EP0819788B1 - Needling aid for producing needle felts, a needle felt produced by using it, and a method for production thereof - Google Patents
Needling aid for producing needle felts, a needle felt produced by using it, and a method for production thereof Download PDFInfo
- Publication number
- EP0819788B1 EP0819788B1 EP97111983A EP97111983A EP0819788B1 EP 0819788 B1 EP0819788 B1 EP 0819788B1 EP 97111983 A EP97111983 A EP 97111983A EP 97111983 A EP97111983 A EP 97111983A EP 0819788 B1 EP0819788 B1 EP 0819788B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- needle
- needling aid
- aid according
- needling
- approx
- 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
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4218—Glass fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
Definitions
- the present invention concerns a needling aid for producing needle felts of mineral wool in accordance with claim 1, and its use for producing a needle felt in accordance with claim 10.
- Needle felts are particularly suited for thermal insulation in household appliances, for instance in ovens and cookers as well as in industrial muffle-type furnaces.
- a needling aid, or finishing agent For needle-punching mineral wool felts, a needling aid, or finishing agent, must be applied onto the fibers as an additive. Such finishing agents are variously produced on the basis of mineral oils, natural oils or fatty acid derivatives. The finishing agent is required for making the fibers smooth and reducing their mutual friction during the needle-punching process to prevent breakage or rupturing of the fibers during needle-punching as far as possible. The finishing agent must furthermore be capable of binding dusts released during the production process, to thereby permit processing and utilisation of the needle felt in the absence of any additional dust protection measures.
- finishing agents are sprayed onto the fibers in the chute of a fiberising machine for the molten glass material, or directly onto the felt mat. This implies a tradeoff with respect to viscosity inasmuch as sufficient spraying must be ensured on the one hand, whereas a material having a sufficiently high viscosity must be retained following evaporation of the carrier material in order to guarantee the above mentioned advantages for the needle-punching process.
- a thixotropising additive is used with a standard finishing agent on a fatty acid polyglycolester basis.
- Such a thixotropising additive has the advantage of having a high viscosity at rest and thus holding the fiber loops in their anchoring positions achieved by the needle-punching process, whereas the presence of a low dynamic viscosity results in good needle-punching properties and a good lubricating effect. Owing to a high degree of fluidity while the needles are acting on the felt to be needle-punched, it is possible to have to add only small quantities of needling aid, whereby malodors under the effect of heat are correspondingly diminished.
- the needling aid of the invention contains an aqueous dispersion of at least one at least partly halogenated polymer and an alcohol, on the one hand there result excellent oil-like finishing agent properties owing to the molecular conditions, and on the other hand those are chemically inert, halogenated polymers which, as a rule, resist thermal decomposition or are otherwise decomposed into nontoxic products.
- Such partly halogenated polymers are selected from the group consisting of:
- perfluorated perchlorated
- perbrominated are meant to indicate that practically each hydrogen atom within the polymer is replaced by a corresponding halogen atom, wherein one or both terminal groups can be not halogenated or partly halogenated.
- Formaldehyde could be detected neither in the chute nor in the final needle felt which was exposed to a temperature of up to 500°C for approx. 1 hour.
- the perfluorated polyethers in accordance with claim 4 have hitherto turned out to be particularly suitable needling aids as they bring about extremely favorable sliding properties between the fiber loops during needle-punching on the one hand, and as practially all hydrogen atoms within the polyether system are replaced by fluorine atoms on the other hand, such perfluorated polyethers are chemically inert and also thermally resistant.
- the perfluorated polyether in accordance with claim 5 has been found to be a particularly preferred embodiment of a needling aid, which is commercially available e.g. under the designation Fomblin FE 20C.
- Adding a sterically inhibited alcohol, preferably t-butanol, to the needling aid in addition to the halogenated polymer in accordance with claims 6 and 7 has the advantage that the dispersion is stabilised by it, with the t-butanol, having a boiling point of approx. 80°C, instantaneously evaporating in the chute without furthermore leaving behind any decomposition products. Addition of such an alcohol stabilises the dispersion or emulsion in water of the polymer used.
- a particularly preferred needling aid is one in accordance with claim 8, wherein the dispersion is present as an aqueous micro-emulsion.
- Such micro-emulsion has the advantage that it presents homogeneous distribution of the utilised halogenated polymer in water even without any costly mixing processes, such that the obtained good results are also reproduceable in subsequent lots.
