EP0824251A1 - Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient - Google Patents

Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient Download PDF

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Publication number
EP0824251A1
EP0824251A1 EP96202264A EP96202264A EP0824251A1 EP 0824251 A1 EP0824251 A1 EP 0824251A1 EP 96202264 A EP96202264 A EP 96202264A EP 96202264 A EP96202264 A EP 96202264A EP 0824251 A1 EP0824251 A1 EP 0824251A1
Authority
EP
European Patent Office
Prior art keywords
layer
container
transfer
ink
label
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.)
Withdrawn
Application number
EP96202264A
Other languages
German (de)
English (en)
Inventor
Thomas Lynn Brandt
Neal Donald Turner
Erwin Anton Rosens
Patrick Johannes Blom
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.)
Heineken Technical Services BV
Brandt Technologies Inc
Original Assignee
Heineken Technical Services BV
Brandt Technologies 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
Application filed by Heineken Technical Services BV, Brandt Technologies Inc filed Critical Heineken Technical Services BV
Priority to EP96202264A priority Critical patent/EP0824251A1/fr
Priority to BR9708112-4A priority patent/BR9708112A/pt
Priority to EP97907475A priority patent/EP0888600B1/fr
Priority to AU19466/97A priority patent/AU711502B2/en
Priority to EE9800320A priority patent/EE03785B1/xx
Priority to AT97907475T priority patent/ATE203845T1/de
Priority to DE69705935T priority patent/DE69705935T2/de
Priority to SI9730195T priority patent/SI0888600T1/xx
Priority to SK1281-98A priority patent/SK128198A3/sk
Priority to PL97329029A priority patent/PL185928B1/pl
Priority to ES97907475T priority patent/ES2162254T3/es
Priority to JP53337297A priority patent/JP2000507363A/ja
Priority to EA199800838A priority patent/EA000487B1/ru
Priority to PT97907475T priority patent/PT888600E/pt
Priority to PCT/NL1997/000137 priority patent/WO1997035290A1/fr
Priority to APAP/P/1998/001345A priority patent/AP1037A/en
Priority to TR1998/01852T priority patent/TR199801852T2/xx
Priority to YU40598A priority patent/YU49317B/sh
Priority to NZ331863A priority patent/NZ331863A/en
Priority to KR10-1998-0707432A priority patent/KR100481951B1/ko
Priority to CN97194790A priority patent/CN1113324C/zh
Priority to CZ0295898A priority patent/CZ298172B6/cs
Priority to IL12624897A priority patent/IL126248A/xx
Priority to DK97907475T priority patent/DK0888600T3/da
Priority to US09/142,936 priority patent/US6250316B1/en
Priority to CA002250140A priority patent/CA2250140C/fr
Priority to NL1006546A priority patent/NL1006546C2/nl
Priority to DE29712526U priority patent/DE29712526U1/de
Priority to CH181397A priority patent/CH689193A5/de
Priority to FR9709651A priority patent/FR2752637B3/fr
Priority to BE9700656A priority patent/BE1010154A6/nl
Publication of EP0824251A1 publication Critical patent/EP0824251A1/fr
Priority to OA9800168A priority patent/OA10877A/en
Priority to NO19984326A priority patent/NO314473B1/no
Priority to BG102776A priority patent/BG64429B1/bg
Priority to LVP-98-182A priority patent/LV12217B/en
Priority to HK99102803A priority patent/HK1017753A1/xx
Priority to GR20010401774T priority patent/GR3036904T3/el
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
    • G09F3/08—Fastening or securing by means not forming part of the material of the label itself
    • G09F3/18—Casings, frames or enclosures for labels
    • G09F3/20—Casings, frames or enclosures for labels for adjustable, removable, or interchangeable labels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08—Cleaning containers, e.g. tanks
    • B08B9/083—Removing scrap from containers, e.g. removing labels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08—Cleaning containers, e.g. tanks
    • B08B9/0861—Cleaning crates, boxes or the like
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B44—DECORATIVE ARTS
    • B44C—PRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
    • B44C1/00—Processes, not specifically provided for elsewhere, for producing decorative surface effects
    • B44C1/16—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like
    • B44C1/165—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like for decalcomanias; sheet material therefor
    • B44C1/17—Dry transfer
    • B44C1/1733—Decalcomanias applied under pressure only, e.g. provided with a pressure sensitive adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65C—LABELLING OR TAGGING MACHINES, APPARATUS, OR PROCESSES
    • B65C9/00—Details of labelling machines or apparatus
    • B65C9/0015—Preparing the labels or articles, e.g. smoothing, removing air bubbles
    • B65C2009/0018—Preparing the labels
    • B65C2009/0028—Preparing the labels for activating the glue
    • B65C2009/0031—Preparing the labels for activating the glue by radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65C—LABELLING OR TAGGING MACHINES, APPARATUS, OR PROCESSES
    • B65C9/00—Details of labelling machines or apparatus
    • B65C9/0015—Preparing the labels or articles, e.g. smoothing, removing air bubbles
    • B65C2009/0018—Preparing the labels
    • B65C2009/0028—Preparing the labels for activating the glue
    • B65C2009/0031—Preparing the labels for activating the glue by radiation
    • B65C2009/0037—UV
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65C—LABELLING OR TAGGING MACHINES, APPARATUS, OR PROCESSES
    • B65C9/00—Details of labelling machines or apparatus
    • B65C9/0015—Preparing the labels or articles, e.g. smoothing, removing air bubbles
    • B65C2009/0018—Preparing the labels
    • B65C2009/0028—Preparing the labels for activating the glue
    • B65C2009/0031—Preparing the labels for activating the glue by radiation
    • B65C2009/004—Preparing the labels for activating the glue by radiation electron beam

