EP1444314B1 - Verwendung von Alkaliphosphat in einem Hochtemperatur-Schmiermittel - Google Patents
Verwendung von Alkaliphosphat in einem Hochtemperatur-Schmiermittel Download PDFInfo
- Publication number
- EP1444314B1 EP1444314B1 EP02782698A EP02782698A EP1444314B1 EP 1444314 B1 EP1444314 B1 EP 1444314B1 EP 02782698 A EP02782698 A EP 02782698A EP 02782698 A EP02782698 A EP 02782698A EP 1444314 B1 EP1444314 B1 EP 1444314B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- lubricant
- alkali
- orthophosphate
- temperature
- melting temperature
- 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.)
- Expired - Lifetime
Links
- 239000000314 lubricant Substances 0.000 title claims abstract description 69
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 12
- 239000010959 steel Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims description 16
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000005461 lubrication Methods 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 claims 1
- 230000001050 lubricating effect Effects 0.000 abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- -1 ferrous metals Chemical class 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011833 salt mixture Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004439 roughness measurement Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- HVTHJRMZXBWFNE-UHFFFAOYSA-J sodium zincate Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Zn+2] HVTHJRMZXBWFNE-UHFFFAOYSA-J 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
- C10M103/06—Metal compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/085—Phosphorus oxides, acids or salts
- C10M2201/0853—Phosphorus oxides, acids or salts used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/02—Groups 1 or 11
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/04—Groups 2 or 12
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/06—Groups 3 or 13
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/241—Manufacturing joint-less pipes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/015—Dispersions of solid lubricants
- C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/08—Solids
Definitions
- the invention relates to the use of alkali metal phosphate in a high-temperature lubricant for lubricating two surface-contacting heated metal objects, which perform a relative movement to each other.
- the mandrel bars For example, in the production of seamless steel or non-ferrous metal pipes, it is important to lubricate the tools, especially the mandrel bars, intensive, so they have the longest possible life.
- the surfaces of the mandrel bars should be uniform and smooth to ensure a uniform material flow of the metal to be processed.
- the quality of the inner pipe surfaces depends on the surface quality of the mandrel bars. If the inner surface of the tubes is rough or wavy, or even has damages due to the quality of the mandrels, a high rejection rate is obtained. It has therefore been tried in the past to increase the service life of the mandrel bars by applying lubricants on them.
- Organic lubricants used in the hot forming of metals have proven unsuitable at high temperatures.
- To improve the lubricating properties was therefore used for example in the DE-PS 4 300 464 or the EP-PS 0 554 822 as an essential component of the lubricant graphite.
- graphite has good release and lubricating properties.
- a disadvantage is the tendency of graphite, at high temperatures to carburize the workpiece surfaces, here the tube surfaces contribute. Also spot welds between the tool and the workpiece can occur. The consequence of both effects is a high tool wear and a high reject rate of the workpieces.
- the JP-A-10168469 also describes salt mixtures which are in the molten state at the operating temperatures at which they are used.
- the lubricants described herein contain 75-95 weight percent disodium hydrogen phosphate and / or potassium phosphate and 5-25 weight percent sodium chloride. The sodium chloride is added to lower the melting point.
- the lubricants described therein optionally contain 10-50% by weight of graphite.
- the GB-A-350275 describes a method of treating wires to be drawn in a cold condition in which the material to be drawn is first treated in an acid bath, then neutralized with a trisodium phosphate solution and cold drawn with mineral oil as a lubricant.
- the problem underlying the invention was thus to obtain a process with a high-temperature lubricant to which no graphite must be added and which reduces the reject rates compared to a use of known lubricant.
- the service life of Domstangen be increased in the metal tube production and the quality of the inner tube surfaces can be improved.
- This object is achieved by the use of alkali metal phosphate in high-temperature lubricants for lubricating two surface contacting heated metal objects that perform a relative movement to each other, wherein the lubricant to at least 80 wt .-%, based on its solids content of at least one Alkali orthophosphate and a melting temperature above the maximum working temperature of the heated metal objects, but at least above 600 ° C, has.
- alkali phosphates in such lubricants only make up a relatively small percentage and are so mixed with other salts that the lubricant is in a molten, that is liquid state, at the working temperatures.
- alkali metal phosphate in a high-temperature lubricant can be used wherever, at high temperatures, two metal objects in contact with each other in a plane make a relative movement relative to one another. These are, for example, bearings in which high temperatures can occur.
- the lubricants according to the invention are used where the surface-contacting metal objects are, on the one hand, a tool and, on the other hand, a workpiece.
- the lubricants are suitable for lubricating mandrel bars in the manufacture of seamless metal tubes.
- the inventive concept is suitable for lubricating any metal objects, but is particularly suitable for the machining of steel objects, in particular, as mentioned above, for the production of seamless steel tubes in which the dowel bars are lubricated with the lubricant according to the invention.
- this should not exclude the use of lubricants of the invention, for example, for the production of tubes made of non-ferrous metals, aluminum or the like.
- the high temperature lubricant in the inventive use is in the form of an aqueous solution.
- This is sprayed or otherwise applied, for example, on the Domstangen in pipe production and forms after evaporation of the water, a fine release and lubricant film, which is extremely resistant to abrasion in use. Since the lubricant does not melt due to its high melting temperature in use, scale is prevented from being fixed by the lubricant on the mandrel bar surface or other tool surface. After drying, the lubricant is in the form of very fine particles, which fill all surface roughness of the tool surface and thus smooth this surface, which is transferred to the workpiece surface.
- the formed release film also promotes the material flow of the metal to be formed on the tool surface and therefore has the property of an excellent lubricating film.