- the aqueous emulsion Upon application onto the fibers of the mineral wool, in particular glass wool, the aqueous emulsion preferably has a concentration of approx. 0.1 to 0.5% (wt.) of halogenated polymer and approx. 0.05 to 0.45% (wt.) of t-butanol. At these final concentrations during application onto the mineral wool, only small quantities of needling aid are required to obtain the properties desired for needle-punching.
- the needle felts according to the invention are therefore well suited for thermal insulation in household appliances, in particular ovens and cookers, inasmuch as they produce neither unpleasant smells nor toxic decomposition products upon initial operation at the location of the end user.
- the needling aid according to the invention is suited for needle-punching mineral wool, particularly, however, having the form of glass wool.
- aqueous micro-emulsion of a perfluoropolyether commercially available under the designation "Fomblin FE 20C" was used.
- This emulsion has a polymer content of approx. 20% (wt.) and is stabilised with approx. 18% (wt.) of t-butanol.
- the commercially available solution is diluted with water to a polymer content of approx. 12% (wt.).
- 3 kg of the 12% emulsion are then added into 250 kg of water and mixed by means of a propeller agitator.
- a needle felt produced from glass wool in this manner has a bulk density of approx. 50 kg/m 3 and a thickness of approx. 17 mm.
- the needle felts thus produced were subjected to thermal load at approx. 250°C in a standard kitchen in accordance with DIN 44971 in previously annealed cookers, and possibly produced decomposition products were analysed.
- the needle felts of the present invention therefore have excellent suitability for use in household appliances such as ovens or cookers as a heat insulation material, as it was also found in tests with such apparatus that malodors occurred neither upon initial use nor upon use over a period of several weeks, and that toxic products are not released into the surrounding atmosphere.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Nonwoven Fabrics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
The present invention concerns a needling aid for producing needle felts
of mineral wool in accordance with claim 1,
and its use for producing a needle felt in accordance with claim 10.
Needle felts are particularly suited for thermal insulation in household
appliances, for instance in ovens and cookers as well as in industrial muffle-type
furnaces.
For needle-punching mineral wool felts, a needling aid, or finishing agent,
must be applied onto the fibers as an additive. Such finishing agents are
variously produced on the basis of mineral oils, natural oils or fatty acid
derivatives. The finishing agent is required for making the fibers smooth and
reducing their mutual friction during the needle-punching process to prevent
breakage or rupturing of the fibers during needle-punching as far as possible.
The finishing agent must furthermore be capable of binding dusts released
during the production process, to thereby permit processing and utilisation of
the needle felt in the absence of any additional dust protection measures.
Typically such finishing agents are sprayed onto the fibers in the chute of
a fiberising machine for the molten glass material, or directly onto the felt mat.
This implies a tradeoff with respect to viscosity inasmuch as sufficient spraying
must be ensured on the one hand, whereas a material having a sufficiently high
viscosity must be retained following evaporation of the carrier material in order
to guarantee the above mentioned advantages for the needle-punching
process.
Formerly, particularly suited finishing agents were therefore lubricating
oils and lubricants on mineral oil basis. A drawback of utilising such substances
as a needling aid did, however, reside in the fact that considerable amounts of
one or several emulsifiers had to be added for producing an aqueous
dispersion or emulsion to thereby prevent phase separation into mineral oil
phase and aqueous phase from occurring even as early as in the storage
container of the finishing agent dispenser. To this end, particularly alcohol,
alkoxylates and/or nonylphenol were used as emulsifiers in the past, however
these had the facultative disadvantage of decomposing and thereby releasing
formaldehyde upon being heated in needle felts which are utilised for thermal
insulation of household appliances, e.g. ovens and cookers, and industrial
muffle-type furnaces.
It has, however, also been found in the past that even if needle felts were
subjected to thermal after-treatment following needle-punching in order to
remove the needling aid - not to mention the increased expense in terms of
energy and costs - residual finishing agent and in particular residues of the
emulsifiers contained in it may still cause malodors or even the release of
formaldehyde at the location of the final user. This is particularly true for the
first few weeks of operation of ovens and cookers.
