Classifications

• • C—CHEMISTRY; METALLURGY
  • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
  • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
  • C10L1/00—Liquid carbonaceous fuels
  • C10L1/10—Liquid carbonaceous fuels containing additives
  • C10L1/14—Organic compounds
  • C10L1/18—Organic compounds containing oxygen
  • C10L1/19—Esters ester radical containing compounds; ester ethers; carbonic acid esters

Definitions

• This invention relates to diesel fuel compositions, their preparation and their uses, as well as to the use of a particular fuel component for a new purpose.
• FAAEs fatty acid alkyl esters
• diesel fuel compositions They are typically derivable from biological sources and can be used to reduce the environmental impact from production and use of a conventional petrol-derived fuel.
• RME rapeseed methyl ester
• fatty acid methyl esters are well known to have poor cold flow properties compared to typical diesel base fuels (as evidenced by their relatively high cold filter plugging points, CFPPs), and it would therefore be expected that when added to another diesel fuel they would impair its low temperature performance. This effect has indeed been observed in many base fuel/FAME blends.
• a diesel fuel composition containing a palm oil alkyl ester (POAE), wherein the POAE concentration is up to 25 % v/v based on the overall composition.
• POAE palm oil alkyl ester
• the POAE concentration is greater than 5 % v/v; more preferably it is 8 or 10 % v/v or greater.
• the composition will contain, in addition to the POAE, a major proportion of a diesel base fuel.
• a "major proportion” means suitably 70 % v/v or greater, preferably 75 or 80 % v/v or greater, in cases up to 85 or 90 % v/v or greater.
• palm oil alkyl ester or "POAE” is meant an alkyl ester of an oil derived from either the fruit or the seed (preferably the fruit) of Elaeis guineensis Jacq., Palmae .
• This palm oil will chiefly comprise palmitin, with some quantities of stearin and linolein.
• the alkyl ester may be synthesised for instance by esterification (typically base-catalysed, such as by KOH) of the palm oil with a suitable alcohol; for example, the methyl ester can be synthesised by esterification with methanol.
• the POAE will be a C 1 to C 5 alkyl ester, more preferably either the methyl, ethyl or propyl (suitably iso-propyl) ester, yet more preferably either the methyl or ethyl ester. Most preferably it will be palm oil methyl ester (POME).
• POME palm oil methyl ester
• the POAE suitably complies with specifications applying to the base fuel which forms the major proportion of the fuel composition, bearing in mind the intended use to which the composition is to be put (for example, in which geographical area and at what time of year).
• the POAE preferably has a flash point (IP 34) of greater than 101 °C; a kinematic viscosity at 40 °C (IP 71) of 1.9 to 6.0 centistokes, preferably 3.5 to 5.0 centistokes; a density from 845 to 910 kg/m 3 , preferably from 860 to 900 kg/m 3 , at 15 °C (IP 365, EN ISO 12185 or EN ISO 3675); a water content (IP 386) of less than 500 ppmw (parts per million by weight); a T95 (the temperature at which 95 % of the fuel has evaporated, measured according to IP 123) of less than 360 °C; an acid number (IP 139) of less than 0.8 mgKOH/g, preferably less than 0.5 mgK
• It also preferably contains (eg, by NMR) less than 0.2 % w/w of free methanol, less than 0.02 % w/w of free glycerol and greater than 96.5 % w/w esters.
• POAE fatty acid methyl esters for use as diesel fuels.
• the cold filter plugging point of the POAE (IP 309) is suitably from +10 to +15 °C, such as from +11 to +14 °C.
• the POAE may be included in the composition with one or more other fatty acid alkyl esters, in particular fatty acid methyl esters, which may be pre-blended with the POAE or added to the fuel composition separately.
• the concentration of the POAE in the fuel composition is preferably up to 22 % v/v, based on the overall fuel composition, more preferably up to 20 % v/v and most preferably up to 15 % v/v. Its concentration may be as low as 15 % v/v, in cases as low as 13 %, 12.5 %, 12 %, 11 %, 10 % or 7.5 % v/v, or in cases as low as 6 %, 5 %, 3 %, 2 % or even 1 % v/v.
