WO2000012809A1 - Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier. - Google Patents

Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier. Download PDF

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Publication number
WO2000012809A1
WO2000012809A1 PCT/DK1999/000436 DK9900436W WO0012809A1 WO 2000012809 A1 WO2000012809 A1 WO 2000012809A1 DK 9900436 W DK9900436 W DK 9900436W WO 0012809 A1 WO0012809 A1 WO 0012809A1
Authority
WO
WIPO (PCT)
Prior art keywords
pattern
paper
colour
printing
web
Prior art date
Application number
PCT/DK1999/000436
Other languages
French (fr)
Inventor
Knud Villefrance Rasmussen
Original Assignee
Dansk Hk Ltd.
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=8100658&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2000012809(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Priority to US09/763,687 priority Critical patent/US6805046B1/en
Priority to EP99936441A priority patent/EP1125015B1/en
Priority to IL14160899A priority patent/IL141608A0/en
Priority to AT99936441T priority patent/ATE236287T1/en
Priority to HU0103230A priority patent/HU226431B1/en
Priority to DE69906563T priority patent/DE69906563T2/en
Priority to MXPA01001986A priority patent/MXPA01001986A/en
Priority to CA002341728A priority patent/CA2341728C/en
Priority to EA200100279A priority patent/EA002519B1/en
Application filed by Dansk Hk Ltd. filed Critical Dansk Hk Ltd.
Priority to SI9930302T priority patent/SI1125015T1/en
Priority to NZ510123A priority patent/NZ510123A/en
Priority to AU51535/99A priority patent/AU755480B2/en
Priority to JP2000567784A priority patent/JP4317979B2/en
Priority to BRPI9913207-9A priority patent/BR9913207B1/en
Priority to DK99936441T priority patent/DK1125015T3/en
Priority to PL346304A priority patent/PL200657B1/en
Publication of WO2000012809A1 publication Critical patent/WO2000012809A1/en
Priority to IL141608A priority patent/IL141608A/en
Priority to NO20010896A priority patent/NO20010896L/en
Priority to HK02103020.6A priority patent/HK1041298B/en

Links

Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/003—Transfer printing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/025—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/502—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording characterised by structural details, e.g. multilayer materials
    • B41M5/508—Supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/025—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet
    • B41M5/0256—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet the transferable ink pattern being obtained by means of a computer driven printer, e.g. an ink jet or laser printer, or by electrographic means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/025—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet
    • B41M5/035—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet by sublimation or volatilisation of pre-printed design, e.g. sublistatic
    • B41M5/0355—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet by sublimation or volatilisation of pre-printed design, e.g. sublistatic characterised by the macromolecular coating or impregnation used to obtain dye receptive properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B41M5/5227—Macromolecular coatings characterised by organic non-macromolecular additives, e.g. UV-absorbers, plasticisers, surfactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B41M5/5236—Macromolecular coatings characterised by the use of natural gums, of proteins, e.g. gelatins, or of macromolecular carbohydrates, e.g. cellulose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
    • D06P1/48—Derivatives of carbohydrates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
    • D06P1/48—Derivatives of carbohydrates
    • D06P1/50—Derivatives of cellulose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651—Compounds without nitrogen
    • D06P1/65106—Oxygen-containing compounds
    • D06P1/65118—Compounds containing hydroxyl groups

