EP0675948B1 - Perfectionnements apportes a un procede de fabrication de pains de savon - Google Patents

Perfectionnements apportes a un procede de fabrication de pains de savon Download PDF

Info

Publication number
EP0675948B1
EP0675948B1 EP94903791A EP94903791A EP0675948B1 EP 0675948 B1 EP0675948 B1 EP 0675948B1 EP 94903791 A EP94903791 A EP 94903791A EP 94903791 A EP94903791 A EP 94903791A EP 0675948 B1 EP0675948 B1 EP 0675948B1
Authority
EP
European Patent Office
Prior art keywords
barrel
screw
screws
feedstock
extruder
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
EP94903791A
Other languages
German (de)
English (en)
Other versions
EP0675948A1 (fr
Inventor
Dhanraj Kalyansundaram Chokappa
Vijay Mukund Nandadeep Cooperative Naik
Jojo Philip
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP0675948A1 publication Critical patent/EP0675948A1/fr
Application granted granted Critical
Publication of EP0675948B1 publication Critical patent/EP0675948B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00Making of soap or soap solutions in general; Apparatus therefor
    • C11D13/14Shaping
    • C11D13/18Shaping by extrusion or pressing

Definitions

  • the present invention relates to improvements relating to a process for the manufacture of soap forms.
  • the invention is particularly concerned with a process which uses an improved so-called soap 'plodder'. While the invention is described with particular reference to the manufacture of soap bars it should be understood that the term 'soap' extends to materials comprising non-soap surfactants, including synthetic surfactants and the term 'forms' extends to other three-dimensional solid forms including soap bars, billets, tablets and so-called noodles.
  • the starting material for the production of a soap bar or billet is a mixture containing surfactants, other functional ingredients and water at appropriate proportions. Depending upon the composition of this mixture, its rheological and processing characteristics vary a great deal.
  • processing/finishing of such a mixture involves various process steps such as homogenisation, shear working, and forming into a required shape.
  • One of the devices very commonly employed to carry out one or more of the above operations is a plodder.
  • the function of a simple plodder is to form the mixture into bars or billets of required cross-sections which may subsequently be cut into smaller bars or stamped into tablets of required shape by suitable other means.
  • the function of a refiner plodder is to clean the mixture free of gritty particles or impurities and additionally homogenise/shear work the same to achieve the required degree of homogeneity or phase structure.
  • the plodders may also be used to convert loose aggregates/chips/flakes into noodles for intermediate storage or for feeding subsequent process operations.
  • the heart of a plodder is a screw extruder.
  • the simplest plodder has an extruder with a single worm.
  • the feed stock either in homogenised and worked form or in the form of noodles or crimpled chips, fed through the hopper enters the extruder barrel and fills the annular space between the extruder worm (screw) and the barrel.
  • the barrel is stationary and the worm rotates inside the barrel. Frictional/viscous drag forces act on the material, both at the barrel as well as at the worm surfaces.
  • the resultant force is responsible for the forward transportation of the processed mass towards the discharge end.
  • the extruder may have a perforated plate, through which the processed mass is forced. This is generally known in the art as a 'noodle plate'.
  • the processed mass emerges in the form of rods/ribbons/sheets from the perforated plate.
  • the objective is to enhance homogenisation or shear working or to filter out gritty particles, then it is advantageous to fit a wire gauze in front of the perforated plate but it tends to reduce throughput.
  • a cone and die/eye plate are provided at the discharge end of the extruder along with or without the noodle plate. The extruder forces the mixed mass through these end fittings to product the noodles, billets or bars. Designs of perforated plates, cones and die/eye plates vary considerably from application to application. It should be noted that the throughput rate is very sensitive to the resistance offered by wire mesh screens, perforated plates, cones and dies.
  • Machines called duplex or twin worm plodders have two worms (or screws) which are parallel, non-intermeshing and mounted tangentially with respect to each other within a barrel.
  • the worms may be co-rotating but usually they are counter-rotating.
  • Intermeshed and co-rotating twin screw extruders are also known for processing of soap/detergent mass.
  • drag forces similar to those encountered in single worm plodders act on the processed mass and push the same in the forward direction.
  • Screw extrusion is apparently a simple operation, but the results in terms of quality of product, throughput rate, specific energy consumption, etc. can be influenced by a number of factors in a rather complex way.
  • plodding is affected by soap factors and by machine factors. It is important to balance the various factors so as to achieve the best results.
  • the functions of the screw extruder in the soap making process include mixing, working and conveying materials.