• the POAE concentration may suitably be from 5 to 20 % v/v, more preferably from 7.5 to 15 or 20 % v/v such as from 10 to 15 % v/v based on the overall composition.
• the diesel base fuel used in a composition according to the invention may be any known diesel base fuel, and it may itself comprise a mixture of diesel fuel components. It will preferably have a sulphur content of at most 2000 ppmw (parts per million by weight). More preferably it will have a low or ultra low sulphur content, for instance at most 500 ppmw, preferably no more than 350 ppmw, most preferably no more than 100 or 50 or 30 or even 10 ppmw, of sulphur.
• the fuel composition after addition of the POAE will also preferably have a sulphur content within these ranges.
• the base fuel is not a sulphur-free (“zero sulphur”) fuel.
• Typical diesel fuel components comprise liquid hydrocarbon middle distillate fuel oils, for instance petroleum derived gas oils.
• Such base fuel components may be organically or synthetically derived. They will typically have boiling points within the usual diesel range of 150 to 400 °C, depending on grade and use. They will typically have densities from 0.75 to 0.9 g/cm 3 , preferably from 0.8 to 0.86 g/cm 3 , at 15 °C (IP 365) and cetane numbers (ASTM D613) of from 35 to 80, more preferably from 40 to 75. Their initial boiling points will suitably be in the range 150 to 230 °C and their final boiling points in the range 290 to 400 °C. Their kinematic viscosity at 40 °C (IP 71) might suitably be from 1.5 to 4.5 centistokes.
• the fuel composition of the invention which includes the POAE, will also preferably fall within these general specifications.
• Such fuels are generally suitable for use in a compression ignition (diesel) internal combustion engine, of either the indirect or the direct injection type.
• the base fuel may be an ultra low sulphur fuel (ie, no more than 50 ppmw sulphur), and/or for it to contain no refinery additives, or at least no additional cold flow additives. It will preferably be a "summer grade" fuel, and/or be suitable and/or intended for use in climates unlikely to suffer extremely low temperatures. This applies for example where the ambient temperature is unlikely to fall below - 6 or even -8 °C. Diesel fuels for use in New Zealand, for instance, currently need only comply with a cold filter plugging point (CFPP) specification down to -6 °C, for South Africa compliance is only necessary to -4 °C and for some regions of China a CFPP between +4 and +12 °C is considered acceptable. In diesel fuel compositions intended for this type of use, the present invention can make it possible to use the POAE as a substitute (either complete or partial) for conventional cold flow additives, as will be described below.
• CFPP cold filter plugging point
• a petroleum derived gas oil may be obtained from refining and optionally (hydro)processing a crude petroleum source. It may be a single gas oil stream obtained from such a refinery process or a blend of several gas oil fractions obtained in the refinery process via different processing routes. Examples of such gas oil fractions are straight run gas oil, vacuum gas oil, gas oil as obtained in a thermal cracking process, light and heavy cycle oils as obtained in a fluid catalytic cracking unit and gas oil as obtained from a hydrocracker unit.
• a petroleum derived gas oil may comprise some petroleum derived kerosene fraction.
• Such gas oils may be processed in a hydrodesulphurisation (HDS) unit so as to reduce their sulphur content to a level suitable for inclusion in a diesel fuel composition.
• HDS hydrodesulphurisation
• the base fuel may be or contain another so-called “biodiesel” fuel component, such as an alcohol (in particular methanol or ethanol) or other oxygenate or a vegetable oil or vegetable oil derivative other than a POAE.
• biodiesel such as an alcohol (in particular methanol or ethanol) or other oxygenate or a vegetable oil or vegetable oil derivative other than a POAE.
• Fischer-Tropsch derived fuel in particular a Fischer-Tropsch derived gas oil.
• Such fuels are known and in use in diesel fuel compositions. They are, or are prepared from, the synthesis products of a Fischer-Tropsch condensation reaction, as for example the commercially used gas oil obtained from the Shell Middle Distillate Synthesis (Gas To Liquid) process operating in Bintulu (Malaysia).
• a diesel fuel composition according to the invention may contain no, or only low levels of, other cold flow additives such as flow improvers and wax anti-settling agents.