Definitions

  • Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier.
  • the present invention relates to a pattern carrier in form of a paper web with a colour pattern printed thereon and to be used in transfer pattern printing of a moist textile web.
  • the invention relates also to the use of a saccharide syrup known per se as an ingredient in a dispersion for coating a paper web so as to obtain a pattern carrier with particular properties.
  • Transfer pattern printing is a well-known and extensively used technique, which involves a continuous transfer of a pre-printed pattern from a pattern carrier web to a moist textile web, where the two webs are continuously brought into contact with one another in a transfer region which is frequently in the form of one or more pairs of pressure rollers, cf. the Figure.
  • DK-PS No. 169 135 is characterised by a suitable choice of pattern carrier and dye formulations, an accurate control of the moistening of the textile web and the use of a suitably high pressure, whereby particularly good reproducible results can be obtained at rather high processing speeds and, as mentioned, without the use of heating and exclusively by the use of water-based dye formulations.
  • the process according to DK-PS No. 169 135 also presented obvious environmental and energy-related advantages as well as a substantially improved working environment.
  • This epoch-making process is, however, also subject to limitations. To be more precise this process presents particular requirements to the paper used as pattern carrier because said paper must be of a specific nature in order to be coated with a colour pattern at the desired printing speed. It is necessary to use a paper quality which is only slightly absorbing, and in order to avoid that the various, applied colours become blurred it is necessary to strongly cool the paper web between each application of colour in order to solidify the colour.
  • the printing of the paper is carried out by means of printing screens as shown in the Figure.
  • DK-PS No. 169 135 necessitates introduction of cooling rollers not shown between the individual printing screens.
  • the coated paper web is carried around these cooling rollers while subjected to a cooling to below -20°C.
  • this "freezing" does, of course, complicate the entire process significantly and intensifies the costs involved, and accordingly it is desired to provide a pattern carrier where the colours do not become blurred - not even at high printing speeds, and which therefore does not require a cooling between the individual applications of colour.
  • Coating a paper surface with a suitably selected substance in order to alter the absorption properties of the paper is per se a well-known process.
  • DE published specification No. 35 04 814 thus discloses a process for transfer pattern printing of a textile web, in which paper coated with for instance carboxymethylcellulose is used as a pattern carrier.
  • DE accepted published specification No. 27 01 392 also discloses a process for transfer pattern printing of a textile material. Paper is used as a pattern carrier in this process, said paper being coated with carboxymethylcellulose and the dye being transferred from the pattern carrier to the textile by means of heat and/or pressure.
  • carboxymethylcellulose As the substance with which a paper surface is coated.
  • a pattern carrier of a lightly absorbing, preferably coated paper is thus used, the coating or application being made with carboxymethylcellulose, an alginate or an aqueous dispersion of polyethylene or polyacrylate, preferably carboxymethylcellulose which is an easily accessible substance with advantageous properties.
  • carboxymethylcellulose is per se not sufficient to provide standard-absorbing crude paper with the desired absorption properties.
  • the transfer paper according to the Japanese publication must be coated twice, the lower coating consisting of an aqueous solution of the cellulose derivative alone and the upper coating consisting of the same solution to which the chosen saccharide has been added.
  • a water-resistant layer is subsequently applied on top of said layers, said water-resistant layer according to the examples being a 30% acetone solution of acetyl cellulose.
  • This known transfer paper is thus considerably more complicated than the coated paper according to the present inven- tion and is used for a completely different purpose.
  • the invention relates therefore to a pattern carrier in form of a paper web with a colour pattern printed thereon to be used in transfer pattern printing of a moist textile web by a compressing of the two webs between one or more pairs of rollers without the use of heat, but under such a linear pressure that the textile web is subjected over a short length to a compressing into a reduced thickness followed by a natural expan- sion, whereby the colour pattern is absorbed from the pattern carrier into the textile web
  • the pattern carrier according to the invention is characterised in that it is made of paper with an air permeability (Bendtsen-porosity) of more than 500 ml/min, measured according to the standard DIN 53120 Tl, and a water absorption corresponding to a Cobb-number measured according to the standard SCAN-P12:64, Cobb 60 , of at least 50, said paper being coated with an aqueous dispersion of carboxymethylcellulose containing a non-crystalline saccharide syrup, preferably in an amount of approximately 30
  • the ingredient of the dispersion providing the paper web with surprising and useful properties is a non-crystalline saccharide syrup, which is preferably a sorbitol syrup.
