermediate expanding, vapour separation and condensing, the amount of butadiene recovered from feedstock can greatly exceed compressor capacity. This makes a strong contrast with hitherto existing solutions, where as a rule plant capacity is smaller than compressor capacity.
- This advantage is attributable to splitting of the extractive distillation bottom stream into two streams containing butadiene. One stream after distillation and condensation is directed to a final purification and hence only the second stream is transferred to a stripping column, where butadiene stripping from solvent occurs and thus obtained concentrated butadiene vapour is compressed.
- Another feature of the invention is its generality in process applications providing the possibility not only to modify flow rate of butadiene streams but also influence the extractive distillation column capacity by such an operation mode that one or two columns are used as bottom or top sections and the selective solvent is introduced to one or more trays of the column.
- FIG. 1 presents the general invention idea in the form of a plant process diagram.
- Figure 2 presents a diagram of the butadiene recovery unit corresponding to the implementation test example.
- the example of realization of this invention is presented on the drawing, which shows that The process of 1 ,3-butadiene recovery from mixture streams of butadiene with other C 4 hydrocarbons consist in that the feed stream (1) is introduced onto one or more trays of the extractive distillation column 2, and the selective solvent stream 3 onto an upper tray. The stream containing olefin and paraffin hydrocarbons 4 is removed as the overhead product.
- the bottoms stream 5 is withdrawn from the bottom of extractive distillation column 2 and is carried to the flash drum 6, where due to expanding of the bottoms 5 as well as partial butadiene vaporization the initial separation of the vapour 7 from the liquid 8 occurs.
- Separated vapours 7 flow to the distillation column 9 operating at lower pressure than the pressure in the extractive distillation column 2, where solvent free concentrated butadiene vapours is obtained overhead as distillate and condensed in the water condenser 10 giving the first butadiene stream 11.1.
- the liquid stream containing the mixture of butadiene and solvent 8 flows from the flash drum 6 to the stripping column 12, from where the overhead concentrated butadiene vapour is obtained overhead and after compression to the pressure higher than the pressure in the extractive distillation column 2, the second butadiene stream 11.2 is obtained.
- a portion of the compressed butadiene stream is recycled from the compressor 13 discharge to the extractive distillation column 2.
- the bottoms product 5 from the extractive distillation column 2 may flash in the initial desorption column encompassing a flash drum 6 and a distillation column 9 as one apparatus.
- the stripping column 12 operates at a pressure close to atmospheric.
- the pressure in the distillation column 9 is lower than the pressure in the extractive distillation column 2, but such that condensing butadiene vapours in the condenser 10 with cooling water of the temperature of 5 ⁇ 35°C is enabled.
- the bottoms product 5 if necessary is warmed up.
- the mixture of hydrocarbons 1 is introduced into two bottom section columns of the extractive distillation column 2a, 2b, from the top of which two overhead vapour streams are obtained and passed to the bottom of the common upper section column 2, while the bottoms product of the upper section 2 is introduced into the bottom section columns 2a, 2b.
- the final capacity of this butadiene recovery process may be higher than the capacity of the compressor 13.
- Butadiene recovery test has been carried out in a plant configuration depicted in figure 2.
- the unit was charged with C 4 hydrocarbon stream 1 whose composition and conditions are specified in column 1 of the table. This stream was fed to columns trays 2a and 2b of the lower extractive distillation columns.
- the extractive distillation column operates at 0.45 MPa pressure.
- the vapour streams from the lower extractive distillation columns were introduced to the bottom part 2 of the extractive distillation column, whereas the bottoms product 5 was introduced to the flash drum 6.
- the butadiene vapour 7 from the flash drum comes to the distillation column 9 that was operating at 0.28 MPa pressure and the distillate of concentrated butadiene as the first butadiene stream 11.1 was obtained from the condenser 10 cooled with water at 28°C.
- This stream characteristic is in 11.1 column of the table.
- the liquid 8 from the flash drum 6 was pumped to the stripping column 12 operating at 0.015MPa pressure.
- the liquid dimethylformamide solvent stream not containing butadiene from the stripper bottoms was cooled down and pumped to three trays of the extractive distillation column: to each lower column 2a and 2b and to the upper column 2.
- the second butadiene stream 11.2 characterized in 11.2 column of the table was obtained by compression of the butadiene vapour in the compressor 13.
Abstract
The butadiene-rich slops (5) is carried to the flash drum (6), where the initial expanding cause separation vapour (7) from the liquid (8), and separated vapours (7) flow to the distillation column (9), where overhead solvent free concentrated butadiene vapours is obtained and condensed in the water condenser (10) giving the first butadiene stream (11. 1), and the liquid stream (8) flows to the stripping column (12), forming the overhead concentrated butadiene vapour and after it compression the second butadiene stream (11.2) is obtained.