In order to avoid these difficulties, various approaches were tried in the
prior art. Thus it was attempted e.g. to disperse mineral oil products in water
via a high-pressure dispersion mixing device in such a way as to do away with
the addition of emulsifier. This did, however, amount to a major technical effort
on the one hand and did not provide the desired results on the other hand.
Another approach to avoid this problem was based on the fact that, in
accordance with DE-PS-42 01 868, a thixotropising additive is used with a
standard finishing agent on a fatty acid polyglycolester basis. Such a
thixotropising additive has the advantage of having a high viscosity at rest and
thus holding the fiber loops in their anchoring positions achieved by the needle-punching
process, whereas the presence of a low dynamic viscosity results in
good needle-punching properties and a good lubricating effect. Owing to a high
degree of fluidity while the needles are acting on the felt to be needle-punched,
it is possible to have to add only small quantities of needling aid, whereby
malodors under the effect of heat are correspondingly diminished.
It is, however, a drawback of this finishing agent, or of these needle felts
of the prior art, that malodors and thermal decomposition products, which are
particularly undesirable in the field of household appliances, continue to occur.
Starting out from this prior art, it is therefore an object of the present
invention to furnish a needling aid for producing a needle felt, which practically
does not release any toxic decomposition products, in particular any
formaldehyde, at temperatures occurring in the heat insulation particularly of
ovens and cookers.
With respect to a needling aid, this object is achieved through the
characterising features of claim 1. With respect to a needle felt, the above
object is achieved by the features of claim 10.
Since the needling aid of the invention contains an aqueous dispersion of
at least one at least partly halogenated polymer and an alcohol, on the one hand there result
excellent oil-like finishing agent properties owing to the molecular conditions,
and on the other hand those are chemically inert, halogenated polymers which,
as a rule, resist thermal decomposition or are otherwise decomposed into nontoxic
products. Such partly halogenated polymers are selected from the
group consisting of:
The terms "perfluorated", "perchlorated" and "perbrominated" are meant
to indicate that practically each hydrogen atom within the polymer is replaced
by a corresponding halogen atom, wherein one or both terminal groups can be
not halogenated or partly halogenated.
Formaldehyde could be detected neither in the chute nor in the final
needle felt which was exposed to a temperature of up to 500°C for approx. 1
hour.
Under practical conditions, the perfluorated polyethers in accordance with
claim 4 have hitherto turned out to be particularly suitable needling aids as they
bring about extremely favorable sliding properties between the fiber loops
during needle-punching on the one hand, and as practially all hydrogen atoms
within the polyether system are replaced by fluorine atoms on the other hand,
such perfluorated polyethers are chemically inert and also thermally resistant.
The perfluorated polyether in accordance with claim 5 has been found to
be a particularly preferred embodiment of a needling aid, which is commercially
available e.g. under the designation Fomblin FE 20C.
Adding a sterically inhibited alcohol,
preferably t-butanol, to the needling aid in addition to the halogenated polymer
in accordance with claims 6 and 7 has the advantage that the dispersion is stabilised
by it, with the t-butanol, having a boiling point of approx. 80°C, instantaneously
evaporating in the chute without furthermore leaving behind any decomposition
products. Addition of such an alcohol stabilises the dispersion or emulsion in
water of the polymer used.
A particularly preferred needling aid is one in accordance with claim 8,
wherein the dispersion is present as an aqueous micro-emulsion. Such micro-emulsion
has the advantage that it presents homogeneous distribution of the
utilised halogenated polymer in water even without any costly mixing
processes, such that the obtained good results are also reproduceable in
subsequent lots.
Upon application onto the fibers of the mineral wool, in particular glass
wool, the aqueous emulsion preferably has a concentration of approx. 0.1 to
0.5% (wt.) of halogenated polymer and approx. 0.05 to 0.45% (wt.) of t-butanol.
At these final concentrations during application onto the mineral wool, only
small quantities of needling aid are required to obtain the properties desired for
needle-punching.
Owing to the small amounts of needling aid according to the invention, the
incurred costs are reasonable compared with those of conventional finishing
agents.
In claim 10 the use of a needling aid according to any one of claims 1 to 9
is claimed to produce a needle felt of mineral wool. An important advantage of the needle
felt according to the invention resides in the fact that for the first time a
formaldehyde-free needle felt is available which will not release formaldehyde
even under a high thermal load of up to approx. 500°C in accordance with
claim 11.