  • a non-crystalline saccharide syrup which is preferably a sorbitol syrup.
  • the invention also relates to the use of a non-crystallizing saccharide syrup as an ingredient in an aqueous dispersion for coating a paper web in order to obtain a pattern carrier with a surface which can drain off immediately the moistness deriving from the printing dye while said dye remains on the surface together with the carboxymethylcellulose.
  • the invention presents several obvious advantages. First of all the choice of paper for the pattern carrier is far less critical than previously because it is possible to use ordinary standard-absorbing crude paper which is considerably less expensive than the paper hitherto used. Moreover, the coated paper according to the invention facilitates the printing thereon of the colour pattern. No skilled work is involved and accordingly no particular training of the employees is required, whereby the printing of the colour pattern on the coated paper to a far higher degree than previously can be carried out locally.
  • the consumption of dye is of the same magnitude as the consumption related to the hitherto used paper, but the wastage rate is significantly lower than previously especially in connection with transfer printing on cellulose fibres and other natural fibres.
  • the ready printed paper can be used in the same manner as previously, viz.
  • the selected crude paper is coated in a covering layer with the aqueous dispersion of carboxymethylcellulose comprising the non-crystalline saccharide syrup, preferably in an amount of approximately 30 g of dispersion per m 2 of paper surface.
  • a typical dispersion presents the following composition (by weight):
  • the paper is coated on the printing side thereof by means of a screen roller. It is also possible to carry out the coating "on-line" in the same cycle of operations on the paper producing machine when the crude paper is produced.
  • the coated paper is subsequently subjected to a printing by passing a number of printing screens (A,B, C,D, ...), cf. the Figure, whereby the desired colour pattern is printed thereon by means of a screen for each colour.
  • the particular nature of the coating implies that the applied colour dries up immediately with the result that the paper can be ad- vanced directly from one screen to the next screen without requiring intermediate drying or freezing.
  • the printing is usually carried out at a paper rate of 60-80 m per minute, ie about 1 m/sec.
  • the printing of the paper proceeds without any problems, as the surface dries up and the colour solidifies so quickly (within less than one second) that the paper surface immediately after passing screen A and long before passing screen B is completely dry etc.
  • the desired colour pattern has been obtained after passing the last printing screen (D on the Figure)
  • the printed paper is subjected to a final drying and then wound up on a roller.
  • the transfer printing per se on a textile web is carried out in a manner known per se by said textile web after moistening thereof in an alkaline bath and a controlled compressing so as to obtain a specific moistness being joined with the printed paper web between one or more pairs of pressing rollers at a suitably high pressure.
  • the colour printed on the textile web is fixed in a manner known per se, and the used pattern carrier is re-circulated so as to allow a reuse of the paper.
  • the saccharide syrup used is preferably based on sorbitol, but other sugars such as glucose, fructose, mannose, galactose, arabinose, xylose, ribose and the like can also be used.
  • a particularly preferred saccharide syrup is the product "Sorbidex 200" from the company Cerestar. This product comprises predominantly sorbitol, but comprises also small amounts of mannitol (approximately 1.1 %) and reducing sugars (approximately 0.1 %).
  • the aqueous dispersion comprises also a carboxymethylcellulose.
  • This carboxymethylcellulose can for instance be “Ambergum ® 1221 ", which is a water-soluble, anionic cellulose polymer from the company Aqualon. This product is also suited as ingredient in the printing colour formulations.
  • the new pattern carrier according to the invention is particularly suited for use in transfer printing on cellulose fibres and other natural fibres by the process according to DK-PS No. 169 135.
  • patterns of any water-soluble or water -dispersible dye such as substative dyes, cationic dyes, chromium-complex dyes, reactive dyes and pigments can be printed on the pattern carrier according to the invention.
  • the reactive dyes are particularly preferred.
  • the pattern carrier according to the invention can be used for printing of dispersion dyes on webs of synthetic fibres.
  • a colour pattern can also be printed on the pattern carrier according to the invention by way of "inkjet" -printing, and a pattern of acid dyes can also be printed thereon.
  • the paper is coated on the printing side with an aqueous dispersion comprising:
  • a two-coloured pattern is applied onto a textile web of cellulose fibres (viscose and cotton).
  • the textile is pre-treated in an ordinary way before the printing: It must be completely clean, and if it tends to roll at the rims it must be glued along said rims.
  • the two colour patterns are printed on the coated paper on a Stork RT printing machine by means of cylindric screens.
  • the two paste recipes are as follows:
  • Reactive dye (Rematrans Rot 358) 100 g
  • Anti-foaming agent (Alcopol o 60%) 1.1 g
  • Reactive dye (Rematrans Blau 257) 200 g
  • Demineralized water up to 1000 g