Description
BUTADIENE RECOVERY PROCESS This invention relates to a process of 1 ,3-butadiene recovery from C4 hydrocarbon mixtures by means of extractive distillation with a selective solvent. There are known from the US Patent description N° 3 798 132 process of recovery 1 ,3-butadiene from its mixtures with other four-carbon molecule hydrocarbons. Accordingly to this process the C4 hydrocarbon mixture is introduced into the intermediate zone of the extractive distillation column and the selective solvent is introduced into the upper section of the column. In the column olefin and paraffin hydrocarbons are separated from the C4 hydrocarbon mixture, and are withdrawn from the column overhead, while 1 -3-butadiene and acetylenes are withdrawn from the column bottoms and transferred to the upper part of the stripping column. In the stripping column, operated at lower pressure than the extractive distillation column, the feed flashes and butadiene rich vapour is withdrawn overhead. The vapour is compressed in a compressor to higher pressure than that in the extractive distillation column and directed partly to the second stripping column, and partly to the extractive distillation column, whereas acetylenes are separated and recovered in an intermediate portion of the first stripping column. Butadiene vapours from the second stripping column overhead are condensed and the finished butadiene product is obtained from there. The solvent is stripped off in the bottom section of the first stripping column and recycled to the extractive distillation column and to the second stripping column, while the selective solvent from the second column bottoms is recycled to the first stripping column to recover butadiene. In the preferred embodiment of this invention, the process consists in that C4 hydrocarbon mixture is introduced to one or more trays of the extractive distillation column and a selective solvent to its upper zone. Olefin and paraffin hydrocarbons are withdrawn from the extractive distillation column top. The bottoms product from this column is sent to a flash (expansion) drum in which due to intermediate flashing at reduced pressure partial butadiene vaporization and vapour/liquid separation takes place. The separated vapour enters a distillation column operating at lower pressure than the pressure in the extractive distillation column. The distillate from the distillation column being concentrated butadiene and condensed in a water cooled condenser is the first butadiene stream.
The liquid phase from the flash drum enters to the stripper operating at almost atmospheric pressure. Concentrated butadiene vapour from the stripper after compression is the second butadiene stream partly recycled to the extractive distillation column. The selective solvent recovered from the bottoms of the stripping column is transferred to the extractive distillation column and can be introduced to one or more trays of this column. In a variation of the invention the extractive distillation column consists of two bottom section columns and one common upper section column, whereas vapour streams from the bottom section columns enter the bottom of the upper section column and the bottoms product from the upper section column is introduced to the top of both lower section columns. The bottoms product from the extractive distillation column can be expanded in a flash drum or in a distillation column operating at a pressure that is lower than the extractive distillation column pressure but high enough to enable vapour condensing in a condenser cooled with water at 5-35°C. The slops expanded in a flash drum or in a column are heated up if necessary. The subject invention enables a substantial increase of butadiene recovery plant capacity, because due to the application of an intermediate expanding, vapour separation and condensing, the amount of butadiene recovered from feedstock can greatly exceed compressor capacity. This makes a strong contrast with hitherto existing solutions, where as a rule plant capacity is smaller than compressor capacity. This advantage is attributable to splitting of the extractive distillation bottom stream into two streams containing butadiene. One stream after distillation and condensation is directed to a final purification and hence only the second stream is transferred to a stripping column, where butadiene stripping from solvent occurs and thus obtained concentrated butadiene vapour is compressed. This enables to remove the inherent "bottleneck" of existing processes resulting from constant limiting capacity of a positive-displacement compressor, that has to be used to recycle a part of the butadiene vapour back to the extractive distillation column. The compressor capacity becomes a limiting factor in a plant capacity. According to the solution in the invention the spill back to the compressor suction can e maintained at necessary minimum which enhances energy savings. Another feature of the invention is its generality in process applications providing the possibility not only to modify flow rate of butadiene streams but also influence the extractive distillation column capacity by such an operation