- alkali metal phosphate in a high-temperature lubricant is particularly suitable in the atelier rolling process with the technology of the "free dome bar” and in the impact bench process. Even when Kontiwalzen, z. B. on the “semifloating" principle, significant advantages in terms of surface quality, the service life of the mandrels and the force between the rolling stands are achieved.
- the lubricants can easily be used to produce clear, high-percentage solutions which are applied to the mandrels by means of an airless pump and nozzles.
- the atomization is also possible by means of air, so-called two-fluid nozzles or the like.
- the lubricant can also be applied in powder form.
- the melting temperature of the lubricant is suitably at least 10 ° C above the maximum working temperature, as defined above, in the use according to the invention.
- the lubricant should largely consist of one or more alkali orthophosphates; the content of alkali orthophosphate is expediently at least 95% by weight. If several Alkali orthophosphates are used, it is important to ensure that even with such mixtures, the melting temperature is above the maximum operating temperature.
- lubricant Up to a maximum of 20% by weight, preferably up to a maximum of 5% by weight, of the lubricant may consist of other substances, which may also include small amounts of graphite, which is generally not preferred.
- the appropriately used alkali orthophosphates are trisodium orthophosphate having a melting temperature of 1583 ° C, tripotassium orthophosphate having a melting temperature of 1340 ° C and trilithium orthophosphate having a melting temperature of 857 ° C. Trisodium orthophosphate and tripotassium orthophosphate are preferred, especially the latter. As far as the melting temperature of the lubricant remains high enough, other phosphates can be added in small amounts.
- the actual melting temperature of the lubricant in the use according to the invention depends on the maximum working temperature in the use of the lubricant and thus on the nature of the surface touching heated metal objects.
- the melting temperature of the lubricant may be relatively low, if it is to be used to produce pipes of non-ferrous metal or aluminum, since relatively low operating temperatures are used for these metallic materials.
- a lubricant with significantly higher melting temperatures which in turn depend on whether chromium-nickel steels with working temperatures of about 1050 to 1100 ° C or steels with higher working temperatures are used.
- the melting temperature for lubricating tools for steel workpieces such as when lubricating mandrel bars for the production of steel pipes above 1100 ° C, preferably above 1200 ° C.
- the melting temperatures may be 600 or 650 ° C.
- the service life of the Asseldome could be increased by 25% compared to known lubricant smeared Asseldornen.
- the roughness measurements of the inner surface of the finished tubes, which were used for rolling bearings, resulted in a reduction of 22 microns to 10 microns.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10154062A DE10154062A1 (de) | 2001-11-02 | 2001-11-02 | Hochtemperatur-Schmiermittel und dessen Verwendung |
| DE10154062 | 2001-11-02 | ||
| PCT/DE2002/003772 WO2003040274A1 (de) | 2001-11-02 | 2002-10-04 | Hochtemperatur-schmiermittel und dessen verwendung |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1444314A1 EP1444314A1 (de) | 2004-08-11 |
| EP1444314B1 true EP1444314B1 (de) | 2007-07-18 |
Family
ID=7704527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP02782698A Expired - Lifetime EP1444314B1 (de) | 2001-11-02 | 2002-10-04 | Verwendung von Alkaliphosphat in einem Hochtemperatur-Schmiermittel |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1444314B1 (pl) |
| AT (1) | ATE367426T1 (pl) |
| DE (2) | DE10154062A1 (pl) |
| ES (1) | ES2288563T3 (pl) |
| PL (1) | PL197304B1 (pl) |
| WO (1) | WO2003040274A1 (pl) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB350275A (pl) * | 1929-11-27 | 1931-06-11 | Rudolf Wilhelm Moll | |
| JPS6017477B2 (ja) * | 1983-02-02 | 1985-05-02 | 日本工作油株式会社 | 水溶性金属加工用潤滑剤 |
| EP0829528B1 (de) * | 1996-09-17 | 2003-06-18 | Chemische Fabrik Budenheim KG | Graphitfreier Dornstangenschmierstoff |
| JPH10168469A (ja) * | 1996-12-11 | 1998-06-23 | Nippon Steel Corp | 継目無鋼管圧延用潤滑剤 |
-
2001
- 2001-11-02 DE DE10154062A patent/DE10154062A1/de not_active Withdrawn
-
2002
- 2002-10-04 DE DE50210522T patent/DE50210522D1/de not_active Expired - Lifetime
- 2002-10-04 WO PCT/DE2002/003772 patent/WO2003040274A1/de active IP Right Grant
- 2002-10-04 ES ES02782698T patent/ES2288563T3/es not_active Expired - Lifetime
- 2002-10-04 AT AT02782698T patent/ATE367426T1/de active
- 2002-10-04 PL PL368159A patent/PL197304B1/pl unknown
- 2002-10-04 EP EP02782698A patent/EP1444314B1/de not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| ES2288563T3 (es) | 2008-01-16 |
| EP1444314A1 (de) | 2004-08-11 |
| PL197304B1 (pl) | 2008-03-31 |
| WO2003040274A1 (de) | 2003-05-15 |
| DE10154062A1 (de) | 2003-05-15 |
| DE50210522D1 (de) | 2007-08-30 |
| PL368159A1 (pl) | 2005-03-21 |
| ATE367426T1 (de) | 2007-08-15 |
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| Date | Code | Title | Description |
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| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
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| AX | Request for extension of the european patent |
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| 17Q | First examination report despatched |
Effective date: 20051118 |
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| GRAP | Despatch of communication of intention to grant a patent |
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| RTI1 | Title (correction) |
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