Definitions

  • the invention relates to a transfer label comprising a backing layer and a transfer layer which is releasably attached to the backing layer, the transfer layer comprising an ink layer.
  • the invention also relates to a container provided with a transfer layer according to the invention and to a method of removing the transfer layer from such a container.
  • a second way of labelling containers encompasses gluing printed paper labels to containers such as plastic crates or bottles at the time of filling and sealing.
  • This type of labels however offer little resistance to label damage from handling and exposure to moisture (wrinkling).
  • paper labels are difficult to remove from crates, and tend to clog the crate washers available today. Upon removal of paper labels from plastic crates, a glue residue may be left on the crates.
  • a third technique for labelling containers, in particular glass bottles is based on the principles described in WO 90/05088.
  • a method of labelling bottles is described which provides a durable, highly impact resistant label and yet permits high definition label printing.
  • a transfer label comprising a removable backing layer is provided which backing layer is reverse printed with a vinyl or acrylic ink which is cured and overprinted with adhesive.
  • the label is applied to the container with its adhesive surface in contact therewith.
  • the backing layer is separated from the transfer layer of the label for instance by the application of heat to either the container, the label or to both.
  • the labelled container is then applied with a coating which is subsequently cured.
  • the cured coating provides the required degree of impact resistance and durability.
  • the disadvantage of permanently attached labels is that when these labels get scratched or otherwise damaged, they cannot be easily removed from the bottles. Also, it is not possible to provide the same containers each time with new and/or different labels, which is desirable for promotional activities.
  • the labels should be applied and removed at relatively high speeds.
  • the transfer label according to the present invention is characterised in that the transfer layer comprises on each side of the ink layer a top and a bottom containment layer, respectively, the top and the bottom containment layer contacting one another outside the perimeter of the ink layer to form a closed envelope around the ink layer.
  • the ink in the envelope between the containment layers By entrapping the ink in the envelope between the containment layers, it is possible to remove the transfer layer from the container to which it has been attached, by a wet removal process such as a soaking process or a process utilizing high pressure water jets.
  • the ink is prevented from leaking out of the envelope during such a process such that no contamination of the wash water occurs.
  • a wet removal process not more than 10% by weight of the ink in a transfer layer is dissolved in an alkaline wash solution.
  • the containers are discoloured by the inks.
  • the ink levels in the wash solution remain low enough to not effect the aerobic and anaerobic treatment in the waste water treatment plants.
  • the low concentrations of inks in the wash water prevent accumulation of metals in the sludge of the waste water treatment plants, such that this sludge will not have to be treated as chemical waste under government regulations.
  • a very economic wash process can be achieved.
  • the ink layer comprises separate zones of dimensions between 0.5 mm 2 and 500 cm 2 , the top containment layer and the bottom containment layer contacting one another outside the separate zones to form individual envelopes around each zone of the ink layer.
  • the areas of the transfer layer connecting the separate zones of the ink layer will have a reduced thickness compared to the zones where an ink layer is present between the containment layers. After transfer of the transfer layer to a container, it is possible that no label material is present outside the separate ink zones. These areas of reduced thickness or open areas of the labels outside the envelopes, form natural points of attack for the wash solution, such that the label can be removed in separate parts.
  • wash solution has access to the label-container interface via the areas outside the envelopes around the print patterns, a very rapid removal of the transfer layer from the container is possible whereby the label is removed in separate pieces.
  • These pieces can be sieved from the wash solution using conventional sieves with openings having a size between 0.1 mm and 10 mm, preferably about 2 mm.
  • the label can also be used in combination with plastic bottles, such as PET-bottles, plastic food trays, glass bottles and the like
  • a preferred transfer label according to the present invention comprises a transfer layer which is permeable for the soaking liquids.
  • a transfer layer has a water uptake value after 3 hours between 0.0 and 100 g/m 2 , preferably about 5 g/m 2 , in water at room temperature.
  • Such labels have a water vapour transmission rate between 50 and 750 g/m 2 , preferably about 600 g/m 2 after 24 hours for water at room temperature.
  • the transfer layer may comprise a cover layer overlaying the ink pattern, which cover layer forms the outwardly facing surface upon attachment of the transfer layer to a container.
  • the cover layer may for instance be formed by an acrylic wax coating.
  • the cover layer may be a continuous layer, or may be discontinuous and printed in register with the ink pattern.
  • the acrylic wax cover layer can very advantageously be penetrated by for instance a 0.5% NaOH-solution, while providing a sufficient barrier to penetration of moisture during storage and use-conditions of the label on a container.
  • Labels according to the present invention which combine sufficient durability with quick and economic removal have a pencil hardness between 1N and 7N in the dry state and a pencil hardness less than 0.5 N after a soaking time between 1 minute and 15 minutes in water at 20°C.
  • the transfer layer has such a configuration that it breaks up in at least four pieces under turbulent soaking conditions in an aqueous liquid of a temperature below 100°C preferably below 70°C within a soaking time of not more than 20 minutes preferably not more than 10 seconds.
  • the size of the majority of the pieces formed upon breaking up of the transfer layer preferably is not smaller than the dimensions of the separate zones of the ink pattern.
  • the topmost containment layer comprises an unpigmented ink which is compatible with the underlying printed zone.
  • the bottom containment layer preferably comprises an adhesive layer or an intermediate layer which is compatible with an underlying adhesive layer and with the above located ink zone layer.