mode that one or two columns are used as bottom or top sections and the selective solvent is introduced to one or more trays of the column. In the preferred embodiment of the process according to this invention is shown on the drawing, where the figure 1 presents the general invention idea in the form of a plant process diagram. Figure 2 presents a diagram of the butadiene recovery unit corresponding to the implementation test example. The example of realization of this invention is presented on the drawing, which shows that The process of 1 ,3-butadiene recovery from mixture streams of butadiene with other C4 hydrocarbons consist in that the feed stream (1) is introduced onto one or more trays of the extractive distillation column 2, and the selective solvent stream 3 onto an upper tray. The stream containing olefin and paraffin hydrocarbons 4 is removed as the overhead product. The bottoms stream 5 is withdrawn from the bottom of extractive distillation column 2 and is carried to the flash drum 6, where due to expanding of the bottoms 5 as well as partial butadiene vaporization the initial separation of the vapour 7 from the liquid 8 occurs. Separated vapours 7 flow to the distillation column 9 operating at lower pressure than the pressure in the extractive distillation column 2, where solvent free concentrated butadiene vapours is obtained overhead as distillate and condensed in the water condenser 10 giving the first butadiene stream 11.1. The liquid stream containing the mixture of butadiene and solvent 8 flows from the flash drum 6 to the stripping column 12, from where the overhead concentrated butadiene vapour is obtained overhead and after compression to the pressure higher than the pressure in the extractive distillation column 2, the second butadiene stream 11.2 is obtained. A portion of the compressed butadiene stream is recycled from the compressor 13 discharge to the extractive distillation column 2. The bottoms product 5 from the extractive distillation column 2 may flash in the initial desorption column encompassing a flash drum 6 and a distillation column 9 as one apparatus. The stripping column 12 operates at a pressure close to atmospheric. The pressure in the distillation column 9 is lower than the pressure in the extractive distillation column 2, but such that condensing butadiene vapours in the condenser 10 with cooling water of the temperature of 5 ÷ 35°C is enabled. The bottoms product 5 if necessary is warmed up. Where it is justified, the mixture of hydrocarbons 1 is introduced into two bottom section columns of the extractive distillation column 2a, 2b, from the top of which two overhead vapour streams are obtained and passed to the bottom of the common upper section column 2, while the bottoms product of the upper section 2 is introduced into the bottom section columns 2a, 2b. The final
capacity of this butadiene recovery process may be higher than the capacity of the compressor 13.
The following sample is included to demonstrate specific embodiment of the invention. The example: Butadiene recovery test has been carried out in a plant configuration depicted in figure 2. The unit was charged with C4 hydrocarbon stream 1 whose composition and conditions are specified in column 1 of the table. This stream was fed to columns trays 2a and 2b of the lower extractive distillation columns. The extractive distillation column operates at 0.45 MPa pressure. The vapour streams from the lower extractive distillation columns were introduced to the bottom part 2 of the extractive distillation column, whereas the bottoms product 5 was introduced to the flash drum 6. The butadiene vapour 7 from the flash drum comes to the distillation column 9 that was operating at 0.28 MPa pressure and the distillate of concentrated butadiene as the first butadiene stream 11.1 was obtained from the condenser 10 cooled with water at 28°C. This stream characteristic is in 11.1 column of the table. The liquid 8 from the flash drum 6 was pumped to the stripping column 12 operating at 0.015MPa pressure. The liquid dimethylformamide solvent stream not containing butadiene from the stripper bottoms was cooled down and pumped to three trays of the extractive distillation column: to each lower column 2a and 2b and to the upper column 2. The second butadiene stream 11.2 characterized in 11.2 column of the table was obtained by compression of the butadiene vapour in the compressor 13.
Table
Claims
CLAIMS 1. The process of 1 ,3-butadiene recovery from mixture streams of butadiene with other C4 hydrocarbons (1) consist in that the stream (1) is introduced onto one tray of the extractive distillation column (2) and the selective solvent stream (3) onto an upper tray, and the stream containing olefin and paraffin hydrocarbons (4) is removed as the overhead product, and the bottoms stream (5) is withdrawn from the bottom of extractive distillation column (2) characterized in that the bottoms (5) is carried to the flash drum (6), where due to expanding of the bottoms (5) as well as partial butadiene vaporization the initial separation of the vapour (7) from the liquid (8) occurs, and separated vapours (7) flow to the distillation column (9) operating at lower pressure than the pressure in the extractive distillation column (2), where solvent free concentrated butadiene vapours is obtained overhead as distillate and condensed in the water condenser (10) giving the first butadiene stream (11.1), the liquid stream containing the mixture of butadiene and solvent (8) flows from the flash drum (6) to the stripping column (12), from where the overhead concentrated butadiene vapour is obtained overhead and after compression to the pressure higher than the pressure in the extractive distillation column (2), the second butadiene stream (11.2) is obtained, and a portion of the compressed butadiene stream is recycled from the compressor (13) discharge to the extractive distillation column (2).
2. The process according to claim 1 , characterized in that the bottoms (5) from the extractive distillation column (2) is flashed in the initial desorption column encompassing a flash drum (6) and a distillation column (9) as one apparatus.
