CA2600493A1 - Method for simultaneous removal of asphaltene, and/or paraffin and scale from producing oil wells - Google Patents
Method for simultaneous removal of asphaltene, and/or paraffin and scale from producing oil wells Download PDFInfo
- Publication number
- CA2600493A1 CA2600493A1 CA002600493A CA2600493A CA2600493A1 CA 2600493 A1 CA2600493 A1 CA 2600493A1 CA 002600493 A CA002600493 A CA 002600493A CA 2600493 A CA2600493 A CA 2600493A CA 2600493 A1 CA2600493 A1 CA 2600493A1
- Authority
- CA
- Canada
- Prior art keywords
- tool
- pressure wash
- set forth
- acid
- surge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract 19
- 239000003129 oil well Substances 0.000 title claims abstract 11
- 239000012188 paraffin wax Substances 0.000 title claims abstract 5
- 239000000839 emulsion Substances 0.000 claims abstract 17
- 210000002445 nipple Anatomy 0.000 claims abstract 14
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract 10
- 239000011707 mineral Substances 0.000 claims abstract 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 10
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract 8
- 239000002253 acid Substances 0.000 claims abstract 8
- 238000004140 cleaning Methods 0.000 claims abstract 8
- 239000003599 detergent Substances 0.000 claims abstract 8
- 229930195733 hydrocarbon Natural products 0.000 claims abstract 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract 8
- 239000002904 solvent Substances 0.000 claims abstract 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 6
- 239000000203 mixture Substances 0.000 claims 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 4
- 230000001143 conditioned effect Effects 0.000 claims 4
- 239000003350 kerosene Substances 0.000 claims 4
- 239000000463 material Substances 0.000 claims 4
- 239000012530 fluid Substances 0.000 claims 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims 2
- 125000000129 anionic group Chemical group 0.000 claims 2
- 239000003945 anionic surfactant Substances 0.000 claims 2
- 239000003093 cationic surfactant Substances 0.000 claims 2
- 239000000446 fuel Substances 0.000 claims 2
- 239000002563 ionic surfactant Substances 0.000 claims 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims 2
- 239000011976 maleic acid Substances 0.000 claims 2
- 239000001630 malic acid Substances 0.000 claims 2
- 235000011090 malic acid Nutrition 0.000 claims 2
- 229910017604 nitric acid Inorganic materials 0.000 claims 2
- 239000002736 nonionic surfactant Substances 0.000 claims 2
- 235000006408 oxalic acid Nutrition 0.000 claims 2
- 235000015096 spirit Nutrition 0.000 claims 2
- 239000004094 surface-active agent Substances 0.000 claims 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims 2
- 239000002888 zwitterionic surfactant Substances 0.000 claims 2
- -1 zylene Substances 0.000 claims 2
- 230000008878 coupling Effects 0.000 claims 1
- 238000010168 coupling process Methods 0.000 claims 1
- 238000005859 coupling reaction Methods 0.000 claims 1
- 125000001145 hydrido group Chemical group *[H] 0.000 claims 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B37/00—Methods or apparatus for cleaning boreholes or wells
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B37/00—Methods or apparatus for cleaning boreholes or wells
- E21B37/08—Methods or apparatus for cleaning boreholes or wells cleaning in situ of down-hole filters, screens, e.g. casing perforations, or gravel packs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S507/00—Earth boring, well treating, and oil field chemistry
- Y10S507/927—Well cleaning fluid
- Y10S507/929—Cleaning organic contaminant
- Y10S507/93—Organic contaminant is asphaltic
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S507/00—Earth boring, well treating, and oil field chemistry
- Y10S507/927—Well cleaning fluid
- Y10S507/929—Cleaning organic contaminant
- Y10S507/931—Organic contaminant is paraffinic
Abstract
A method for cleaning oil wells to increase the flow of oil thereof by use of a unique aqueous cleaning emulsion comprising of water, hydrocarbon solvent, detergent and mineral acid. This one step method provides for the simultaneously cleaning/removal of asphaltine and/or paraffin and scale. This method can be used alone or with the assistance of a wash tool which is a combination pressure and surge wash tool having a nipple assembly. A by-pass port is coupled to the nipple assembly and a diverter cup is coupled to the by-pass port. A plurality of pressure wash cups are positioned on the tool. A
pressure wash port is located between the plurality of pressure wash cups and a pump shoe assembly is coupled to a bottom pressure wash cup.
pressure wash port is located between the plurality of pressure wash cups and a pump shoe assembly is coupled to a bottom pressure wash cup.