• a "low level” in this context is suitably 200 ppmw or less, preferably 100 or 50 ppmw or less, yet more preferably 25 or 10 or 5 ppmw or less.
• the composition of the invention may contain other components in addition to the diesel base fuel and the POAE.
• fuel additives include detergents such as polyolefin substituted succinimides or succinamides of polyamines, for instance polyisobutylene succinimides or polyisobutylene amine succinamides, aliphatic amines, Mannich bases or amines and polyolefin (eg, polyisobutylene) maleic anhydrides (suitable detergents can be obtained from Infineum (eg, F7661 and F7685) and Octel (eg, OMA 4130D)); lubricity enhancers such as EC 832 and PARADYNETM (ex Infineum), HITECTM E580 (ex Ethyl Corporation) and VEKTRONTM 6010 (ex Infineum) and amide-based additives such as those available from the Lubrizol Chemical Company, for instance LZ 539 C; dehazers, e
• the fuel composition will suitably contain only a minor amount of such additives.
• the (active matter) concentration of each such additional component in the overall fuel composition is preferably up to 1 % w/w, more preferably in the range from 5 to 1000 ppmw, advantageously from 75 to 300 ppmw, such as from 95 to 150 ppmw.
• a lubricity enhancer be included in the composition, especially when it has a low (eg, 500 ppmw or less) sulphur content.
• the lubricity enhancer is conveniently present at a concentration from 50 to 1000 ppmw, preferably from 100 to 1000 ppmw, based on the overall fuel composition.
• the POAE may itself help to improve lubricity, lower levels of lubricity enhancer may be sufficient.
• Additives may be added at various stages during the production of a fuel composition; those added at the refinery for example might be selected from anti-static agents, pipeline drag reducers and (subject to the above comments) flow improvers (eg, ethylene/vinyl acetate copolymers or acrylate/maleic anhydride copolymers) and wax anti-settling agents (eg, those commercially available under the trade marks "OCTEL” (eg, OCTELTM W 5000, ex Octel) and "DODIFLOW” (eg, DODIFLOWTM v 3958, ex Hoechst) or as R474 (ex Infineum)).
• OCTEL eg, OCTELTM W 5000, ex Octel
• DODIFLOW eg, DODIFLOWTM v 3958, ex Hoechst
• R474 Ex Infineum
• a POAE in a diesel fuel composition, for the purpose of improving the cold flow performance of the composition.
• a POAE in a diesel fuel composition means incorporating the POAE into the composition, typically as a blend (ie, a physical mixture) with one or more other fuel components and optionally with one or more fuel additives.
• the POAE is conveniently incorporated before the composition is introduced into an internal combustion engine or other system which is to be run on the composition.
• the use may involve running a diesel engine on the fuel composition containing the POAE, typically by introducing the composition into a combustion chamber of the engine.
• “Improving” embraces any degree of improvement compared to the cold flow performance of the fuel composition before the POAE is added.
• a POAE can act to improve the cold flow performance of a diesel fuel composition.
• certain fatty acid alkyl esters have poor cold flow properties compared with typical diesel base fuels.
• the cold filter plugging point (CFPP) of palm oil methyl ester (POME) is +10 to +15 °C, typically ⁇ 11 °C, as compared to -6 to -8 °C for a typical ultra low sulphur diesel base fuel without cold flow additives.
• CFPP cold filter plugging point
• POME palm oil methyl ester
• the present invention is able to provide a more optimised method for improving the cold flow performance (ie, reducing the CFPP) of a diesel fuel composition to reach a particular target value, as will be further described in connection with the third aspect of the invention.
• the invention moreover makes possible - and indeed desirable - the use of a POAE in a diesel fuel composition, often at higher concentrations than have previously been thought suitable.
• This can bring other benefits in addition to the improvement in cold flow performance, for example improved lubricity performance (it is already known to add fatty acid alkyl esters to diesel fuel compositions for this purpose), a reduction in life cycle greenhouse gas emissions and potentially reduced costs in particular compared to the use of other available "biofuels" such as RME.
• the cold flow performance of the fuel composition is suitably assessed by measuring its cold filter plugging point (CFPP), preferably using the standard test method IP 309 or an analogous technique.
