EP0675215B1 - A process for preparing a thermal bondable fiber - Google Patents

A process for preparing a thermal bondable fiber Download PDF

Info

Publication number
EP0675215B1
EP0675215B1 EP95104015A EP95104015A EP0675215B1 EP 0675215 B1 EP0675215 B1 EP 0675215B1 EP 95104015 A EP95104015 A EP 95104015A EP 95104015 A EP95104015 A EP 95104015A EP 0675215 B1 EP0675215 B1 EP 0675215B1
Authority
EP
European Patent Office
Prior art keywords
fibers
molten polymer
fiber
spinneret
filament
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
Application number
EP95104015A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0675215A1 (en
Inventor
Eric J. Evain
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Basell North America Inc
Original Assignee
Montell North America Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US08/331,319 external-priority patent/US5507997A/en
Application filed by Montell North America Inc filed Critical Montell North America Inc
Publication of EP0675215A1 publication Critical patent/EP0675215A1/en
Application granted granted Critical
Publication of EP0675215B1 publication Critical patent/EP0675215B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • D01F6/06—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins from polypropylene
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected

Definitions

  • This invention relates to a process of preparing fibers, in particular, an improved process of preparing thermal bondable fibers of fiber grade material.
  • Fibers of certain thermoplastic materials are used widely in the manufacturing of thermally bonded products, such as nonwoven textiles, by various processes. Said processes, such as calendering and spun bonding, require that the fibers have the capability of thermally bonding at temperatures lower than the melting point of the particular polymer(s) from which they are made, and that the fibers and articles manufactured therefrom be resistant to aging, yellowing and color variations caused by gas fading and oxidation.
  • Another approach is to add to the fiber grade polymer a low melting material, such as oligomers and waxes.
  • a low melting material such as oligomers and waxes.
  • the disadvantage of this approach is that the process must be modified to ensure adequate mixing of the materials so that gels are not formed in the fiber.
  • one component of the fiber has a lower melting point than the other, and covers the surface of the other component which has a higher melting point.
  • These fibers are generally referred to as a "sheath-core" or “side-by-side” bicomponent fibers.
  • the lower melting component enables thermal bonding at a temperature below the melting point of the fiber core.
  • fibers typically contain only one fiber grade polymer, such as "skin fiber". Modification of the fiber surface can be obtained using various methods, such as irradiation, plasma treatment, ozone treatment, corona discharge treatment or chemical treatment.
  • the polymer is heated in an extruder to the melting point and the molten polymer is pumped at a constant rate under pressure through a spinneret containing one or more orifices of desired diameter, thereby producing filaments of the molten polymer.
  • the molten polymer filaments are fed downward from the face of the spinneret into a cooling stream of gas, generally air.
  • the filaments of molten polymer are solidified as a result of cooling to form fibers.
  • the fibers are spread to form a fiber web and bonded directly, like in the spun bond method.
  • the fibers are gathered together and, if desired, drawn to orient the macromolecular structure of the fibers, and are then wound on bobbins. Bonding or calendering is then performed in a separate step.
  • the modification of the filaments or fibers takes place after the molten polymer filaments have solidified as a result of cooling to form the fiber, or on the preformed fiber itself.
  • the thermal bondability of fibers can be enhanced by treating the fiber grade polymer during the formation of the filaments, instead of treating the filaments or fibers after they are formed.
  • the process of the present invention is not limited to any specific fiber preparation technique where a resin is melted and formed into a fiber, such as long spin, short spin, spun bond and melt blown fiber production methods.
  • the spinning process limited to being carried out in any particular spinning environment, e.g. the presence or absence of oxygen or nitrogen.
  • Applicant has found that fibers having improved thermal bondability can be produced at lower spinning temperatures and increased spinning speeds by irradiating the molten fiber grade polymer filaments as soon as the filaments exit the orifices of the spinneret with electromagnetic radiation.
  • the present invention provides an improved process for the production of thermal bondable fibers comprising exposing the molten polymer filaments to from 1 x 10 -2 to 50 W/cm 2 of electromagnetic energy at the spinneret face.
  • Figure 1 is a schematic representation of a melt spinning arrangement used in the process of the present invention.
  • spinneret face is intended to include the upper portion of the spin line and the exit point of the molten material from one or more orifices, having any desired diameter, of the spinneret.
  • fiber grade polymer means any polymer that is capable of being spun into filaments to produce a fiber.
  • the fiber grade polymer is charged into a hopper 1 , and fed into an extruder 2 of known or conventional type, containing single or multiple screws and equipped with controls for regulating the temperature of the barrel in various zones along the length of the barrel, where the polymer is heated to its melting point.
  • the molten polymer is then fed to a metering pump 3 , which delivers the molten polymer at a constant rate to a heated spinneret 4 containing one or more orifices.
  • the fluid molten polymer filaments emerging in a downward direction from the face of the spinneret are exposed to electromagnetic radiation from a radiation source 5 .
  • the radiation source is positioned whereby the source encompasses the spinneret face.
  • the molten polymer filaments are then solidified by cooling to form fibers 6 .