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Coloring (AREA)
  • Decoration By Transfer Pictures (AREA)
  • Paper (AREA)
  • Paints Or Removers (AREA)
  • Printing Methods (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A pattern carrier for use in transfer pattern printing of textiles comprises paper with an air permeability (Bendtsen-porosity) of more than 500 ml/min and a water absorption corresponding to a Cobb-number of at least 50, said paper being coated with an aqueous dispersion of carboxymethylcellulose containing a non-crystallizing saccharide syrup, preferably in an amount of approximately 30 g of dispersion per m2, whereafter one or more colour patterns are printed on said paper, each colour pattern comprising a water-soluble or dispersible dye admixed an easily soluble thickening carrier with a temporary binding effect, preferably in form of carboxymethylcellulose. The use of a saccharide syrup, preferably a sorbitol syrup, for the coating renders it possible to use standard-absorbing crude paper as the basis of the pattern carrier, which provides obvious financial and production-related advantages.

Description

Title: Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier.
Technical Field
The present invention relates to a pattern carrier in form of a paper web with a colour pattern printed thereon and to be used in transfer pattern printing of a moist textile web. The invention relates also to the use of a saccharide syrup known per se as an ingredient in a dispersion for coating a paper web so as to obtain a pattern carrier with particular properties.
Background Art
Transfer pattern printing is a well-known and extensively used technique, which involves a continuous transfer of a pre-printed pattern from a pattern carrier web to a moist textile web, where the two webs are continuously brought into contact with one another in a transfer region which is frequently in the form of one or more pairs of pressure rollers, cf. the Figure.
In principle various types of the technique have been known since the twenties, but the technique did not become commercially interesting until the late fifties. Various types of transfer printing have been described inter alia in US-PS Nos. 1 651 470 and 1 783 606, FR-PS Nos. 1 034 816 and 1 036 510, DK patent applications Nos. 5666/68 and 1 566/69, SE-PS No. 137 674, GB-PS Nos. 1 430 832 and 1 480 328, US-PS Nos. 1,965,257 and 1,993,524, DE published specification Nos. 2 710 158 and 2 702 300 and US-PS No. 4 057 864. Common to the procedures described in these publications was that it was not possible to obtain acceptable results without involving a heating and/or dyes based on volatile organic solvents. Frequently, useful results required the use of so long contact times that it was in fact not a question of continuous printing processes.
Therefore it was a major breakthrough for the transfer printing when the Applicant in the late eighties succeeded in developing a process for transfer pattern printing whereby it was possible simultaneously to avoid the heating and the use of organic solvents. The process is described in DK-PS No. 169 135 and is characterised by a suitable choice of pattern carrier and dye formulations, an accurate control of the moistening of the textile web and the use of a suitably high pressure, whereby particularly good reproducible results can be obtained at rather high processing speeds and, as mentioned, without the use of heating and exclusively by the use of water-based dye formulations. In addition to the production-related advantages and the particularly good product qualities, the process according to DK-PS No. 169 135 also presented obvious environmental and energy-related advantages as well as a substantially improved working environment.
This epoch-making process is, however, also subject to limitations. To be more precise this process presents particular requirements to the paper used as pattern carrier because said paper must be of a specific nature in order to be coated with a colour pattern at the desired printing speed. It is necessary to use a paper quality which is only slightly absorbing, and in order to avoid that the various, applied colours become blurred it is necessary to strongly cool the paper web between each application of colour in order to solidify the colour.
The printing of the paper is carried out by means of printing screens as shown in the Figure. Thus the process according to DK-PS No. 169 135 necessitates introduction of cooling rollers not shown between the individual printing screens. The coated paper web is carried around these cooling rollers while subjected to a cooling to below -20°C. In this manner it is possible to prevent the colours applied from various printing screens from being blurred. However, this "freezing" does, of course, complicate the entire process significantly and intensifies the costs involved, and accordingly it is desired to provide a pattern carrier where the colours do not become blurred - not even at high printing speeds, and which therefore does not require a cooling between the individual applications of colour.
Coating a paper surface with a suitably selected substance in order to alter the absorption properties of the paper is per se a well-known process. DE published specification No. 35 04 814 thus discloses a process for transfer pattern printing of a textile web, in which paper coated with for instance carboxymethylcellulose is used as a pattern carrier. DE accepted published specification No. 27 01 392 also discloses a process for transfer pattern printing of a textile material. Paper is used as a pattern carrier in this process, said paper being coated with carboxymethylcellulose and the dye being transferred from the pattern carrier to the textile by means of heat and/or pressure.