• CFPP cold filter plugging point
• IP 309 standard test method
• the CFPP of the composition is reduced by at least 1 °C compared to its value prior to addition of the POAE, more preferably by at least 2 °C, yet more preferably by at least 3 °C and most preferably by at least 4 °C.
• the CFPP of the composition is reduced by at least 0.3 % of its value (expressed in Kelvin) prior to addition of the POAE, more preferably by at least 0.5 or 0.7 % and most preferably by at least 1 or 1.2 or 1.5 or even 1.6 %.
• the POAE is preferably used in the fuel composition at a concentration of up to 25 % v/v, based on the overall fuel composition after POAE addition, more preferably at a concentration of up to 22 % v/v, yet more preferably at up to 20 % v/v and most preferably at up to 15 % v/v. It may be used at a concentration of as low as 12 %, 10 % or 7.5 % v/v, or in cases as low as 6 %, 5 %, 3 %, 2 % or even 1 % v/v.
• the POAE may suitably be used at a concentration of from 5 to 20 % v/v, more preferably from 7.5 to 15 or 20 % v/v, such as from 10 to 15 % v/v, based on the overall fuel composition after POAE addition.
• the fuel composition prior to addition of the POAE, suitably comprises a major proportion of a diesel base fuel.
• major proportion here is meant typically 80 % v/v or greater, suitably 90 or 95 % v/v or greater; most preferably 98 or 99 or 99.5 % v/v or greater or in cases 100 %.
• the composition which results from carrying out the present invention will contain only the diesel base fuel and the POAE; the invention thus embraces the addition of a POAE to a diesel base fuel so as to improve its cold flow properties, and the improvement may be with respect to the properties of the base fuel alone.
• the composition may contain other components, in particular diesel fuel additives, as described above in connection with the first aspect of the invention.
• composition which results from the method of the invention may contain no, or only low levels of, other cold flow additives.
• a "low level” in this context is suitably 200 ppmw or less, preferably 100 or 50 ppmw or less, yet more preferably 25 or 10 or 5 ppmw or less.
• the invention thus embraces the use of a POAE in a diesel fuel composition for the purpose of reducing the level of cold flow additives in the composition.
• reducing embraces reduction to zero; in other words, the POAE may be used to replace one or more cold flow additives either partially or completely.
• the reduction may be as compared to the level of the relevant additive(s) which would otherwise have been incorporated into the fuel composition in order to achieve a desired target CFPP, for instance in order to meet government fuel specifications or consumer expectations.
• the POAE can help in reducing the overall additive levels in the composition and their associated costs.
• the POAE is used to reduce the w/w concentration of the relevant additive(s) in the fuel composition by at least 10 %, more preferably by at least 20 or 30 %, yet more preferably by at least 50 or 70 or 80 or even 90 % or, as described above, by 100 %.
• cold flow additive(s) may for instance be used to replace cold flow additive(s) to an extent that the concentration of cold flow additives remaining in the fuel composition is 300 ppmw or less, preferably 200 ppmw or less, more preferably 100 or 50 ppmw or less. Most preferably it may be used to replace cold flow additive(s) substantially entirely, the fuel composition being nearly or essentially free of such additives and containing for example 10 or 5 ppmw or less, preferably 1 ppmw or less, of cold flow additives.
• cold flow additive refers to an additive, other than the POAE, which improves the low temperature performance of a fuel (eg, lowering its CFPP).
• the fuel composition may contain no, or only low levels of, refinery additives other than cold flow additives.
• the POAE may be used in the fuel composition for one or more other purposes in addition to the desire to improve cold flow performance, for instance to reduce environmental impact, to improve lubricity and/or to reduce costs.
• the cold flow performance of the resultant fuel composition it may be sufficient, for the purposes of the invention, that the cold flow performance of the resultant fuel composition be no worse than, or not substantially worse than, the cold flow performance of the composition before addition of the POAE; in other words the cold flow performance of the composition is maintained alongside the other purposes achieved by addition of the POAE.
• maintenance of the cold flow properties may mean that the CFPP of the composition is not increased by more than 1 % of its value (in Kelvin) prior to addition of the POAE, preferably not by more than 0.75 or 0.5 % and most preferably not by more than 0.2 or even 0.1 or 0.05 %. It may mean that the CFPP of the composition is not increased by more than 3 °C, preferably not by more than 2 °C, most preferably not by more than 1 or 0.5 °C, compared to its value prior to addition of the POAE.