  • the top containment layer may be discontinuous and printed in register with the ink pattern. In this way the bottom containment layer may be directly attacked by the wash liquid during removal of the transfer layer. When the bottom containment layer is also discontinuous, the underlying adhesive layer can be directly attacked by the wash liquid. In a preferred embodiment both containment layers and an underlying adhesive layer are discontinuous and all printed in register.
  • a cover layer may be applied across the transfer layer the cover layer comprising an acrylic wax.
  • the acrylic wax is relatively impervious to water such that a good resistance of the label against scratching and removal of the label during use of the container is provided.
  • the acrylic wax cover layer however is pervious to an aqueous alkaline solution such that the transfer layer can easily be removed by for instance a 0.5% NaOH-solution.
  • the transfer layer is heat-treated after having been applied to a container to cause a shrinking of at least parts of the transfer layer.
  • a coalescing of the different layers of the transfer label takes place.
  • a label according to the present invention that combines sufficient durability during storage and use with quick and economic removal has preferably been heat treated after application to the container at a temperature between 40°C and 100°C, more preferably between 50°C and 90°C.
  • the selection of the adhesive to be used in adhering the label image to the container surface will influence the wash-off properties.
  • the adhesive must have been activated prior to or during application of the transfer layer to the container.
  • An easy and generally preferred method of applying the image is through the use of heat activatable adhesives that have been applied to the image in the form of a reverse printed label.
  • Other methods include the use of adhesive that can be activated through radiation, chemicals, electron-beam, micro-wave, UV and the like. It is also possible to use adhesives that can be activated through photo initiation, humidity, enzymatic action, pressure or ultrasonic treatment.
  • a preferred adhesive has a low tack temperature, preferably between 60° and 90,° more preferably between 80° and 90°.
  • a separate layer of adhesive it is also possible to use in the transfer layer an ink which in itself has adhesive properties upon activation.
  • the application surface of the container for receiving the transfer layer has a surface tension of at least 60 Dyne per cm.
  • the method of washing a container comprising a transfer layer according to the present invention comprises the steps of:
  • a transfer layer according to the present invention can be removed using conventional crate-washing equipment wherein the detached label pieces can be removed from the soaking solution by means of sieving. As no parts of the label dissolve in the soaking solution, no specific treatment equipment needs to be employed for cleaning the wash solution.
  • Figure 1 shows an embodiment of a transfer label 1 according to the present invention comprising a carrier, or backing layer 2 formed by for instance a two-mil thickness polypropylene film.
  • a silicone layer 3 is located on the carrier, or backing layer 2.
  • a transfer layer 4 is placed which consists of a top containment layer 5,5' an ink layer 7, 7', a bottom containment layer 6,6' and an adhesive layer 8, 8'.
  • the carrier layer 2 and the silicone layer 3 are removed under application of heat and pressure.
  • the adhesive layer 8 bonds the transfer layer 4 to an underlying container surface, and the outwardly facing layer is formed by the top containment layer 5, 5'.
  • the label carrier 2 which is provided with the electron beam cured silicon layer 3 can be for instance a polypropylene film of 1 to 3 mils thickness as supplied by Mobil Chemical, Films Division, Rochester, New York.
  • the silicone surface Prior to printing of the top containment layer 5, 5' onto the silicone layer 3, the silicone surface must be corona treated.
  • a corona treatment will allow uniform wetting of the print materials and still allow for release of the transfer layer 4.
  • the corona treatment is applied to the carrier layer 2 and silicone layer 3 shortly before the first print of the top containment layer 5 is applied.
  • a target treatment level should be approximately 30% of 3,5 kW.
  • the top containment layer 5, 5' consists for instance of unpigmented ink and has several functions. Firstly it slows or prevents water penetration into the underlying ink layer 7,7'. As the layer 5, 5' is printed wider than the underlying ink pattern 7,7' it forms part of an envelope which totally surrounds the colored ink layers 7, 7'. Furthermore the top containment layer 5, 5' provides a consistent medium between the inks and the silicone release surface 3. The layer 5, 5' is very important to the overall transferability of the label and should be applied at a weight of at least 1.4 g/m 2 . It is important that upon application of the top containment layer 5, 5' this layer is free of airbubbles and pinholes. Furthermore the top containment layer must be dry before printing the subsequent ink layer 7,7' thereon.
  • top containment layer 5,5' After printing the top containment layer 5,5' onto the release layer 3, an optimum peel force of 100 g or less should be measured in a standard tape peel test. Within five hours after application, the peel force of the top containment layer will be about 60% less, or 40 g. With the specified peel force, the containment layer 5 should be removed completely.
  • a suitable material for the top containment layer 51 is available from Environmental Inks and Coatings, Morganton, North Carolina under type number 1304.
  • Examples of a preferred ink for the ink layer 7,7' include a waterborne organic as available from Environmental Inks and Coatings, Morganton, North Carolina under type number Aqua BW EH-31721, EH 53016, EH 90967. These inks have a high stability even at temperatures over 200°C without discoloration or loss of adhesion.
  • the bottom containment layer 6,6' provides a strong interface between the adhesive layer 8,8' and the colored ink layers 7,7'. It is formulated to chemically anchor to the ink and provide excellent wetting and bounding of the adhesive layer.
  • the bottom containment layer 6,6' attaches outside the ink layer 7,7' to the top containment layer 5,5' such that a closed envelop is formed around the separate ink patterns 7, 7'.
  • a suitable material for the bottom containment layer 6,6' is available from Environmental Inks and Coatings under type no. XP 11358.
  • the adhesive layer 8,8' can be formed by a waterborne organic material which is printed in a number of consecutive flexographic stations such as three stations, or can be floodcoated on a single station.
  • the adhesive layer 8,8' may also be applied by a single gravure printing station.
  • the adhesive 8,8' is heat-activated and has a low tack temperature from 80°C up to 107°C.
  • the preferred weight of adhesive is approximately, 3.5 g/m 2 .