It is on the whole well-known to use carboxymethylcellulose as the substance with which a paper surface is coated. According to the above DK patent No 169 135 a pattern carrier of a lightly absorbing, preferably coated paper is thus used, the coating or application being made with carboxymethylcellulose, an alginate or an aqueous dispersion of polyethylene or polyacrylate, preferably carboxymethylcellulose which is an easily accessible substance with advantageous properties. However, the carboxymethylcellulose is per se not sufficient to provide standard-absorbing crude paper with the desired absorption properties.
The use of saccharides in the manufacture of transfer paper has hitherto only been described in JP patent application No 44-16135. However, this application relates to a transfer paper for transferring colour patterns to porcelain and ceramics. By adding one or several mono- or oligosaccharides to the water-soluble paste containing a cellulose derivate with which the paper is coated a paper is sought to be obtained which is more easily removed from the porcelain or ceramic object after the pattern has been transferred thereto. Furthermore, by using a transfer paper containing such saccharides, a pattern is obtained which retains its clear outlines after baking of the porcelain or ceramic object. The transfer paper according to the Japanese publication must be coated twice, the lower coating consisting of an aqueous solution of the cellulose derivative alone and the upper coating consisting of the same solution to which the chosen saccharide has been added. A water-resistant layer is subsequently applied on top of said layers, said water-resistant layer according to the examples being a 30% acetone solution of acetyl cellulose. This known transfer paper is thus considerably more complicated than the coated paper according to the present inven- tion and is used for a completely different purpose.
Brief Description of the Invention
It has now surprisingly been found that it is possible to produce such a pattern carrier from standard-absorbing paper by coating said paper with an aqueous dispersion of carboxymethylcellulose containing a non-crystalline saccharide syrup. This coating presents the unexpected feature that it allows an immediate penetration of the moist- ness from the printing dye while the dye concentrate remains on the surface together with the carboxymethylcellulose. As a result the paper surface remains dry and the individual colour patterns do not become blurred. These colour patterns can be easily removed again from the paper during the subsequent transfer printing.
The invention relates therefore to a pattern carrier in form of a paper web with a colour pattern printed thereon to be used in transfer pattern printing of a moist textile web by a compressing of the two webs between one or more pairs of rollers without the use of heat, but under such a linear pressure that the textile web is subjected over a short length to a compressing into a reduced thickness followed by a natural expan- sion, whereby the colour pattern is absorbed from the pattern carrier into the textile web, and the pattern carrier according to the invention is characterised in that it is made of paper with an air permeability (Bendtsen-porosity) of more than 500 ml/min, measured according to the standard DIN 53120 Tl, and a water absorption corresponding to a Cobb-number measured according to the standard SCAN-P12:64, Cobb60, of at least 50, said paper being coated with an aqueous dispersion of carboxymethylcellulose containing a non-crystalline saccharide syrup, preferably in an amount of approximately 30 g of dispersion per m2, whereafter one or more colour patterns are printed on said paper, each colour pattern comprising a water-soluble or dispersible dye admixed an easily soluble thickening carrier with a temporary binding effect, preferably in form of carboxymethylcellulose.
The ingredient of the dispersion providing the paper web with surprising and useful properties is a non-crystalline saccharide syrup, which is preferably a sorbitol syrup. Such products are conventionally used within the food industry, whereas the use thereof for coating ordinary paper is less widely known. The products have thus never been used for coating of ordinary paper which subsequently are used as pattern carriers in connection with transfer printing on textiles.
Therefore the invention also relates to the use of a non-crystallizing saccharide syrup as an ingredient in an aqueous dispersion for coating a paper web in order to obtain a pattern carrier with a surface which can drain off immediately the moistness deriving from the printing dye while said dye remains on the surface together with the carboxymethylcellulose.
The invention presents several obvious advantages. First of all the choice of paper for the pattern carrier is far less critical than previously because it is possible to use ordinary standard-absorbing crude paper which is considerably less expensive than the paper hitherto used. Moreover, the coated paper according to the invention facilitates the printing thereon of the colour pattern. No skilled work is involved and accordingly no particular training of the employees is required, whereby the printing of the colour pattern on the coated paper to a far higher degree than previously can be carried out locally. The consumption of dye is of the same magnitude as the consumption related to the hitherto used paper, but the wastage rate is significantly lower than previously especially in connection with transfer printing on cellulose fibres and other natural fibres. The ready printed paper can be used in the same manner as previously, viz. by the same process and in the same machines as de- scribed in DK-PS No. 169 135. As a result the same advantages as at the process according to DK patent No. 169 135 are obtained, viz. transfer printing on textiles carried out at a high production rate without use of volatile solvents and without heating while using standard-absorbing crude paper as pattern carrier, any form of drying or cooling between each printing screen being rendered superfluous when printing the pattern carrier.