• the present invention therefore also embraces the use of a POAE in a diesel fuel composition for two or more simultaneous purposes, one of which is to maintain the CFPP of the composition below a certain desired level.
• This desired level may be the CFPP of the composition prior to addition of the POAE.
• the present invention provides a method for altering (typically reducing) the CFPP of a diesel fuel composition which contains a major proportion of a diesel base fuel, in order to reach a target CFPP X, which method comprises adding to the base fuel an amount x of a POAE having a CFPP B which is higher than the CFPP A of the base fuel, wherein x is greater than the amount of POAE which could be added to the base fuel, without exceeding the target CFPP X, if linear blending rules applied.
• a "major proportion" of a base fuel means typically 80 % v/v or greater, more suitably 90 or 95 % v/v or greater, yet more suitably 98 or 99 or 99.5 % v/v or greater or in cases 100 %.
• "Reaching" a target CFPP generally means attaining a CFPP at or below the target value.
• the POAE will typically be added to the base fuel as a blend (ie, a physical mixture), conveniently before the overall composition is introduced into an internal combustion engine or other system which is to be run on the composition.
• Other fuel components and/or fuel additives may also be incorporated into the composition, either before or after addition of the POAE and either before or during use of the composition in a combustion system.
• the actual volume fraction of the POAE, v may be at least 0.02 or 0.05 greater than the "linear" volume fraction v', more preferably at least 0.08 or 0.1 greater, most preferably at least 0.15 or 0.2 greater than v'.
• the actual volume fraction v is preferably 0.25 or less, more preferably 0.22 or less, yet more preferably 0.2 or 0.15 or 0.1 or 0.07 or less. It may for example be from 0.01 to 0.25, preferably from 0.05 to 0.25, more preferably from 0.05 or 0.1 to 0.2.
• the concentration of the POAE in the overall fuel composition (or at least in the base fuel/POAE mixture) will preferably be as described above in accordance with the first and/or the second aspect of the invention.
• the present invention provides a method for reducing the CFPP of a diesel fuel composition, and/or for preparing a diesel fuel composition with a CFPP at or below a desired target CFPP X, the method comprising selecting a diesel base fuel and a POAE; measuring the CFPP of mixtures of the base fuel and the POAE at 2 or more, preferably 3 or 5 or 7 or more, POAE concentrations between 0 and 100 % v/v; determining an optimal POAE concentration, or a range of optimal POAE concentrations, where the CFPP is lower than that of the base fuel alone and preferably where the CFPP reaches a minimum level; and formulating a diesel fuel composition containing the diesel base fuel and the POAE at the optimal concentration or at a concentration within the optimal range.
• This method may be used in a similar fashion to that of the third aspect of the invention.
• the methods of the second, third and fourth aspects of the invention may additionally or alternatively be used to adjust any property of the diesel fuel composition which is equivalent to or directly or indirectly associated with CFPP or cold flow performance generally.
• a method according to the second, third or fourth aspect of the invention may form part of a process for, or be implemented using a system for, controlling the blending of a fuel composition, for example in a refinery.
• a system will typically include means for introducing a POAE and a diesel base fuel into a blending chamber, flow control means for independently controlling the volumetric flow rates of the POAE and the base fuel into the chamber, means for calculating the volume fraction of the POAE needed to achieve a desired target CFPP input by a user into the system and means for directing the result of that calculation to the flow control means which is then operable to achieve the calculated volume fraction in the product composition by altering the flow rates of its constituents into the blending chamber.
• a process or system of this type will suitably make use of known CFPP values for the base fuel and POAE concerned, and conveniently also a model predicting the CFPP of varying concentration blends of the two according to linear blending rules.
• the process or system may then, according to the invention, select and produce a POAE volume fraction higher than that predicted by the linear blending model to be possible.
• It may use a so-called quality estimator which will provide, using a model, a real-time prediction of the CFPP of each resulting blend from available raw process measurements, such as for example the measured CFPP values and the volumetric flow rates of the constituents. More preferably such a quality estimator is calibrated on-line by making use of for example a method analogous to that described in WO-A-02/06905.