  • the layers of the transfer layer 4 may be applied in a flexographic printing press with up to 10 printing stations. Five stations may be used for printing the layers 5,5', 6,6' and the adhesive layer 8,8' which can be composed of three separate adhesive layers. Five types of colored ink 7,7' may be applied using the five remaining flexographic printing stations.
  • a gravure press equiped with a corona treater may be used instead of a flexographic printing process. Because material laydown is heavier than in the flexographic process, only three gravure printing stations may be necessary for applying the containment layers 5, 5' and 6, 6' and the adhesive layer 8, 8'.
  • rotary screen printing processes can be used for applying layers 5,5', 6,6' and 8,8'.
  • the adhesive layer 8,8' extends beyond the perimeter of the bottom containment layer and matches the perimeter of the topmost containment layer 5,5'.
  • FIG. 2 shows a schematic side view of a crate washing apparatus for removing the transfer layers according to the present invention from crates 12 that are supplied to the crate washer 10 via a transport conveyor 11.
  • Crates 12 are first transported to pre-rinsing station 13 and sprayed with a pre-rinsing solution which is applied from a number of nozzles 14 located above and below the transport conveyor 12.
  • the speed of the conveyor 11 is such that the dwell time of the crate 11 in the pre-rinsing station is between 6 and 8 seconds.
  • the temperature of the pre-rinse solution is 60°C.
  • the pre-rinse solution preferably comprises a 0.5% NaOH solution.
  • the crates After passing through the pre-rinsing station 13, the crates are transported through a soaking station 15 via a downwardly sloping section 16 of the conveyor 11.
  • the dwell time of crate in the soaking station is between 10 and 40 seconds.
  • the crate In the soaking station, the crate is completely submerged and a soaking solution is recirculated in the soaking station 15 by means of nozzles 35 to cause turbulent soaking conditions.
  • the turbulent soaking conditions may for instance include recirculating the liquid from the soaking station 15 via the nozzles 35 at a rate of 60 m 3 /h for a total volume of the soaking solution of 5 m 3 . It is important that the transfer layers are completely removed from the crates 12 in the soaking station 15, without any pieces remaining on the crates. Such remaining pieces would, when dried, adhere firmly to the crates and form an undesired contamination of the crate surface.
  • the crates are transported via the upwardly sloping conveyor track 17 to an after-rinse station 18.
  • the after-rinse solution may comprise water at a temperature of 30°C.
  • the dwell time of the crates in the after-rinse station 18 is between 6 and 13 seconds.
  • each sieving section comprises a rotating belt sieve 23, 24, 25, which are driven by motors 26, 27, 28 respectively.
  • Pumps 29, 30 and 31 draw the rinsing liquid and the soaking liquid from each perspective station through the rotating sieve belts 23, 24, 25 a rate of for instance 60 m 3 /h.
  • the sieved liquids are recirculated back to nozzles 14 and 19 in the pre-rinse and after-rinse stations 13, 18 respectively and to the soaking station 15.
  • Figure 3 shows a cross-sectional view along the lines III-III of figure 2. It can be seen that the sieve belt 24 is rotated around two rollers 37, 38. The top end of the sieve belt 24 extends above the level of the soaking liquid in the soaking station 15.
  • the sieve belt 24 comprises a dual layer belt-like sieving element with a mesh size of 2 millimetres. During operation it is important to continuously rotate the sieve belt 24 to prevent the label pieces from the transfer layers that break up into pieces in the soaking station 15, from clogging the sieve belt.
  • a spraying nozzle 39 cleans the surface of the belt-like sieving elements by high pressure water or air jets. The removed label elements are collected in a collection compartment 40.
  • Figure 4 shows an alternative embodiment of a transfer label according to the invention comprising a backing layer 48, a silicone release layer 49 and a transfer layer 50.
  • the ink layer 52 of the transfer layer 50 is a continuous layer which may for instance have dimensions of 10 by 10 centimetres.
  • the top containment layer 51 and the bottom containment layer 53 encase the ink layer 52 and engage one another around the perimeter of the ink layer.
  • a single envelope is formed around the ink layer 52.
  • the transfer layer 50 may rupture into several pieces. Thereby the envelope formed by the top and bottom containment layers 51, 53 will be ruptured. However it was found that still sufficient containment in that case occurs to prevent the ink layer 52 from dissolving in the wash solution.
  • the ink layer 52 is formed of separate zones 52,52'. Each zone of the ink layer may be formed by for instance individual letters, individual sentences, or individual blocks of words. The individual zones 52,52' can also be formed by other graphic objects. It is shown that the top containment layer 51 attaches to the bottom containment layer 53 around the perimeter of each individual ink zone 52,52'. Thereby envelopes around each individual ink zone are formed and efficient containment is possible.
  • the top containment layer 51 is formed of separate zones 51,51'. Through the open areas between the separate zones of the top containment layer 51,51' the wash solution can easily penetrate and attack the underlaying containment layers 53 and adhesive layer 54.
  • the adhesive layer 54, the bottom containment layer 53, the ink layer 52 and the top containment layer 51 are each printed in register and form separate zones 51, 51', 52, 52', 53, 53' and 54, 54'.
  • Such a transfer layer has a very attractive appearance and the container surface is clearly visible in between each individual ink zone 52, 52'.
  • a very rapid washability is achieved as the wash liquid can very rapidly attack the adhesive layer 54, 54' by penetrating through the open areas between each ink zone 52, 52'.
  • a transfer layer according to the present invention can be comprised of several parts.
  • a graphic object 55 such as a picture can consist of a single ink layer which around its perimeter 55' is encased between an upper and a lower containment layer, of a structure as shown in figure 4.
  • separate lines of text 56 may be encased between an upper and a lower containment layer, for instance with a structure according to figure 5, figure 6 or figure 7.
  • individual letters in a sentence may be each be individually encased between the top and bottom containment layer.
  • Figure 9 shows a schematic view of the application process of a transfer layer from a transfer label according to the invention to a returnable crate 59.
  • Station 60 shows the step of surface treatment and temperature stabilization by means of a pre-heating treatment using a flame heater or burner 60'.