Claims (32)
1. A one step process for removing both asphaltines and/or paraffins and scale simultaneously from an oil well containing clogged perforations or openings comprising the steps of:
a. Preparing an aqueous cleaning emulsion comprising:
i) from about 50% to about 98% by weight, water;
ii) from about 0.1% to about 15% by weight, detergent;
iii) from about 0.1% to about 20.0% by weight, hydrocarbon solvent; and iv) from about 0.1% to about 15.0% by weight, mineral acid, with the proviso that said emulsion is in a stable state over a wide range of temperatures and that the four materials, (i) -(iv) are in solution.
b. Contacting said emulsion with the interior of the oil well for a period of time sufficient to dispense asphaltines, paraffins and scale within the well from said openings.
a. Preparing an aqueous cleaning emulsion comprising:
i) from about 50% to about 98% by weight, water;
ii) from about 0.1% to about 15% by weight, detergent;
iii) from about 0.1% to about 20.0% by weight, hydrocarbon solvent; and iv) from about 0.1% to about 15.0% by weight, mineral acid, with the proviso that said emulsion is in a stable state over a wide range of temperatures and that the four materials, (i) -(iv) are in solution.
b. Contacting said emulsion with the interior of the oil well for a period of time sufficient to dispense asphaltines, paraffins and scale within the well from said openings.
2. The process as set forth in claim 1, wherein the water is conditioned water.
3. The process as set forth in claim 1 wherein the detergent contains a material selected from the group consisting of zwitterionic, ampholytic, nonionic, anionic and cationic surfactants and mixtures thereof.
4. The process as set forth in claim 1 wherein the hydrocarbon solvent is selected from the group consisting of gasoline, diesel, jet fuel, kerosene, zylene, mineral spirits and mixtures thereof.
5. The process as set forth in claim 1 wherein the mineral acid is selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, citric acid, oxalic acid, maleic acid, acetic acid, malic acid, glutaric acid and mixtures thereof.
6. The process as set forth in claim 1 wherein (a) the water is conditioned;
(b) the detergent contains a surfactant; (c) the hydrocarbon solvent is kerosene; and (d) the mineral acid is hydrochloric acid.
(b) the detergent contains a surfactant; (c) the hydrocarbon solvent is kerosene; and (d) the mineral acid is hydrochloric acid.
7. A method of cleaning an oil well containing asphaltine and/or paraffin and scale to increase oil flow therefrom comprising the steps of:
a. adding an aqueous cleaning emulsion comprising water, a detergent, a hydrocarbon solvent, and a mineral acid into the oil well containing a tubing string;
b. coupling a surge and pressure wash tool to said tubing string of the oil well;
c. moving the surge and pressure tool to the bottom of said oil well; and d. raising the surge and pressure wash tool after a reasonable period of time, thereby providing a period of contact under pressure and vacuum of said emulsion with said asphaltine, paraffin and scale.
a. adding an aqueous cleaning emulsion comprising water, a detergent, a hydrocarbon solvent, and a mineral acid into the oil well containing a tubing string;
b. coupling a surge and pressure wash tool to said tubing string of the oil well;
c. moving the surge and pressure tool to the bottom of said oil well; and d. raising the surge and pressure wash tool after a reasonable period of time, thereby providing a period of contact under pressure and vacuum of said emulsion with said asphaltine, paraffin and scale.
8. The method of Claim 7 further comprising the step of injecting said additional emulsion into the surge and pressure wash tool.
9. The method of Claim 7 further comprising the steps of:
a). moving the surge and pressure tool to the bottom of said oil well after raising the surge and pressure wash tool; and b) raising the surge and pressure wash tool after a reasonable period of time.
a). moving the surge and pressure tool to the bottom of said oil well after raising the surge and pressure wash tool; and b) raising the surge and pressure wash tool after a reasonable period of time.
10. The method of Claim 7 wherein the surge and pressure wash tool is replaced with a hydro self-rotating high pressure wash tool which is moved up and down the oil well.
11. The method of Claim 7 wherein the surge and pressure wash tool comprises:
a) a nipple assembly b) a by-pass port coupled to the nipple assembly wherein the port by-pass port allows the emulsion to enter the tool on an upward movement of the tool;
c) a diverter cup coupled to the by-pass port wherein the diverter cup diverts the emulsion with debris down the tool and out a bottom section of the tool;
d) a plurality of pressure wash cups positioned on the tool for creating a suction below each of the plurality of cups;
e) a pressure wash port located between the plurality of pressure wash cups wherein the pressure wash port allows the emulsion to exit the tool at an elevated pressure to clean the wells; and f) a pump shoe assembly coupled to a bottom pressure wash cup.
a) a nipple assembly b) a by-pass port coupled to the nipple assembly wherein the port by-pass port allows the emulsion to enter the tool on an upward movement of the tool;
c) a diverter cup coupled to the by-pass port wherein the diverter cup diverts the emulsion with debris down the tool and out a bottom section of the tool;
d) a plurality of pressure wash cups positioned on the tool for creating a suction below each of the plurality of cups;
e) a pressure wash port located between the plurality of pressure wash cups wherein the pressure wash port allows the emulsion to exit the tool at an elevated pressure to clean the wells; and f) a pump shoe assembly coupled to a bottom pressure wash cup.