• Methods according to the invention may thus conveniently be used to automate, at least partially, the formulation of a diesel fuel composition, preferably providing real-time control over the relative proportions of the POAE and base fuel incorporated into the composition, for instance by controlling their relative flow rates.
• a POAE in any of the ways described above may also embrace supplying a POAE, or a formulation containing a POAE, together with instructions for its use in a diesel fuel composition to improve or maintain the cold flow performance of the composition and/or to reduce the level of cold flow or other additives in the composition and/or to achieve a target maximum CFPP X.
• the POAE may be supplied as a component of a formulation suitable and/or intended for use as a fuel additive, in which case the POAE may be included in the formulation for the purpose of influencing the effects of the overall formulation on the cold flow performance of a fuel.
• the POAE is preferably a C 1 to C 5 alkyl ester, more preferably a methyl, ethyl or propyl (suitably iso-propyl) ester, yet more preferably a methyl or ethyl ester and most preferably the methyl ester. It is preferably used in the absence of other cold flow enhancing additives.
• a fifth aspect of the invention provides a diesel fuel composition prepared, or preparable, using a method according to the second or the third aspect.
• This composition will suitably contain a major proportion of a diesel base fuel having an ultra low sulphur content (for example, less than 50 ppmw); and/or a CFPP (IP 309) of -6 to -10 °C.
• Preferred features of the fifth aspect of the invention for instance regarding the nature of the POAE, the diesel base fuel and any other constituents of the fuel composition, may be as described above in connection with the first aspect.
• the invention provides a method of operating a diesel engine, and/or a vehicle which is driven by a diesel engine, which method involves introducing into a combustion chamber of the engine a diesel fuel composition according to the first and/or the fifth aspect of the invention.
• the fuel composition may be used in this way for a purpose as referred to in connection with the second, third and/or fourth aspects of the invention, conveniently to improve the low temperature performance of the engine.
• a seventh aspect of the invention provides a process for the preparation of a diesel fuel composition, such as a composition according to the first or the fifth aspect, which process involves blending a diesel base fuel with a POAE, either for the purpose of improving the cold flow performance of the composition and/or so as to achieve a POAE concentration of up to 25 % v/v, preferably more than 5 % v/v, in the overall composition.
• the example shows fuel compositions according to the present invention and illustrates the effect of a palm oil alkyl ester on the cold flow performance of a typical ultra low sulphur diesel base fuel.
• the base fuel used was a summer grade ultra low sulphur diesel having the properties listed in Table A. It contained no cold flow additives and no refinery additives.
• Table A Fuel property Test method Density @ 15 °C (kg/m 3 ) IP 365 827.1 Viscosity @ 40 °C IP 71 2.467 (centistokes) Distillation (°C) IP 123 IBP 168 10% recovery 200 20% 214 30% 231 40% 249 50% 264 60% 279 70% 294 80% 310 90% 329 95% 345 FBP 352 Cloud point (°C) IP 219 -7 Sulphur (ppmw) ASTM D2622 46
• the POME was sourced from Malaysia and had the properties listed in Table B.
• Table B POME property Test method Density @ 15 °C (kg/m 3 ) IP 365 874.2 Acid number (total) IP 139 0.16 (mgKOH/g) Iodine number IP 84 52 (gI 2 /100g) Water content (ppmw) UK 3367 315 Viscosity @ 40 °C IP 71 4.385 (centistokes) Distillation (°C) IP 123 IBP 320.1 10% recovery 323.7 20% 324.3 30% 325.2 40% 325.4 50% 326.5 60% 327.1 70% 328.5 80% 329.7 90% 332.9 95% 336.8 FBP 346.3 Cloud point (°C) IP 219 14 Sulphur (ppmw) ASTM D2622 ⁇ 5
• FAME fatty acid methyl ester
• Other fatty acid alkyl esters have demonstrated similar trends in a range of diesel base fuels, acting to increase the CFPP (and hence worsen cold flow performance) at any concentration. This makes the effect observed with palm oil alkyl esters even more surprising.

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• 2004
  • 2004-12-24 EP EP04258148A patent/EP1674552A1/fr not_active Withdrawn

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