  • Other apparatus exists for the performance of some or all of these process operations.
  • mixing can be performed in z or Sigma-blade mixers: products can be worked by chilled rolls and transported using conveyors.
  • these apparatus also have their disadvantages e.g. mixers generally only operate in batch mode, chilled rolls are expensive to manufacture and maintain and sticky products are difficult to transport on conveyors.
  • Twin screw extruders have previously been described for use in working up dry powdered or farinaceous substances to foods in digestible forms and for producing high-temperature resistant, ample heat-conductive, electrically insulating plastics in European Patent Specifications 41 641 and 199 340 respectively.
  • the present invention provides a process for the manufacture of soap forms which includes the step of treating a soap feedstock by passage through a twin screw, intermeshing, counter-rotating extruder.
  • the extruder comprises two oppositely-threaded, closely intermeshing screws mounted for rotation within a barrel having a first end and a second end, said screws having a minimal screw-to-screw and screw to barrel clearance such that as the feedstock passes along at least a part of the barrel from said first end and towards said second end it is divided into a plurality of discrete, substantially C-shaped segments bounded by the screw and barrel surfaces and conveyed in a path whereby the bulk of the feedstock move substantially parallel to the rotational axis of the screws.
  • volumetric efficiencies of above 60% can be attained using the present invention whereas in single screw plodders according to the prior art the volumetric efficiency was typically 9-19%.
  • the screws should be a matching pair, i.e. that they should have the same diameters and be substantially different only as regards the handedness of the screw.
  • the screws are preferably detachable from the extruder whereby whenever necessary the screws can be changed with another pair of screws having different screw layout.
  • the screw may be either continuous or segmented.
  • the segmented screws have removable sections which can have varying pitches so that they can be manipulated depending upon the composition of the material being processed.
  • the screws may be single-start or multi-start.
  • processes according to embodiments of the present invention will further comprise means for rotating the screws in mutually opposite directions.
  • the positive pumping characteristic of extruders used in the process according to the present invention can be used either to increase the throughput of the extruder at a given rotational speed or to reduce the rotational speed required for a given throughput. Reduction in screw speed is particularly advantageous as it reduces the extent to which the product is heated during treatment, and enables the power input to be reduced.
  • processes according to embodiments of the present invention will further comprise means for supplying the feedstock to the barrel of the extruder at the first end of the barrel.
  • said means for supplying the feedstock comprise hopper means located above one end of the screws.
  • processes according to embodiments of the present invention will further comprise means for forming the feedstock into soap forms at the second end of the barrel.
  • Such means are well-known in the art.
  • the forms can comprise noodles, bars and/or billets.
  • the precise nature of the means for forming the feedstock will depend on the nature of the forms desired. Where noodles are desired said means comprise a perforated plate through which the feedstock is extruded. Where bars or billets are desired a conventional cone and eyeplate can be employed.
  • the pitch angle of the screws decreases in the direction of flow.
  • the pitch angle is 20-30 degrees adjacent the first end of the barrel and 10-20 degrees adjacent the second end of the barrel. This is particularly useful where feedstock is being compacted and its overall density is increasing during progress down the screw from the first to the second end of the barrel.
  • the width of the flights increases in the direction of flow relative to the width of the channel between the flights.
  • the width of the channel is at least three times the flight width adjacent the first end of the barrel and less than three times the flight width adjacent the second end of the barrel. This is particularly useful where feedstock is being compacted and its overall density is increasing during progress down the screw from the first to the second end of the barrel.
  • cooling means are provided to cool the feedstock within the barrel.
  • the cooling means can include means for circulating a cooling fluid through a cooling jacket around the barrel and/or through passages within one or both of the screws. While cooling means are generally employed in single screw extruders, the cooling means are optional in the present invention.
  • some degree of cooling can be employed if it is desirable to cool the process stream during its passage through the extruder, thus enabling the apparatus used in the process according to the invention to replace the chilled rolls used in conventional plant.
  • the efficiency of cooling can be improved by cooling the screws in addition to the barrel.