  • a flame heater or burner 60' For adhesion of two polymeric materials to occur, many factors must be considered such as cleanliness, pressure, temperature, contact time, surface roughness, movement during bonding and adhesive film thickness. An additional important consideration is the critical surface tension.
  • the commonly accepted method of measuring the critical surface tension is with a Dyne solution, which is well known.
  • the critical surface tension of polyethylene is 31 Dynes per centimetre.
  • a series of tests were performed which demonstrated for best adhesion of the adhesive previously described to the polyethylene surface, a treatment level of 60 to 70 Dynes per centimetre was necessary. Further testing of commercially available equipment showed that flame treatment optimized both capital cost, operating cost and time required to achieve the required critical surface treatment.
  • Station 62 illustrates the method of label application whereby the printed ink materials are transferred from the polypropylene film substrate to the polyethylene surface utilizing the tactile characteristics of the heat activated adhesive to overcome the bond of the transfer layer to the corona treated silicone coating.
  • the factors that influence transfer are time to contact, temperature and pressure applied during contact and film tension during contact particularly tension of the film after ink release.
  • the diameter of pressure roll 63 is also a factor but not a variable. For this application the roll diameter is 38 mm.
  • the roller 63 is made of silicone rubber over a steel core, with rubber durometer ranging from 50 Shore A to 80 Shore A. It should be noted that distortion (flattening) of the rubber roller is less at higher durometer, consequently the contact area is less and the transfer pressure is greater.
  • Roller pressure is provided by an air cylinder 64 activated by a conventional solenoid valve which in turn is operated by two (2) proximity switches, one to advance the roller and the other to retract. Other means, such as mechanical linkage are obvious and will not be listed here.
  • the pressure is distributed across the length of the cylinder and for this particular label, transfer ranges from 12 to 17 kilograms per centimetre of roller length are desirable.
  • the invention results in the film being advanced at exactly the same rate as the crate is moving past the roller by virtue of the heat activated adhesive adhering to the high energy crate surface.
  • the pressure roller 63 which rotates freely, maintains the same tangential speed as the linear speed of the film and crate. Thus the ink is transferred completely and without distortion.
  • the pressure roller 63 is molded to a hollow core. Suspended within the hollow core is a resistance heater operated through a controller. The heating element, rated at 500 W, will maintain the roller surface at any predetermined temperature. For purposes of the invention, the roller surface temperature range between 250°F and 370°F (120°C and 190°C).
  • High temperature films such as polyester may be operated in continuous contact with the heated roller.
  • Low temperature films such as polypropylene must be prevented from contacting the heated roller during pauses in the labelling operation.
  • film guides 65 are used to support the film when the roller is retracted. The guides 65 are mounted to maintain a clearance of approximately 13 mm between the guides and the labelled surface. At the same time the roller is retracted approximately 13 mm behind the film. By maintaining those clearances, stretching and distortion of the film such as polypropylene is avoided. High temperature films would not require the guides.
  • Conventional nip rollers and stepping motor are used to advance the film to the next label and position it accurately, using a printed mark to trigger an optical scanning device.
  • the final processing step is to coalesce the layers of the coating, label ink, and adhesive at station 67 by means of flame heater 67' and also to inter diffuse the adhesive layer with the polyethylene substrate formed by the crate 59.
  • a transfer layer 50 having the configuration as shown in figure 4 was applied to a polyethylene crate.
  • the dimensions of the label were about 10 by 10 centimetre and the adhesive layer 54 was a 100% urethane adhesive with a tack temperature of 79°C.
  • the labels were applied to the crate with a temperature of roller 63 in figure 9 of 155°C at a roller pressure of 2.5 bar.
  • the pre-heat temperature of the crate (in stations 60 and 61 of figure 9), was 75°C.
  • the speed of the crates 59 through the label applicator was 40 crates per minute.
  • post-treat temperatures 40°C, 65°C and 90°C were used.
  • the crates were stored for at least 24 hours at a temperature of 20°C.
  • the crates to which a label was applied, were thereafter soaked in a 0.5% NaOH-solution at temperatures of 20°C, 50°C and 70°C.
  • the soaking of the crates was carried out in a soaking bath of 20 litres without turbulence, for such a soaking time (10-50 seconds) that after spraying the soaked crate with a showerhead at a rate of 6 litres/minutes, the label was completely removed within 2 seconds.
  • a second set of crates was prepared wherein after label application, a coating layer of wax was applied, such as at station 66 of figure 9.
  • the purpose of the pencil scratch test is to identify the minimum and maximum durability of a label which can be obtained by taking different measures such as the use of a covering wax layer and heat treatment to cause coalescing of the label layers. Crates with labels which were applied with different post-heating temperatures, with and without wax, have been tested.
  • the labels were the same labels as used in the washing trial described above, and were applied to the crates under the same conditions.
  • the crates were stored for at least 24 hours at a temperature of 20°C. Prior to scratching, the crates were soaked in a water without turbulence at 20°C. The results of the scratch test are given in table III and table IV in which the scratch results are given in N.
  • Pencil scratch test (in N) label without wax coating Post-heat Temperature (°C) soaking time (min) 0 0.5 1 1.5 2 2.5 3 3.5 none 1 0.4 0.2 0.1 1 0.3 0.2 0.1 40 1.3 0.9 0.2 0.1 1.1 0.7 0.2 0.1 65 1.1 0.7 0.2 0.1 1 0.5 0.1 0.1 90 1.5 1.2 0.8 0.6 0.6 0.4 0.2 0.1 1.1 1 0.8 0.6 0.5 0.3 0.2 0.1 Pencil scratch test (in N) label with wax coating Posttreat soaking time (°C) (min) 0 0.5 1 1.5 2 2.5 3 4 5 6 7 8 9 10 none 5 3 1.4 0.5 0.3 0.2 0.1 5 3 1.5 0.7 0.4 0.2 0.1 40 5 2.8 1.3 0.4 0.3 0.1 5 3 1.4 0.6 0.4 0.2 0.1 65 5 2.5 1.2 0.5 0.3 0.2 0.1 5 2.9 1.3 0.5 0.2 0.1 90 5 4 2.5 1.3 0.7 0.7 0.6 0.4 0.4 0.3 0.3
  • the strength of the labels was found to be insufficient for labels which did not have a wax coating.
  • the target pencil hardness in the dry state should be around 1.2 N and the soaking time until the scratch force drops below 0.3 Newton should be below 3 minutes.