  • the filaments produced by the process of this invention are typically combined into one or more fibers of varying thickness. Fibers made up of one filament are generally referred to as monofilament fibers and fibers made up of more than one filament are generally referred to as multifilament fibers.
  • the spun denier of the fibers produced accordinq to the method of this invention range from less than 1.1 dtex to at least 55.6 dtex (1 to at least 50 dpf, denier) per filament. (Denier is the weight in grams of 9000 meters of fiber).
  • the fiber forming polymers useful in the present invention can be any polymer typically used to prepare fibers.
  • the fiber grade polymer is polyethylene, polypropylene, random copolymer of propylene and ethylene, polyisobutylene, polyamide, polyester, polystyrene, polyvinyl chloride, polyacrylate and mixtures thereof.
  • Most preferred is polypropylene and random copolymers of propylene and ethylene.
  • the electromagnetic radiation can be ultraviolet, visible or infrared radiation.
  • the total amount of electromagnetic energy that reaches the filament(s), referred to as irradiance, can be adjusted by changing the distance between the source of the radiation and the filament(s), changing the wavelength emitted by the source, and by changing the power, intensity, of the source.
  • the total amount of electromagnetic energy that reaches the filament(s) is from 1 x 10 -2 to 50 M/cm 2 and from 1 x 10 -1 to 10 W/cm 2.
  • additives may be blended with the fiber forming polymer used to produce the thermal bondable fibers of the present invention.
  • additives include, stabilizers, antioxidants, antislip agents, antistatic agents, flame retardants, nucleating agents, pigments, antisoiling agents, photosensitizers and the like.
  • the molten polymer is fed to the meter pump, and pumped at a constant rate under pressure to a spinneret, containing one orifice with a diameter of 0.05cm (0.020 inches).
  • the molten polymer filament emerging downward from the orifice of the spinneret is exposed to 0.88 W/cm 2 ultraviolet radiation.
  • the filament of molten polymer is solidified as a result of cooling to form a monofilament fiber, and is collected on the godet.
  • the processing conditions are as follows: Extruder Feed Zone Temp. 220°C Metering Pump Temp. 300°C Spinneret Temp. 300°C Fiber Spun Denier 2.2 dtex (2 g/9000 m) Godet Take-up Speed 1000 m/min
  • the monofilament fibers prepared above were then tested for bond strength according to the following procedure.
  • the fibers were cut into 400 mm lengths.
  • the samples weighed between 0.160 and 0.170 grams.
  • the fibers were then mechanically twisted eighty times and folded in half.
  • the bundle was hand twisted six times and allowed to wrap around itself.
  • the sample was bonded in a Sentinel Model 1212 heat sealer at 2.812 kg/cm 2 (40 psi) for 1.50 seconds at the desired temperature.
  • the force required to separate the bonded segments was recorded on an Instron Model 114 universal testing machine.
  • Fibers were prepared according to the procedure of Example 1 using the same ingredients and processing conditions, except that the molten polymer filament emerging downward from the face of the spinneret was not exposed to the ultraviolet radiation.
  • the bonding strength of the fibers of the present invention is substantially higher than the bonding strength of the fibers of the Comparative Example 1 at the same bonding temperature.
  • Irgafos 168 tris(2,4-di-tert-butylphenyl)phosphite stabilizer and 1000 ppm wt.
  • calcium stearate are prepared by according to the process of Example 1, except the processing conditions were as follows: Extruder Feed Zone Temp. 220°C Metering Pump Temp. 275°C Spinneret Temp. 275°C Fiber Spun Denier 9.9 dtex (9 g/9000 m) Godet Take-up Speed 1000 m/min Ultraviolet radiation 2.8 W/cm 2
  • Fibers were prepared according to the procedure of Example 2 using the same ingredients and processing conditions, except that the molten polymer filament emerging downward from the face of the spinneret was not exposed to the ultraviolet radiation.
  • the fibers of the present invention demonstrate better bonding strength as compared to the fibers of Comparative Example 2.
  • Irgafos 168 tris-(2,4-di-tert-butylphenyl)phosphite stabilizer and 1000 ppm wt.
  • calcium stearate were prepared by according to the process of Example 1, except the processing conditions were as follows: Extruder Feed Zone Temp. 220°C Metering Pump Temp. 300°C Spinneret Temp. 300°C Fiber Spun Denier 2.2 dtex (2 g/9000 m) Godet Take-up Speed 4000 m/min Ultraviolet radiation 0.88 W/cm 2
  • Fibers were prepared according to the procedure of Example 4 using the same ingredients and processing conditions, except that the molten polymer filament emerging downward from the face of the spinneret was not exposed to the ultraviolet radiation.
  • the fibers of the present invention demonstrate better bonding strength as compared to the fibers of Comparative Example 3.
  • Fibers were prepared according to the procedure of Example 4 using the same ingredients and processing conditions, except that the molten polymer filament emerging downward from the face of the spinneret was not exposed to the ultraviolet radiation.
  • the fibers of the present invention demonstrate better bonding strength as compared to the fibers of Comparative Example 4.
  • the thermal bondable fibers prepared according to the process of the present invention can be used in the manufacturing of nonwovens, by spun bonded and melt blown processes.
  • Nonwovens are useful in the production of personal hygiene products, for example, infant care and adult incontinence products, protective covering, for example surgical gowns and shoe covers and other disposable medical and clothing products.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Inorganic Fibers (AREA)
  • Multicomponent Fibers (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Nonwoven Fabrics (AREA)
  • Adhesives Or Adhesive Processes (AREA)
EP95104015A 1994-03-31 1995-03-18 A process for preparing a thermal bondable fiber Expired - Lifetime EP0675215B1 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US22130594A 1994-03-31 1994-03-31
US221305 1994-03-31
US08/331,319 US5507997A (en) 1994-03-31 1994-10-28 Process for preparing a thermal bondable fiber
US331319 1994-10-28