The selected crude paper is coated in a covering layer with the aqueous dispersion of carboxymethylcellulose comprising the non-crystalline saccharide syrup, preferably in an amount of approximately 30 g of dispersion per m2 of paper surface. A typical dispersion presents the following composition (by weight):
68% of water
20% of saccharide syrup
12% of carboxymethylcellulose (dry weight).
It is possible to add a light dye pigment in order to allow a visual evaluation of whether the coating is covering or not.
The paper is coated on the printing side thereof by means of a screen roller. It is also possible to carry out the coating "on-line" in the same cycle of operations on the paper producing machine when the crude paper is produced. The coated paper is subsequently subjected to a printing by passing a number of printing screens (A,B, C,D, ...), cf. the Figure, whereby the desired colour pattern is printed thereon by means of a screen for each colour. The particular nature of the coating implies that the applied colour dries up immediately with the result that the paper can be ad- vanced directly from one screen to the next screen without requiring intermediate drying or freezing. The printing is usually carried out at a paper rate of 60-80 m per minute, ie about 1 m/sec. Even though this rate is fairly high, according to the invention the printing of the paper proceeds without any problems, as the surface dries up and the colour solidifies so quickly (within less than one second) that the paper surface immediately after passing screen A and long before passing screen B is completely dry etc. When the desired colour pattern has been obtained after passing the last printing screen (D on the Figure), the printed paper is subjected to a final drying and then wound up on a roller.
The transfer printing per se on a textile web is carried out in a manner known per se by said textile web after moistening thereof in an alkaline bath and a controlled compressing so as to obtain a specific moistness being joined with the printed paper web between one or more pairs of pressing rollers at a suitably high pressure. Finally, the colour printed on the textile web is fixed in a manner known per se, and the used pattern carrier is re-circulated so as to allow a reuse of the paper.
The saccharide syrup used is preferably based on sorbitol, but other sugars such as glucose, fructose, mannose, galactose, arabinose, xylose, ribose and the like can also be used. A particularly preferred saccharide syrup is the product "Sorbidex 200" from the company Cerestar. This product comprises predominantly sorbitol, but comprises also small amounts of mannitol (approximately 1.1 %) and reducing sugars (approximately 0.1 %).
The aqueous dispersion comprises also a carboxymethylcellulose. This carboxymethylcellulose can for instance be "Ambergum®1221 ", which is a water-soluble, anionic cellulose polymer from the company Aqualon. This product is also suited as ingredient in the printing colour formulations.
The new pattern carrier according to the invention is particularly suited for use in transfer printing on cellulose fibres and other natural fibres by the process according to DK-PS No. 169 135. In principle, patterns of any water-soluble or water -dispersible dye, such as substative dyes, cationic dyes, chromium-complex dyes, reactive dyes and pigments can be printed on the pattern carrier according to the invention. Among these dyes, the reactive dyes are particularly preferred.
In addition, the pattern carrier according to the invention can be used for printing of dispersion dyes on webs of synthetic fibres. A colour pattern can also be printed on the pattern carrier according to the invention by way of "inkjet" -printing, and a pattern of acid dyes can also be printed thereon.
The invention is illustrated in greater detail by means of the following Examples:
EXAMPLES
The following examples involve the use of a machine-glazed base paper of the brand "Transferroto Classico" type 814 from the company Cham Tenero. This paper has a weight of a thousand grains indicated in grammes of 65.0 g/m2, a "Bendtsen-porosity" (air permeability) of 700 ml/min, measured according to the standard DIN 53120 Tl, a water absorption corresponding to a Cobb-number of 55.5 measured according to the standard SCAN-P12:64, Cobb60, a relative wet strength of 9.5% and an ultimate strength of 63.6 N/ 15 mm measured according to the standard DIN EN ISO 1924-2.
The paper is coated on the printing side with an aqueous dispersion comprising:
83.4 kg "Sorbidex 200" and
50.0 kg "Ambergum®1221 " carboxymethylcellulose (CMC)
stirred in 283.6 kg of water. For the toning of the dispersion it is possible to add, if desired, 1.25 kg of the dyes Pigmatex red and Pigmatex yellow (half of each) in order to visualize the coating.
Example 1
A two-coloured pattern is applied onto a textile web of cellulose fibres (viscose and cotton). The textile is pre-treated in an ordinary way before the printing: It must be completely clean, and if it tends to roll at the rims it must be glued along said rims.
The two colour patterns are printed on the coated paper on a Stork RT printing machine by means of cylindric screens. The two paste recipes are as follows:
Recipe 1:
Reactive dye (Rematrans Rot 358) 100 g
Natural thickener (Na-CMC) 120 g
Synthetic thickener (Alcoprint RTA) 6.8 g
Anti-foaming agent (Alcopol o 60%) 1.1 g
Complexing agent (Ladiquest 1097) 11 g Demineralized water up to 1000 g
Recipe 2:
Reactive dye (Rematrans Blau 257) 200 g
Natural thickener (Na-CMC) 120 g
Synthetic thickener (Alcoprint RTA) 6.8 g Anti-foaming agent (Alcopol o 60%) 1.1 g
Complexing agent (Ladiquest 1097) 11 g
Demineralized water up to 1000 g