  • cooling means whether to assist in pumping or remove heat generated by shear adds a considerable capital cost and increases operating costs per ton of capacity whereas in the present invention the capacity of the cooling means to remove heat from the feedstock need not be as great. In practice, this enables a higher temperature coolant to be used, e.g. cooled water rather than chilled water. Moreover, the relatively low temperatures which can be attained in the product emerging from the apparatus according to the present invention greatly facilitate subsequent handling and processing of the product.
  • the cooling means in embodiments of the present invention can include means for circulating a cooling fluid through a cooling jacket around the barrel and through passages within one or both of the screws and this can significantly improve the heat transfer rate, by increasing the heat transfer area.
  • the process according to the present invention can be applied to a wide range of feedstocks and use is not limited to those feedstocks which comprise synthetic, non-soap surfactants.
  • the invention can be applied to the processing of transparent and/or translucent soap formulations which are known to be of high viscosity and difficult or expensive to process, or to soap forms comprising structuring and/or hardening aids. It is envisaged that all manner of aerated/solid and/or toilet/laundry soaps can be manufactured by a process according to the present invention.
  • the apparatus used in the process according to the present invention need not be manufactured to the same high engineering tolerances required in the manufacture of conventional counter-rotating extruders thereby further reducing set-up and manufacturing costs.
  • a particular advantage as regards manufacturing is that the screws can be at least in part cast rather than machined from a blank.
  • the extruder comprises two closely intermeshed screws 1 and 2 mounted within a jacketed barrel 3 and driven by a motor 4.
  • the two screws are oppositely threaded and closely intermeshed with each other. When one screw rotates clockwise, the other screw rotates anticlockwise.
  • the screws shown are single-start screws, but they may even be multi-start ones.
  • a cross section of a typical screw is shown in figure 3.
  • a hopper 5 is typically provided, through which the soap/detergent material enters the extruder.
  • a perforated plate (not shown), a cone jacket (not shown) and an eye plate (not shown).
  • eyeplate, jacket and plate would be mounted on the flange at the output end of the extruder as shown in figure 1.
  • FIG 6b An apparatus used in a less preferred embodiment of the invention, with partially intermeshing screws, is shown in figure 6b, whereas figure 6a shows the more preferable arrangement having closely intermeshed screws. It should be noted that the screws of figure 6 do not have the particular features of the embodiment shown in figure 4 but rather represent the two extremes of the variation in flight width which occurs in figure 4.
  • extruders described above all have single-stage extruder mechanism, it will be appreciated that the invention may equally be carried out using two- or other multi- stage extruders and in particular those which correspond to multi-stage vacuum plodders or refiners.
  • a particular advantage of those embodiments of the present invention in which closely intermeshing screws are used is that the soap/detergent material to a considerable extent is prevented from rotating with the screws. This ensures that the bulk of the material moves substantially parallel to the extruder axis and thereby avoids any rheological or structural damages or rise in temperature in the material and results in soap/detergent mass with better downstream processing qualities.
  • Such a process delivers a higher throughput at a giver rpm, i.e. a better volumetric efficiency and a lower specific energy consumption in comparison to plodding methods hitherto being used in the soap/detergent industry.
  • Fig.5 shows a comparison of actual and theoretical volumetric efficiency through an apparatus used in a process embodying the present invention for a range of soap blends.
  • results are given for a formulation based on sodium cocoyl isethionate and containing relatively low levels of soap, a formulation based on a mixture of sodium cocoyl isethionate and soap, and a formulation based on an acyl isethionate, sulphosuccinate, betaine surfactant system.
  • These differences in formulation are not distinguished between, but are in part responsible for the spread of results.
  • Triangles are results obtained with closely intermeshing shafts similar to those shown in figure 6a.
  • Crosses are results obtained with partially intermeshing shafts similar to those shown in figure 6b.
  • Squares are results obtained with a conventional single screw extruder having the same screw size as the double screw apparatus.
  • volumetric efficiency of the apparatus employing closely intermeshed shafts is generally above 50%, whereas with partially intermeshing shafts the volumetric efficiency falls to 25-50% of the theoretical maximum. It should be noted that 25-50% volumetric efficiency still exhibits a general improvement over the results obtained in the conventional single screw plodder.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