Publications (2)

Publication Number Publication Date
EP0675215A1 EP0675215A1 (en) 1995-10-04
EP0675215B1 true EP0675215B1 (en) 1998-09-30

Family

ID=26915667

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95104015A Expired - Lifetime EP0675215B1 (en) 1994-03-31 1995-03-18 A process for preparing a thermal bondable fiber

Country Status (15)

Country Link
EP (1) EP0675215B1 (zh)
JP (1) JP3693374B2 (zh)
CN (1) CN1058063C (zh)
AT (1) ATE171733T1 (zh)
AU (1) AU691569B2 (zh)
BR (1) BR9501291A (zh)
CA (1) CA2144934A1 (zh)
DE (1) DE69505033T2 (zh)
EG (1) EG20572A (zh)
ES (1) ES2124927T3 (zh)
FI (1) FI951556A (zh)
NO (1) NO306911B1 (zh)
PH (1) PH31402A (zh)
RU (1) RU2139189C1 (zh)
TR (1) TR28851A (zh)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6787066B2 (en) 2001-11-16 2004-09-07 Sunoco Inc (R&M) Stabilization system for improving the melt viscosity of polypropylene during fiber processing
SI2230350T1 (sl) * 2009-03-18 2011-07-29 Baumhueter Extrusion Gmbh Polimerno vlakno, njegova uporaba in postopek za njegovo izdelavo
CN106835375A (zh) * 2017-03-26 2017-06-13 响水县永泰纺织制衣有限公司 一种用于熔融纺织和冷却多根合成长丝装置
EP3608742B1 (en) 2018-08-07 2021-10-06 ABB Schweiz AG Apparatus for alarm information determination

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54138076A (en) * 1978-04-19 1979-10-26 Toray Ind Inc Surface modification of plastic molded article
EP0013538B1 (de) * 1979-01-03 1983-04-06 Manahl, Robert, Dipl.-Ing. Einrichtung zur Gewinnung von Methangas aus organischen Abfällen
DE4113524A1 (de) * 1991-04-25 1992-10-29 Abb Patent Gmbh Verfahren zur behandlung von oberflaechen