3. The process according to claim 1 , characterized in that the selective solvent may be introduced into two or more trays of the extractive distillation column (2).
4. The process according to claim 1 , characterized in that the stripping column (12) operates at a pressure close to atmospheric.
5. The process according to claim 1, characterized in that the pressure in the distillation column (9) is lower than the pressure in the extractive distillation column (2), but such that condensing butadiene vapours in the condenser (10) with cooling water of the temperature of 5 ÷ 35°C is enabled.
6. The process according to claim 1 , characterized in that the bottoms product (5) is warmed up.
7. The process according to claim 1 , characterized in that the mixture of hydrocarbons (1) is introduced into two bottom section columns of the extractive distillation column (2a, 2b), from the top of which two overhead vapour streams are obtained and passed to the bottom of the common upper section column (2), while the bottoms product of the upper section (2) is introduced into the bottom section columns (2a, 2b).
8. The process according to claim 1 , characterized in that the final capacity of the butadiene may be higher than the capacity of the compressor (13).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PLP-362953 | 2003-10-20 | ||
| PL362953A PL201117B1 (en) | 2003-10-20 | 2003-10-20 | Method for releasing butadiene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2005037396A1 true WO2005037396A1 (en) | 2005-04-28 |
Family
ID=34464956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/PL2004/000083 WO2005037396A1 (en) | 2003-10-20 | 2004-10-19 | Butadiene recovery process |
Country Status (2)
| Country | Link |
|---|---|
| PL (1) | PL201117B1 (en) |
| WO (1) | WO2005037396A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010008109A1 (en) * | 2008-07-17 | 2010-01-21 | Sk Energy Co., Ltd. | Process for 1,3-butadiene separation from a crude c4 stream with acetylene converter |
| US8080140B2 (en) | 2007-04-18 | 2011-12-20 | Exxonmobil Chemical Patents Inc. | Process for debottlenecking a system for the separation of a conjugated diolefin |
| CN102336626A (en) * | 2010-07-28 | 2012-02-01 | 中国石油化工股份有限公司 | Utilization method of waste gas discharged from butadiene extracting apparatus |
| EP2914568B1 (en) * | 2012-10-30 | 2018-03-28 | Lummus Technology Inc. | Butadiene extraction process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3772158A (en) * | 1971-03-29 | 1973-11-13 | Shell Oil Co | Butadiene recovery process |
| US4162198A (en) * | 1977-05-28 | 1979-07-24 | Basf Aktiengesellschaft | Separation of a mixture of C4 -hydrocarbons by extractive distillation |
| EP0036735A1 (en) * | 1980-03-15 | 1981-09-30 | Japan Synthetic Rubber Co., Ltd. | Process for producing 1,3-butadiene or 2-methyl-1,3-butadiene of high purity |
| GB2077753A (en) * | 1980-06-12 | 1981-12-23 | Nippon Zeon Co | Process for extractive distillation of hydrocarbons |
-
2003
- 2003-10-20 PL PL362953A patent/PL201117B1/en unknown
-
2004
- 2004-10-19 WO PCT/PL2004/000083 patent/WO2005037396A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3772158A (en) * | 1971-03-29 | 1973-11-13 | Shell Oil Co | Butadiene recovery process |
| US4162198A (en) * | 1977-05-28 | 1979-07-24 | Basf Aktiengesellschaft | Separation of a mixture of C4 -hydrocarbons by extractive distillation |
| EP0036735A1 (en) * | 1980-03-15 | 1981-09-30 | Japan Synthetic Rubber Co., Ltd. | Process for producing 1,3-butadiene or 2-methyl-1,3-butadiene of high purity |
| GB2077753A (en) * | 1980-06-12 | 1981-12-23 | Nippon Zeon Co | Process for extractive distillation of hydrocarbons |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8080140B2 (en) | 2007-04-18 | 2011-12-20 | Exxonmobil Chemical Patents Inc. | Process for debottlenecking a system for the separation of a conjugated diolefin |
| WO2010008109A1 (en) * | 2008-07-17 | 2010-01-21 | Sk Energy Co., Ltd. | Process for 1,3-butadiene separation from a crude c4 stream with acetylene converter |
| CN102336626A (en) * | 2010-07-28 | 2012-02-01 | 中国石油化工股份有限公司 | Utilization method of waste gas discharged from butadiene extracting apparatus |
| EP2914568B1 (en) * | 2012-10-30 | 2018-03-28 | Lummus Technology Inc. | Butadiene extraction process |
Also Published As
| Publication number | Publication date |
|---|---|
| PL362953A1 (en) | 2005-05-02 |
| PL201117B1 (en) | 2009-03-31 |
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