The needle felts according to the invention are therefore well suited for
thermal insulation in household appliances, in particular ovens and cookers,
inasmuch as they produce neither unpleasant smells nor toxic decomposition
products upon initial operation at the location of the end user.
It should be noted in the framework of the present invention that the
needling aid according to the invention is suited for needle-punching mineral
wool, particularly, however, having the form of glass wool.
Further advantages and features of the present invention result from the
description of an embodiment.
For producing a needling aid composition according to the invention, an
aqueous micro-emulsion of a perfluoropolyether commercially available under
the designation "Fomblin FE 20C" was used. This emulsion has a polymer
content of approx. 20% (wt.) and is stabilised with approx. 18% (wt.) of t-butanol.
The perfluorated polyether used in the example had the following general
formula:
CF3-(O-CF(CF3)-CF2)n-(O-CF2)m-O-CF2-R,
with R = -COO- NH4 + or -C(OH)2-CF3, and n and m being integers with n/m
approx. 20 to 40.
For producing a practically applicable solution or dispersion, the
commercially available solution is diluted with water to a polymer content of
approx. 12% (wt.). In the preparing vessel of the needle felt line, 3 kg of the
12% emulsion are then added into 250 kg of water and mixed by means of a
propeller agitator.
This solution containing a final concentration of approx. 0.15% (wt.)
polymer, e.g. perfluoropolyether, was then sprayed onto e.g. a glass wool felt,
and the latter conveyed under a needle bench and subjected to a needle-punching
process. As an alternative, the needling aid of thet above example is
sprayed directly onto the fibers in the chute.
A needle felt produced from glass wool in this manner has a bulk density
of approx. 50 kg/m3 and a thickness of approx. 17 mm.
The needle felts thus produced were subjected to thermal load at approx.
250°C in a standard kitchen in accordance with DIN 44971 in previously
annealed cookers, and possibly produced decomposition products were
analysed.
Here it was found that on the one hand no toxic products were produced
at all, in particular neither formaldehyde nor hydrogen fluoride could be
detected in the oven exhaust air.
Thus annealing of the needling aid subsequent to the needle-punching
process, as it is frequently required with conventional finishing agents, is not
necessary. The needle felts of the present invention therefore have excellent
suitability for use in household appliances such as ovens or cookers as a heat
insulation material, as it was also found in tests with such apparatus that
malodors occurred neither upon initial use nor upon use over a period of
several weeks, and that toxic products are not released into the surrounding
atmosphere.
Claims (12)
- Needling aid for producing needle felts of mineral wool,
characterised in that
it contains an aqueous dispersion of at least one at least partly halogenated polymer which is selected from the group consisting of:halogenated polyethers, halogenated polyesters, halogenated polyols, as well as mixtures thereof, and an alcohol. - Needling aid according to claim 1,
characterised in that the polyethers, polyesters and/or polyols are fluorinated, chlorinated and/or brominated. - Needling aid according to claim 2,
characterised in that the polyethers, polyesters and/or polyols are perfluorinated, perchlorinated and/or perbrominated. - Needling aid according to claim 3, characterised in that it contains a perfluorinated polyether.
- Needling aid according to claim 4, characterised in that the perfluorinated polyether has the following general formula:
- Needling aid according to any one of claims 1 to 5, characterised in that the alcohol is a sterically inhibited alcohol.
- Needling aid according to claim 6, characterised in that the alcohol is t-butanol.
- Needling aid according to any one of claims 1 to 7, characterised in that the dispersion is present in the form of an aqueous micro-emulsion.
- Needling aid according to any one of claims 1 to 8, characterised in that the aqueous emulsion has the following concentrations upon application onto the fibers of the mineral wool:approx. 0,1 to 0,5 % (wt.) of polymerapprox. 0,05 to 0,45 % (wt.) of t-butanol.
- Use of a needling aid according to any one of claims 1 to 9 for producing a needle felt of mineral wool.
- Use according to claim 10, characterised in that the needle felt produced does not liberate any formaldehyde upon being heated to approx. 500 °C.