Also Published As

Publication number Publication date
FI951556A (fi) 1995-10-01
BR9501291A (pt) 1995-10-31
JPH07278944A (ja) 1995-10-24
CN1111294A (zh) 1995-11-08
FI951556A0 (fi) 1995-03-31
ES2124927T3 (es) 1999-02-16
RU95105024A (ru) 1997-01-27
PH31402A (en) 1998-10-29
DE69505033T2 (de) 1999-03-18
EP0675215A1 (en) 1995-10-04
NO306911B1 (no) 2000-01-10
CA2144934A1 (en) 1995-10-01
ATE171733T1 (de) 1998-10-15
CN1058063C (zh) 2000-11-01
AU691569B2 (en) 1998-05-21
NO951227D0 (no) 1995-03-30
RU2139189C1 (ru) 1999-10-10
TR28851A (tr) 1997-07-17
NO951227L (no) 1995-10-02
EG20572A (en) 1999-08-30
DE69505033D1 (de) 1998-11-05
AU1618895A (en) 1995-10-26
JP3693374B2 (ja) 2005-09-07

Similar Documents

Publication Publication Date Title
US5507997A (en) Process for preparing a thermal bondable fiber
KR100387546B1 (ko) 고열강도결합섬유
KR100382441B1 (ko) 용융방사시스템으로제조한고열결합강도의스킨-코아섬유
US4228118A (en) Process for producing high tenacity polyethylene fibers
FI72350B (fi) Polyolefina fibrer med foerbaettrade vaermebindningsegenskaperoch foerfarande foer framstaellning av dessa
US4276348A (en) High tenacity polyethylene fibers and process for producing same
JPH06508892A (ja) ポリエチレン二成分繊維
JPS62191509A (ja) 溶融紡糸組成物用の冷却調節剤としての枝分れポリオレフイン
JPS58191215A (ja) ポリエチレン系熱接着性繊維
AU771652B2 (en) Thermal bondable polyolefin fibers comprising a random copolymer of propylene
EP0298767B1 (en) Highly filled yarns and the production of yarns
EP0675215B1 (en) A process for preparing a thermal bondable fiber
KR20030011806A (ko) 친수성 첨가제
JPH026613A (ja) ポリスチレンを含む伝導性フィラメント，その製造方法，多フィラメント系及びカーペット
EP0140559B1 (en) Improved high speed process for forming fully drawn polyester yarn
US5443898A (en) Nonwoven webs and method of making same
JP4270734B2 (ja) 嵩高性を有する生分解性繊維の製造方法
EP0250664B1 (en) Process for combining and codrawing antistatic filaments with undrawn nylon filaments
JP2021070897A (ja) 超吸水速乾樹脂繊維、不織布及び超吸水速乾樹脂繊維の製造方法
JP2000226746A (ja) へたり性の改善された複合嵩高糸およびその製造方法
JPH0814064B2 (ja) 熱融着不織布
KR20040039671A (ko) 스판본드 부직포 위생재 및 그 제조방법
JPH0571057A (ja) ポリプロピレン系複合短繊維と不織布の製造方法
JPH11315413A (ja) ポリテトラメチレンアジパミドからなる繊維の製造法およびこの種の繊維材料
JPH0122374B2 (zh)

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE ES FR GB IT LI NL SE

17P Request for examination filed

Effective date: 19960217

17Q First examination report despatched

Effective date: 19970219

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH DE ES FR GB IT LI NL SE

REF Corresponds to:

Ref document number: 171733

Country of ref document: AT

Date of ref document: 19981015

Kind code of ref document: T

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: DIPL.-ING. ETH H. R. WERFFELI PATENTANWALT

Ref country code: CH

Ref legal event code: EP

REF Corresponds to:

Ref document number: 69505033

Country of ref document: DE

Date of ref document: 19981105

REG Reference to a national code

Ref country code: CH

Ref legal event code: AEN

Free format text: DAS PATENT IST AUFGRUND DES WEITERBEHANDLUNGSANTRAGS VOM 06.01.1999 REAKTIVIERT WORDEN.

ET Fr: translation filed
REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2124927

Country of ref document: ES

Kind code of ref document: T3

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SE

Payment date: 20010306

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20010313

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CH

Payment date: 20010315

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20010316

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20010330

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 20010516

Year of fee payment: 7

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020318

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020319

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020319

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020331

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020331

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20020331

BERE Be: lapsed

Owner name: *MONTELL NORTH AMERICA INC.

Effective date: 20020331

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20021001

EUG Se: european patent has lapsed

Ref document number: 95104015.3

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 20021001

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20030312

Year of fee payment: 9

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040318

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20030410

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20040318

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20050413

Year of fee payment: 11

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20060317

Year of fee payment: 12

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20060331

Year of fee payment: 12

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20061003

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20071130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070402

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20070318