  • the target scratch force should be about 5 Newton in the dry state and the soaking time until the scratch force drops below 0.3 N should be below 10 minutes. Transfer layers having the above properties were found to have an optimal combination of durability and washability.
  • the labels according to the present invention can be easily removed from a container, in particular from a plastic crate due to their specific water permeability which allows the soaking solution to penetrate the label, and subsequently beak up the label in pieces and detach it from the container. It was found that preferred labels have a water absorption of around 5 g/m 2 after 3 hours in a water uptake test as described below. Labels according to the invention have a water uptake value higher than 0 and less than 100 g/m 2 in 3 hours. The water release of a preferred label was 4.5 g/m 2 within 30 minutes in the water release test as described below. Preferred labels according to the present invention will have a water release value greater than 0 (a complete barrier) and less than 100 g/m 2 after 3 hours.
  • the samples were prepared as follows: the glass supports were thoroughly cleaned and placed in a heating oven until an approximate temperature of 250°F was reached on the glass surface. The glass was then removed from the heating oven and placed on a silicone rubber mat. A label was immediately set on the glass and secured to the surface by the use of a silicone roller. Rolling pressure was continually supplied to the full length of the label until all entrapped air was removed (approximately 5-6 back and forth motions). After the glass had cooled, the carrier film was removed.
  • the opposite side of the glass plates were labelled by heating a clean aluminium plate (slightly larger than the glass plate) to approximately 250°F in a convective oven, then placing the glass on the surface of the aluminium plate (label surface down) which allowed the heating of the glass upper surface.
  • the label was then applied and secured in place by the silicone roller as described above.
  • the carrier film was removed.
  • a wax coating having a dry weight of 0.043 grams was applied to the surface of both labels.
  • flame treatment was applied to both labels by quickly passing the flame across the entire surface of the label sample. Once the samples were cooled the labels were ready for the Water Uptake test.
  • a stainless steel immersion tank of a 33.66 centimetre diameter and 24.13 centimetre height was filled with the deionized water. Care was taken that the water level was deep enough to allow total immersion of the sample.
  • the sample was placed with the short dimension set perpendicular to the bottom of the tank.
  • the glass supports were placed on a thin wire frame in the immersion tank.
  • a thermocouple was installed inside the water immersion tank. After each time period, as given in table V, the sample was removed from the tank, excess surface water was blotted dry, the sample was weighted and placed back in the tank. This procedure was continued for the duration of the test. The results are shown in table V.
  • sample 1 With regard to sample 1, this sample reached it maximum absorption of 0.04 grams at the 3 hour mark and maintained this level to the 5 hour mark before giving up its ability to retain water at this level. After the 5 hour period the label lost its ability to hold water. We believe this phenomenon was caused because of label structure degradation. For sample 2, this sample also reached its maximum absorption of 0.04 grams at a 3 hour mark. At the 5 hour mark this sample was terminated from further testing in preparation for the water release test described below.
  • a preferred label of a thickness of 12.7 microns has a water uptake value of 0.04g/85.8 cm 2 or about 5g/m 2 after 3 hours at room temperature.
  • Water Uptake Test Time Sample 1 Weight in grams Sample 2 Weight in grams Relative Humidity (%) Tank Water Temperature (°F) Room Air Temperature (°F) 8:00 a.m. 59.77 59.77 47 71 72.4 8:10 a.m. 59.80 59.80 47 71 72.4 9:00 a.m. 59.81 59.81 47 71 72.4 10:00 a.m. 59.83 59.83 47 71 72.4 11:00 a.m.
  • the sample 2 as prepared above was subjected to the water release test.
  • the sample was blotted to remove access water, weighted and the data were recorded.
  • the sample was first exposed to ambient temperature for one half hour and weighed.
  • Half an hour after weighing the sample it was placed in a prewarmed (53°C) test oven (small electrically heated oven, Quieny Lab Inc., Model 20 Lab oven or equivalent).
  • the sample was left in the prewarmed oven for more than one hour and weighted. Thereafter the sample was placed back in the test oven and remained there for 3.5 hours.
  • the optimum combination of durability and washability of the labels according to the invention is at least partly due to the permeability of the label for the soaking solution.
  • a sample of the transfer layer of the same type as tested in the water uptake/release test of a thickness of 12.7 microns was tested for water vapour transmission.
  • a 25 millilitre glass container with a 15.9 millilitre orifice was cleaned with acetone and filled with approximately 10 millilitres of deionized water.
  • the orifice area of the container was heated to approximately 118°F and a circle segment of the transfer layer was firmly applied using a small piece of silicone rubber as a pressure pad. After the container/label had cooled, the backing film was gently removed.
  • the sample preparation was completed by adding a wax coating (0.001 g across the 1.99 cm 2 surface) and let air dry.
  • a second glass container of the same dimensions as described above was cleaned thoroughly with acetone and filled with 10 millilitre of deionized water. The orifice area of the sample was heated as well. This sample was used as the control sample.
  • the completed samples were then weighted various intervals over a 26.6 hour time period.
  • the water vapour transmission rate over the total time of the experiment equated to 568.75 g/m 2 in a 24 hour time period at 22.2°C at 46% relative humidity. It was found that a "steady state” water vapour transmission rate was not achieved until approximately 28 minutes from time 0. When using the "steady state” data after 28 minutes from time 0, the water vapour transmission rate was found to be about 526.93 g/m 2 in 24 hours.
  • the water vapour transmission rate of the preferred label according to the present invention will lay between 50 g/m 2 and 750 g/m 2 after 24 hours (22.2°C, 44% relative humidity), preferably around 500 g/m 2 after 24 hours.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Theoretical Computer Science (AREA)
  • Details Of Rigid Or Semi-Rigid Containers (AREA)
  • Decoration By Transfer Pictures (AREA)
  • Laminated Bodies (AREA)
EP96202264A 1996-03-20 1996-08-12 Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient Withdrawn EP0824251A1 (fr)