Procédé de fabrication de pains de savon, consistant à soumettre du savon brut à un traitement par passage dans une extrudeuse à deux vis engrenées contrarotatives, et appareil de fabrication de pains de savon selon le procédé. Ledit appareil comporte une extrudeuse à deux vis engrenées contrarotatives. Cette extrudeuse comporte deux vis engrenées de manière serrée, filetées dans des sens contraires, et montées rotatives dans un logement présentant des première et seconde extrémités. Le jeu entre les vis et entre celles-ci et le logement est minimisé de sorte qu'en avançant de la première extrémité vers la seconde extrémité en longeant au moins une partie du logement, le savon brut soit divisé en une pluralité de segments distincts sensiblement en forme de C délimités par les faces des vis et du logement, et qu'il avance en suivant une trajectoire sensiblement parallèle à l'axe de rotation des vis.

Claims (9)

  1. Un procédé pour la fabrication de formes de savon qui comprend l'étape consistant à traiter une matière de charge de savon par passage dans une extrudeuse à deux vis qui s'engrènent, dont les vis tournent en sens inverse.
  2. Procédé selon la Revendication 1, dans lequel l'extrudeuse comprend deux vis qui s'engrènent fortement et présentent 2 filetages symétriques, montées pour tourner à l'intérieur d'un tambour présentant une première extrémité et une seconde extrémité, lesdites vis présentant un écartement "vis à vis" et un écartement "vis à tambour" minimum de sorte que, lorsque la matière de charge passe le long d'au moins une partie du tambour depuis ladite première extrémité et vers ladite seconde extrémité, elle est divisée en une pluralité de segments discrets substantiellement en forme de C, contenus par les surfaces de la vis et du tambour et transportés dans une voie selon laquelle le volume de la matière de charge se déplace substantiellement parallèlement à l'axe de rotation des vis.
  3. Procédé selon la Revendication 2, dans lequel la matière de charge alimente le tambour de l'extrudeuse au niveau de la première extrémité du tambour en utilisant un moyen d'introduction.
  4. Procédé selon la Revendication 2, dans lequel la matière de charge est formée en forme de savons au niveau de la seconde extrémité du tambour.
  5. Procédé selon la Revendication 2, dans lequel, dans l'extrudeuse, l'angle de pas de chaque vis est compris entre 20 et 30 degrés prés de la première extrémité du tambour et entre 10 et 20 degrés près de la seconde extrémité du tambour.
  6. Procédé selon la Revendication 2, dans lequel, dans l'extrudeuse, la largeur du canal de chaque vis est au moins trois fois égale à la largeur du pas de vis adjacente à la première extrémité du tambour et trois fois inférieure à la largeur du pas de la vis adjacente avec la seconde extrémité du tambour.
  7. Procédé selon la Revendication 2, dans lequel la matière de charge est refroidie à l'intérieur du tambour en utilisant un moyen de refroidissement.
  8. Procédé selon la Revendication 7, dans lequel le moyen de refroidissement comprend un moyen destiné à faire circuler un fluide réfrigérant à travers une chemise de refroidissement autour du tambour.
  9. Procédé selon la Revendication 8, dans lequel le moyen de refroidissement comprend un moyen destiné à faire circuler un fluide réfrigérant via des passages pratiqués à l'intérieur d'une ou de deux des vis.
EP94903791A 1992-12-17 1993-12-13 Perfectionnements apportes a un procede de fabrication de pains de savon Expired - Lifetime EP0675948B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB929226309A GB9226309D0 (en) 1992-12-17 1992-12-17 Improved method of manufacture
GB9226309 1992-12-17
PCT/EP1993/003561 WO1994013778A1 (fr) 1992-12-17 1993-12-13 Perfectionnements apportes a un procede de fabrication de pains de savon et appareil associe

Publications (2)

Publication Number Publication Date
EP0675948A1 EP0675948A1 (fr) 1995-10-11
EP0675948B1 true EP0675948B1 (fr) 1996-07-03

Family

ID=10726757

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94903791A Expired - Lifetime EP0675948B1 (fr) 1992-12-17 1993-12-13 Perfectionnements apportes a un procede de fabrication de pains de savon

Country Status (7)

Country Link
EP (1) EP0675948B1 (fr)
AU (1) AU5811894A (fr)
BR (1) BR9307677A (fr)
DE (1) DE69303495T2 (fr)
ES (1) ES2089914T3 (fr)
GB (1) GB9226309D0 (fr)
WO (1) WO1994013778A1 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9402837D0 (en) * 1994-02-15 1994-04-06 Unilever Plc Extruder
GB9524576D0 (en) * 1995-12-01 1996-01-31 Unilever Plc Pressure plate
MY115749A (en) 1997-05-16 2003-08-30 Unilever Plc Process for the production of a detergent composition
ID24359A (id) 1997-05-16 2000-07-13 Unilever Nv Proses untuk memproduksi suatu komposisi detergen
US8871807B2 (en) 2008-03-28 2014-10-28 Ecolab Usa Inc. Detergents capable of cleaning, bleaching, sanitizing and/or disinfecting textiles including sulfoperoxycarboxylic acids