12. The method of Claim 11 wherein the nipple assembly is a perforated nipple assembly having a plurality of annuli located around an outer top perimeter.
13. The method of Claim 11 wherein the nipple assembly is a non-port nipple assembly.
14. The method of Claim 11 wherein the pump shoe assembly comprises:
a. a connector coupled to a bottom section of the tool;
b. a pump shoe valve coupled to the connector; and c. a blow plug coupled to the pump shoe valve.
a. a connector coupled to a bottom section of the tool;
b. a pump shoe valve coupled to the connector; and c. a blow plug coupled to the pump shoe valve.
15. The method of Claim 14 and further comprising a swing flap internal to the pump shoe valve wherein the swing flap is open on an upward movement of the tool and closed on the downward movement of the tool.
16. An aqueous cleaning emulsion useful to remove asphaltine and/or paraffin and scale simultaneously from oil wells comprising:
i) from about 50% to about 98% by weight, water;
ii) from about 0.1% to about 15% by weight, detergent;
iii) from about 0.1% to about 20.0% by weight, hydrocarbon solvent; and iv) from about 0.1% to about 15.0% by weight, mineral acid, with the proviso that said emulsion is in a stable state over a wide range of temperatures and that the four materials, (i) -(iv) are in solution.
i) from about 50% to about 98% by weight, water;
ii) from about 0.1% to about 15% by weight, detergent;
iii) from about 0.1% to about 20.0% by weight, hydrocarbon solvent; and iv) from about 0.1% to about 15.0% by weight, mineral acid, with the proviso that said emulsion is in a stable state over a wide range of temperatures and that the four materials, (i) -(iv) are in solution.
17. The emulsion as set forth in Claim 16 wherein the water is conditioned water.
18. The emulsion as set forth in Claim 17 wherein the detergent contains a material selected from the group consisting of zwitterionic, ampholytic, nonionic, anionic and cationic surfactants and mixtures thereof.
19. The emulsion as set forth in claim 18 wherein the hydrocarbon solvent is selected from the group consisting of gasoline, diesel, jet fuel, kerosene, zylene, mineral spirits and mixtures thereof.
20. The emulsion as set forth in claim 19 wherein the mineral acid is selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, citric acid, oxalic acid, maleic acid, acetic acid, malic acid, glutaric acid and mixtures thereof.
21. The emulsion as set forth in Claim 16 wherein (a) the water is conditioned; (b) the detergent contains a surfactant; (c) the hydrocarbon solvent is kerosene; and (d) the mineral acid is hydrochloric acid.
22. A combination surge and pressure wash tool for cleaning wells comprising, in combination:
a. a nipple assembly b. a by-pass port coupled to the nipple assembly;
c. a diverter cup coupled to the by-pass port;
d. a plurality of pressure wash cups positioned on the tool;
e. a pressure wash port located between the plurality of pressure wash cups;
and f. A pump shoe assembly coupled to a bottom pressure wash cup.
a. a nipple assembly b. a by-pass port coupled to the nipple assembly;
c. a diverter cup coupled to the by-pass port;
d. a plurality of pressure wash cups positioned on the tool;
e. a pressure wash port located between the plurality of pressure wash cups;
and f. A pump shoe assembly coupled to a bottom pressure wash cup.
23. The combination surge and pressure wash tool as set forth in Claim 22 wherein the nipple assembly is a perforated nipple assembly having a plurality of annuli located around an outer top perimeter.
24. The combination surge and pressure wash tool as set forth in Claim 22 wherein the nipple assembly is a non-port nipple assembly.
25. The combination surge and pressure wash tool as set forth in Claim 22, further comprising a collar assembly coupled to a top section of the tool.
26. The combination surge and pressure wash tool as set forth in Claim 22 wherein the by-pass port allows fluid to enter the tool on an upward movement of the tool.
27. The combination surge and pressure wash tool as set forth in Claim 22 wherein the diverter cup diverts fluid with debris down the tool and out the pump shoe assembly.
28. The combination surge and pressure wash tool as set forth in Claim 22 wherein the plurality of wash cups create a suction below each of the plurality of cups.