Priority Applications (37)

Application Number Priority Date Filing Date Title
EP96202264A EP0824251A1 (fr) 1996-08-12 1996-08-12 Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient
PL97329029A PL185928B1 (pl) 1996-03-20 1997-03-19 Etykieta nośna na pojemnik i sposób zmywania etykiety nośnej z pojemnika
PCT/NL1997/000137 WO1997035290A1 (fr) 1996-03-20 1997-03-19 Etiquette imprimee par transfert a chaud pourvue de couches d'isolement, contenant pourvu d'une couche de transfert et procede de nettoyage de ce contenant
AU19466/97A AU711502B2 (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such container
EE9800320A EE03785B1 (et) 1996-03-20 1997-03-19 Siirdeetikett konteinerile ja siirdeetiketi mahapesemise meetod konteinerilt
AT97907475T ATE203845T1 (de) 1996-03-20 1997-03-19 Etikett zum übertragen mit tintenhaltigen schichten, behälter mit transferschicht und verfahren zum reinigen eines solchen behälters
DE69705935T DE69705935T2 (de) 1996-03-20 1997-03-19 Etikett zum übertragen mit tintenhaltigen schichten, behälter mit transferschicht und verfahren zum reinigen eines solchen behälters
SI9730195T SI0888600T1 (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container
SK1281-98A SK128198A3 (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container
KR10-1998-0707432A KR100481951B1 (ko) 1996-03-20 1997-03-19 잉크봉쇄층을갖는전사라벨,전사라벨로이루어진용기및그용기의세척방법
ES97907475T ES2162254T3 (es) 1996-03-20 1997-03-19 Etiqueta de transferencia que tiene capas de contencion de tinta, envase que comprende una capa de transferencia y metodo de lavado de dicho envase.
JP53337297A JP2000507363A (ja) 1996-03-20 1997-03-19 インキ包み込み層を有する転写ラベル、転写層を含む容器並びにかかる容器を洗浄する方法
EA199800838A EA000487B1 (ru) 1996-03-20 1997-03-19 Переводная этикетка, тара, содержащая переводной слой, способ мойки тары
PT97907475T PT888600E (pt) 1996-03-20 1997-03-19 Etiqueta de estampar que possui camadas de contencao de tinta contentor que compreende uma camada de estampar e processo para a lavagem de um tal contentor
EP97907475A EP0888600B1 (fr) 1996-03-20 1997-03-19 Etiquette imprimee par transfert a chaud pourvue de couches d'isolement, contenant pourvu d'une couche de transfert et procede de nettoyage de ce contenant
APAP/P/1998/001345A AP1037A (en) 1996-03-20 1997-03-19 Transfere label having ink containment layers, container comprising a transfer layer and method of washing such a container.
TR1998/01852T TR199801852T2 (xx) 1996-03-20 1997-03-19 M�rekkep i�eren katlar� mevcut ��kartma tipi etiket, �zerine s�z konusu etiket tatbik edilmi� kutular ve bu t�r kutular� y�kama y�ntemi.
YU40598A YU49317B (sh) 1996-03-20 1997-03-19 Prenosna etiketa koja ima slojeve za zadržavanje boje, kontejner koji sadrži prenosni sloj i postupak pranja takvog kontejnera
NZ331863A NZ331863A (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container
BR9708112-4A BR9708112A (pt) 1996-03-20 1997-03-19 Rótulo de transferência recipiente compreendeno uma camada de transferência e processo para lavar um recipiente.
CN97194790A CN1113324C (zh) 1996-03-20 1997-03-19 转印标签及包含这种标签的容器
CZ0295898A CZ298172B6 (cs) 1996-03-20 1997-03-19 Obtisková nálepka, kontejner s obtiskovou nálepkou a zpusob mytí kontejneru
IL12624897A IL126248A (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers container comprising a transfer layer and method of washing such a layer
DK97907475T DK0888600T3 (da) 1996-03-20 1997-03-19 Overførselsetiket, der har farveindeslutningslag, beholder, der omfatter et overførselslag, og fremgangsmåde til vask af en sådan beholder
US09/142,936 US6250316B1 (en) 1996-03-20 1997-03-19 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container
CA002250140A CA2250140C (fr) 1996-03-20 1997-03-19 Etiquette imprimee par transfert a chaud pourvue de couches d'isolement, contenant pourvu d'une couche de transfert et procede de nettoyage de ce contenant
NL1006546A NL1006546C2 (nl) 1996-08-12 1997-07-10 Overdruklabel met inktopsluitende lagen, houder voorzien van een overdruklaag en werkwijze voor het wassen van een dergelijke houder.
DE29712526U DE29712526U1 (de) 1996-08-12 1997-07-15 Transferetikett bzw. Abziehlabel mit Druckfarben-Schutzschichten sowie Behälter mit einem solchen Abziehlabel
FR9709651A FR2752637B3 (fr) 1996-08-12 1997-07-29 Etiquette a decalquer contenant des couches de confinement pour l'encre, recipient comportant une couche de transfert et procede pour laver un tel recipient
CH181397A CH689193A5 (de) 1996-08-12 1997-07-29 Transferetikett bzw. Abziehlabel mit Druckfarben-Schutzschichten sowie Behaelter mit einem solchen Abziehlabel.
BE9700656A BE1010154A6 (nl) 1996-08-12 1997-08-01 Overdruklabel met inktopsluitende lagen, houder voorzien van een overdruklaag en werkwijze voor het wassen van een dergelijke houder.
OA9800168A OA10877A (en) 1996-03-20 1998-09-16 Transfer label having ink containment layers container comprising transfer layer and method of washing such a container
NO19984326A NO314473B1 (no) 1996-03-20 1998-09-17 Overföringsmerkelapp, beholder med et overföringssjikt påfört ved hjelp avoverföringsmerkelappen, samt fremgangsmåte ved vasking av beholder
BG102776A BG64429B1 (bg) 1996-03-20 1998-09-18 Сменяем етикет, притежаващ слоеве за защита на мастилото, контейнер, върху който е разположен трансферен слой, и метод за измиване на този контейнер
LVP-98-182A LV12217B (en) 1996-03-20 1998-09-18 FOLDING LABEL WITH SURFACE LUBRICATED LAYER WITH CLEANING LABEL AND THE WASHING METHOD OF THIS BOX
HK99102803A HK1017753A1 (en) 1996-03-20 1999-07-03 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container
GR20010401774T GR3036904T3 (en) 1996-03-20 2001-10-16 Transfer label having ink containment layers, container comprising a transfer layer and method of washing such a container