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1030555B (de) * 1953-04-10 1958-05-22 Hermann Berstorff Maschb Ansta Schneckenpresse zur Verarbeitung von organischen plastischen Massen
NL123670C (fr) * 1961-02-28 1900-01-01
DE2049268B2 (de) * 1970-10-07 1978-08-24 Blendax-Werke R. Schneider Gmbh & Co, 6500 Mainz Verfahren zur kontinuierlichen Herstellung zweifarbiger Reinigungsmittelstücke, insbesondere Seifen
JPS5245606A (en) * 1975-10-09 1977-04-11 Ideal Setsuken Kk Apparatus for extruding stick of solid soap having stripe patterns

Also Published As

Publication number Publication date
WO1994013778A1 (fr) 1994-06-23
BR9307677A (pt) 1999-06-15
ES2089914T3 (es) 1996-10-01
EP0675948A1 (fr) 1995-10-11
AU5811894A (en) 1994-07-04
DE69303495T2 (de) 1996-11-28
GB9226309D0 (en) 1993-02-10
DE69303495D1 (de) 1996-08-08

Similar Documents

Publication Publication Date Title
US2048286A (en) Apparatus for treating plastic materials
AU2003242655B2 (en) Method and device for liquefying of a powdery fat based product particularly in the production of chocolate and the like
EP0574172B1 (fr) Machine à mélanger du type "Transfermix"
US2494891A (en) Process and apparatus for making floating soap
US3434974A (en) Continuous manufacture of detergent laundry bars
PL175217B1 (pl) Podgrzewarko-wytłaczarka do termicznego przetwarzania biopolimerów i sposób termicznego przetwarzania biopolimerów
EP0675948B1 (fr) Perfectionnements apportes a un procede de fabrication de pains de savon
US3764114A (en) Process for continuously producing soap and device for carrying out the process
US5534212A (en) Process for the manufacture of soap bars and apparatus for use in same process
JPS61260829A (ja) パン製造とパン菓子製造用練り粉を混練するためおよび食品成分と飼料成分を低温分解および均質化するための装置
US20220204893A1 (en) Apparatus, process, and extrusion screw for producing syndet soaps
PL200535B1 (pl) Urządzenie do wytwarzania ciągłego kazeinianu
US3741702A (en) Apparatus for pressure rolling soaps and similar products
US2525081A (en) Process for making floating soap
Spitz Bar soap finishing
EP0090650B1 (fr) Procédé de fabrication de détergent
JPH07133500A (ja) 高粘度物の処理装置および石鹸の製造方法
JPS60176556A (ja) パン粉の製造装置
CN212488398U (zh) 一种饲料膨化机的挤出机构
CN109366788B (zh) 一种天然橡胶初加工湿搅挤洗一体机
JPH01165699A (ja) 固型石鹸の製造法
Hwang et al. Experimental development of processing technology for yuba-like films using twin screw extrusion
JPH08295900A (ja) 石鹸の製造方法

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

17P Request for examination filed

Effective date: 19950526

AK Designated contracting states

Kind code of ref document: A1

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

17Q First examination report despatched

Effective date: 19951016

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): CH DE ES FR GB IT LI NL SE

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 FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 19960703

Ref country code: LI

Effective date: 19960703

Ref country code: CH

Effective date: 19960703

REF Corresponds to:

Ref document number: 69303495

Country of ref document: DE

Date of ref document: 19960808

ITF It: translation for a ep patent filed

Owner name: JACOBACCI & PERANI S.P.A.

ET Fr: translation filed
REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2089914

Country of ref document: ES

Kind code of ref document: T3

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

Ref country code: SE

Effective date: 19961003

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2089914

Country of ref document: ES

Kind code of ref document: T3

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

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
REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

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

Ref country code: FR

Payment date: 20051216

Year of fee payment: 13

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

Ref country code: GB

Payment date: 20061222

Year of fee payment: 14

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

Ref country code: ES

Payment date: 20061226

Year of fee payment: 14

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

Ref country code: IT

Payment date: 20061231

Year of fee payment: 14

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

Ref country code: DE

Payment date: 20070131

Year of fee payment: 14

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20070831

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: 20070102

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

Effective date: 20071213

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: 20080701

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: 20071213

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20071214

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

Ref country code: ES

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

Effective date: 20071214

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: 20071213