Claims

The two-coloured pattern is transferred from the paper web to the textile web on a "Cotton Art" standard machine, said textile web being moistened in advance by means of a mixture ofNaOH, 34° Be 50 g/1 Sodium silicate, 36° Be 100 g/1Complexing agent (Ladiquest 1097 1 g/1Demineralized water up to 1 1The fluid absorption in the textile web is approximately 65 % .The dye is fixed on the textile in a manner known per se by way of the "Cold-pad-batch "-process.Example 2The same textile web and the same pretreatment are used as in Example 1.A multicoloured pattern is printed on the coated paper in an "Ink Jet Printer" total width machine (width 140 to 180 cm). Concentrated colours of the brand Rematrans are used in the machine, preferably:Rematrans Gelb 089Goldgelb 070 Orange 035 Rot 004 - Rot 358Blau 267 Blau 257 Tϋrkis 216 Griin 201 Schwarz 288 Schwarz 263 Schwarz 258The paper with the colour pattern printed thereon is used for transfer printing of the textile web as described in Example 1, whereafter the colour is fixed on the textile as described in Example 1.Example 3A two-coloured pattern is applied onto a textile web of polyamide which has been subjected to an ordinary pretreatment.The two colour patterns are printed on the coated paper on a Stork RT printing machine by means of cylindric screens. The two paste recipes are as follows:Recipe 1:Acid dye (Erionyl Blau) 300 g Natural thickener (Na-CMC) 150 gComplexing agent 10 gDemineralized water up to 1000 gAn adjustment is carried out to pH 8 by means of NaOH.Recipe 2:Acid dye (Erionyl Bordeaux) 400 gNatural thickener (Na-CMC) 100 g Complexing agent 10 gDemineralized water up to 1000 gAn adjustment is carried out to pH 8 by means of NaOH.The two-coloured pattern is transferred from the paper web to the textile web on a "Cotton Art" standard machine, said textile web being moistened in advance in a fluid bath of the following composition:Natural thickener (Na-CMC) 5 gDemineralized water up to 1000 gAn adjustment is carried out by means of an acid/buffer to pH 3.The fluid absorption in the textile web is approximately 45 % .The dye is fixed on the textile by way of the "Cold-pad-batch "-process.Example 4A three-coloured pattern is applied onto a textile web of polyester, which has been subjected to an ordinary pretreatment.The three colour patterns are printed on the coated paper on a Stork RT printing machine by means of cylindric screens. The three paste recipes are as follows:Recipe 1:Teraprint Rot 5 g (dispersion dye) 100 gLyoprint TFA 27 g Lyoprint AP 7 gLyoprint BS Cone. 90 gNaOH 5 gRecipe 2:Teraprint Gelb G (dispersion dye) 100 gLyoprint TFA 27 gLyoprint AP 7 gLyoprint BS Cone. 90 gNaOH 5 gRecipe 3Teraprint Blau 6R (dispersion dye) 100 gLyoprint TFA 27 gLyoprint AP 7 gLyoprint BS Cone. 90 gNaOH 5 gThe colour pattern is transferred from the paper web to the textile web on a Lemaire HTP standard machine for transfer printing. The machine is set at 215° C, and a contact time of 25 sec. is used.Here it is a question of a dry process. The colour has been fixed when the textile leaves the machine. Claims.
1. A pattern carrier in form of a paper web with a colour pattern printed thereon to be used in transfer pattern printing of a moist textile web by a compressing of the two webs between one or more pairs of rollers without the use of heat, but under such a linear pressure that the textile web is subjected over a short length to a compressing into a reduced thickness followed by a natural expansion, whereby the colour pattern is absorbed from the pattern carrier into the textile web, characterised in that the pattern carrier is made of paper with an air permeability (Bendtsen-porosity) of more than 500 ml/min, measured according to the standard DIN 53120 Tl, and a water absorption corresponding to a Cobb-number, measured according to the standard SCAN-P12:64, Cobb60, of at least 50, said paper being coated with an aqueous dispersion of carboxymethylcellulose containing a non-crystalline saccharide syrup, preferably in an amount of approximately 30 g of dispersion per m2, whereafter one or more colour patterns are printed on said paper, each colour pattern comprising a water-soluble or dispersible dye admixed an easily soluble thickening carrier with a temporary binding effect, preferably in form of carboxymethylcellulose.
2. A pattern carrier according to claim 1, characterised in that the saccharide syrup used comprises sorbitol as main ingredient.
3. A pattern carrier according to claim 2, characterised in that the saccharide syrup used in addition to sorbitol comprises small amounts of mannitol and reducing sugars.
4. A pattern carrier according to claim 3, characterised in that the saccharide syrup used represents approximately 20% by weight of the dispersion.
5. The use of a non-crystallizing saccharide syrup as an ingredient in an aqueous dispersion for coating a paper web in order to obtain a pattern carrier with a surface which can drain off immediately the moistness deriving from the printing dye while said dye remains on the surface together with the carboxymethylcellulose.
PCT/DK1999/000436 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier. WO2000012809A1 (en)