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP96202264A EP0824251A1 (fr) 1996-08-12 1996-08-12 Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient

Publications (1)

Publication Number Publication Date
EP0824251A1 true EP0824251A1 (fr) 1998-02-18

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EP96202264A Withdrawn EP0824251A1 (fr) 1996-03-20 1996-08-12 Etiquette appliquée par transfert, munie de couches contenant de l'encre, récipient comprenant une couche de transfert et méthode de nettoyage d'un tel récipient

Country Status (6)

Country Link
EP (1) EP0824251A1 (fr)
BE (1) BE1010154A6 (fr)
CH (1) CH689193A5 (fr)
DE (1) DE29712526U1 (fr)
FR (1) FR2752637B3 (fr)
NL (1) NL1006546C2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0976580A1 (fr) * 1998-07-28 2000-02-02 Heineken Technical Services B.V. Etiquette adhésive sensible à la pression et procédé pour apposer l'étiquette
US6376069B1 (en) 1999-06-25 2002-04-23 Avery Dennison Corporation Heat-transfer label including non-wax release layer
US6893717B1 (en) 1999-07-08 2005-05-17 Kuolih Tsai Heat-transfer label including non-wax release coating
EP3995221A1 (fr) * 2020-11-05 2022-05-11 Milla Masanas, S.L.U. Installation destinée à enlever automatiquement les étiquettes des caisses
CN116080294A (zh) * 2022-12-12 2023-05-09 库尔兹压烫科技（合肥）有限公司 转移膜、用于制造转移膜的方法和用于回收转移膜的方法

Families Citing this family (4)

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DE20319250U1 (de) * 2003-12-10 2005-04-21 Rottaler Fruchtsaft Eg Folienmantel
WO2009034466A2 (fr) * 2007-09-14 2009-03-19 Ooo 'likoflex' Étiquette autocollante
DE102014108624B4 (de) * 2014-06-18 2021-01-07 Trautwein Gmbh & Co. Siegelsystem
CN109604290A (zh) * 2018-11-10 2019-04-12 无锡芯启博科技有限公司 一种料盒清洗周期的标记方法及其料盒

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DE3037250A1 (de) * 1980-10-02 1982-04-29 Joachim 7440 Nürtingen Dudzik Selbstklebeetikett
WO1990005088A1 (fr) 1988-11-07 1990-05-17 Brandt Manufacturing Systems, Inc. Etiquette pour recipient et systeme d'application de l'etiquette
EP0510403A1 (fr) * 1991-04-26 1992-10-28 Zweckform Etikettiertechnik Gesellschaft Mit Beschränkter Haftung Etiquette
EP0615838A1 (fr) * 1993-02-12 1994-09-21 Cofradec S.A. Produit composite stratifié

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DE3037250A1 (de) * 1980-10-02 1982-04-29 Joachim 7440 Nürtingen Dudzik Selbstklebeetikett
WO1990005088A1 (fr) 1988-11-07 1990-05-17 Brandt Manufacturing Systems, Inc. Etiquette pour recipient et systeme d'application de l'etiquette
EP0510403A1 (fr) * 1991-04-26 1992-10-28 Zweckform Etikettiertechnik Gesellschaft Mit Beschränkter Haftung Etiquette
EP0615838A1 (fr) * 1993-02-12 1994-09-21 Cofradec S.A. Produit composite stratifié

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0976580A1 (fr) * 1998-07-28 2000-02-02 Heineken Technical Services B.V. Etiquette adhésive sensible à la pression et procédé pour apposer l'étiquette
US6376069B1 (en) 1999-06-25 2002-04-23 Avery Dennison Corporation Heat-transfer label including non-wax release layer
US6423406B1 (en) 1999-06-25 2002-07-23 Avery Dennison Corporation Heat-transfer label including non-wax release layer
US6893717B1 (en) 1999-07-08 2005-05-17 Kuolih Tsai Heat-transfer label including non-wax release coating
EP3995221A1 (fr) * 2020-11-05 2022-05-11 Milla Masanas, S.L.U. Installation destinée à enlever automatiquement les étiquettes des caisses
US11938526B2 (en) 2020-11-05 2024-03-26 Mimasa Washtech, S.L.U. Installation intended to automatically remove labels of crates
CN116080294A (zh) * 2022-12-12 2023-05-09 库尔兹压烫科技（合肥）有限公司 转移膜、用于制造转移膜的方法和用于回收转移膜的方法
CN116080294B (zh) * 2022-12-12 2024-03-26 库尔兹压烫科技（合肥）有限公司 转移膜、用于制造转移膜的方法和用于回收转移膜的方法

Also Published As

Publication number Publication date
NL1006546C2 (nl) 1997-10-23
CH689193A5 (de) 1998-11-30
NL1006546A1 (nl) 1997-10-15
DE29712526U1 (de) 1997-09-18
BE1010154A6 (nl) 1998-01-06
FR2752637A3 (fr) 1998-02-27
FR2752637B3 (fr) 1998-07-24

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