29. The combination surge and pressure wash tool as set forth in Claim 22 wherein the pressure wash port allows fluid to exit the tool at an elevated pressure to clean the wells.
30. The combination surge and pressure wash tool as set forth in Claim 22 wherein the pump shoe assembly comprises:
a. a connector coupled to a bottom section of the tool;
b. a pump shoe valve coupled to the connector; and c. a blow plug coupled to the pump shoe valve.
a. a connector coupled to a bottom section of the tool;
b. a pump shoe valve coupled to the connector; and c. a blow plug coupled to the pump shoe valve.
31. The combination surge and pressure wash tool as set forth in Claim 30 further comprising a collar assembly coupled to the pump shoe valve and the blow plug.
32. The combination surge and pressure wash tool as set forth in Claim 30 further comprising a swing flap internal to the pump shoe valve wherein the swing flap is open on an upward movement of the tool and closed on the downward movement of the tool.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/092,422 US7296627B2 (en) | 2005-03-29 | 2005-03-29 | Method for simultaneous removal of asphaltene, and/or paraffin and scale from producing oil wells |
| US11/092,422 | 2005-03-29 | ||
| PCT/US2006/009600 WO2006104711A2 (en) | 2005-03-29 | 2006-03-16 | Method for removal of asphaltene, paraffin and/or scale from producing wells |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2600493A1 true CA2600493A1 (en) | 2006-10-05 |
| CA2600493C CA2600493C (en) | 2011-12-06 |
Family
ID=37053881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2600493A Expired - Fee Related CA2600493C (en) | 2005-03-29 | 2006-03-16 | Method for simultaneous removal of asphaltene, and/or paraffin and scale from producing oil wells |
Country Status (3)
| Country | Link |
|---|---|
| US (4) | US7296627B2 (en) |
| CA (1) | CA2600493C (en) |
| WO (1) | WO2006104711A2 (en) |
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| US8541347B2 (en) * | 2007-01-26 | 2013-09-24 | Halliburton Energy Services, Inc. | Hydrocarbon-acid emulsion compositions and associated methods |
| US20090120633A1 (en) * | 2007-11-13 | 2009-05-14 | Earl Webb | Method for Stimulating a Well Using Fluid Pressure Waves |
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| US5762138A (en) * | 1996-12-09 | 1998-06-09 | Halliburton Energy Services, Inc. | Method of preventing incompatibility between aqueous well treating fluids and hydrocarbons |
| US6536523B1 (en) * | 1997-01-14 | 2003-03-25 | Aqua Pure Ventures Inc. | Water treatment process for thermal heavy oil recovery |
| US6242388B1 (en) * | 1998-11-23 | 2001-06-05 | Eastman Chemical Company | Mutual solvents comprising 2,2,4-trimethyl-1,3-pentanediol mono-or di-isobutyrate and stable emulsions thereof |
| US6593279B2 (en) * | 1999-12-10 | 2003-07-15 | Integrity Industries, Inc. | Acid based micro-emulsions |
| US20030111226A1 (en) * | 2001-12-13 | 2003-06-19 | Dyer Richard J. | Combination surge/pressure wash tool for oil wells and method therefor |
| US7296627B2 (en) * | 2005-03-29 | 2007-11-20 | Dyer Richard J | Method for simultaneous removal of asphaltene, and/or paraffin and scale from producing oil wells |
-
2005
- 2005-03-29 US US11/092,422 patent/US7296627B2/en active Active
-
2006
- 2006-03-16 CA CA2600493A patent/CA2600493C/en not_active Expired - Fee Related
- 2006-03-16 WO PCT/US2006/009600 patent/WO2006104711A2/en active Application Filing
-
2007
- 2007-09-18 US US11/901,530 patent/US7670993B2/en not_active Expired - Fee Related
- 2007-10-01 US US11/906,484 patent/US7497261B2/en active Active
-
2009
- 2009-01-28 US US12/321,978 patent/US7632785B2/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| US7296627B2 (en) | 2007-11-20 |
| US20080047712A1 (en) | 2008-02-28 |
| WO2006104711A3 (en) | 2009-04-16 |
| CA2600493C (en) | 2011-12-06 |
| US7670993B2 (en) | 2010-03-02 |
| US7632785B2 (en) | 2009-12-15 |
| US20080006408A1 (en) | 2008-01-10 |
| WO2006104711A2 (en) | 2006-10-05 |
| US20090137430A1 (en) | 2009-05-28 |
| US7497261B2 (en) | 2009-03-03 |
| US20060219409A1 (en) | 2006-10-05 |
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| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed |
Effective date: 20220316 |