- Use according to claim 10 or 11, characterised in that a needling aid according to any one of claims 1 to 9 is added to a felt mat, and the latter is then needle punched.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SI9730567T SI0819788T1 (en) | 1996-07-15 | 1997-07-14 | Needling aid for producing needle felts, a needle felt produced by using it, and a method for production thereof |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19628477A DE19628477C1 (en) | 1996-07-15 | 1996-07-15 | Needle aids and their use for the production of needle felts and needle felts produced with them |
| DE19628477 | 1996-07-15 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0819788A2 EP0819788A2 (en) | 1998-01-21 |
| EP0819788A3 EP0819788A3 (en) | 2000-02-02 |
| EP0819788B1 true EP0819788B1 (en) | 2003-05-07 |
Family
ID=7799867
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP97111983A Expired - Lifetime EP0819788B1 (en) | 1996-07-15 | 1997-07-14 | Needling aid for producing needle felts, a needle felt produced by using it, and a method for production thereof |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP0819788B1 (en) |
| DE (2) | DE19628477C1 (en) |
| ES (1) | ES2197268T3 (en) |
| SI (1) | SI0819788T1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102016202401A1 (en) | 2016-02-17 | 2017-08-17 | Saint-Gobain Isover G+H Ag | Needle aid for the production of needle felt made of mineral wool and needle felt made therewith |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2801243B1 (en) | 1999-11-18 | 2006-06-02 | Saint Gobain Isover | METHOD FOR APPLYING AN INSULATING LAYER ON A SURFACE OF AN OBJECT AND CORRESPONDING ISO PRODUCT |
| ITVE20130008A1 (en) | 2013-03-18 | 2014-09-19 | Eurofibre Spa | WATER DISPERSION USED AS A GUIDING AID TO PRODUCE FELTS IN MINERAL FIBERS.- |
| ITUA20164647A1 (en) * | 2016-06-24 | 2017-12-24 | Eurofibre Spa | ANGLING ASSIST TO BE USED IN THE PRODUCTION OF FERTILIZED FELT IN MINERAL WOOL AND A METHOD FOR REALIZING FELT AGUGLIATI |
| FR3054636B1 (en) | 2016-08-01 | 2019-01-25 | Saint-Gobain Isover | INSULATION METHOD AND APPARATUS OBTAINED |
| GB201615896D0 (en) * | 2016-09-19 | 2016-11-02 | Knauf Insulation Doo Skofja Loka | Mineral wool insulation |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3913191A (en) * | 1972-01-28 | 1975-10-21 | Fiberwoven Corp | Fluid aid for needling |
| US4654235A (en) * | 1984-04-13 | 1987-03-31 | Chemical Fabrics Corporation | Novel wear resistant fluoropolymer-containing flexible composites and method for preparation thereof |
| DE3835007A1 (en) * | 1988-10-13 | 1990-04-19 | Gruenzweig & Hartmann | METHOD FOR PRODUCING NEEDLE FELT FROM STONE WOOL |
| CA2129380A1 (en) * | 1993-08-11 | 1995-02-12 | Kenichi Sanechika | Lubricant oil composition comprising a fluorine-containing aromatic compound and an alkyl- or alkyl derivative-substituted aromatic compound, and a refrigerant composition containing the same |
-
1996
- 1996-07-15 DE DE19628477A patent/DE19628477C1/en not_active Expired - Lifetime
-
1997
- 1997-07-14 EP EP97111983A patent/EP0819788B1/en not_active Expired - Lifetime
- 1997-07-14 SI SI9730567T patent/SI0819788T1/en unknown
- 1997-07-14 DE DE69721649T patent/DE69721649T2/en not_active Expired - Fee Related
- 1997-07-14 ES ES97111983T patent/ES2197268T3/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102016202401A1 (en) | 2016-02-17 | 2017-08-17 | Saint-Gobain Isover G+H Ag | Needle aid for the production of needle felt made of mineral wool and needle felt made therewith |
| EP3208246A1 (en) | 2016-02-17 | 2017-08-23 | Saint-Gobain Isover | Needling additive for the manufacture of needle felts of mineral wool and needle felt manufactured therewith |
Also Published As
| Publication number | Publication date |
|---|---|
| DE19628477C1 (en) | 1998-01-22 |
| ES2197268T3 (en) | 2004-01-01 |
| DE69721649T2 (en) | 2003-11-27 |
| EP0819788A2 (en) | 1998-01-21 |
| SI0819788T1 (en) | 2003-10-31 |
| EP0819788A3 (en) | 2000-02-02 |
| DE69721649D1 (en) | 2003-06-12 |
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