Priority Applications (19)

Application Number Priority Date Filing Date Title
PL346304A PL200657B1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
NZ510123A NZ510123A (en) 1998-08-26 1999-08-16 A pattern carrier produced from standard-absorbing paper by coating the paper with carboxymethylcellulose thereby allowing immediate penetration of the dye
SI9930302T SI1125015T1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing
AU51535/99A AU755480B2 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
EP99936441A EP1125015B1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing
DE69906563T DE69906563T2 (en) 1998-08-26 1999-08-16 PATTERN CARRIER FOR TRANSFER PRINTING OF PATTERNS
MXPA01001986A MXPA01001986A (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier.
CA002341728A CA2341728C (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
EA200100279A EA002519B1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
US09/763,687 US6805046B1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
IL14160899A IL141608A0 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
HU0103230A HU226431B1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
AT99936441T ATE236287T1 (en) 1998-08-26 1999-08-16 PATTERN CARRIER FOR TRANSFER PRINTING OF PATTERNS
JP2000567784A JP4317979B2 (en) 1998-08-26 1999-08-16 Use of amorphous sugar syrup in a pattern carrier used for pattern transfer printing and dispersions covering paper webs to obtain this pattern carrier
BRPI9913207-9A BR9913207B1 (en) 1998-08-26 1999-08-16 standard carrier in the form of a continuous sheet of paper with a color pattern printed thereon.
DK99936441T DK1125015T3 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and using a non-crystalline saccharide syrup in a dispersion to coat a paper web to obtain such a pattern carrier
NO20010896A NO20010896L (en) 1998-08-26 2001-02-22 Pattern bearer for use in transfer pattern printing and use of a non-crystalline saccharide syrup in a dispersion for coating a paper web to obtain such pattern bearer
IL141608A IL141608A (en) 1998-08-26 2001-02-22 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier
HK02103020.6A HK1041298B (en) 1998-08-26 2002-04-22 Pattern carrier for use in transfer pattern printing and the use of non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DKPA199801070 1998-08-26
DKPA199801070 1998-08-26

Publications (1)

Publication Number Publication Date
WO2000012809A1 true WO2000012809A1 (en) 2000-03-09

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PCT/DK1999/000436 WO2000012809A1 (en) 1998-08-26 1999-08-16 Pattern carrier for use in transfer pattern printing and the use of a non-crystalline saccharide syrup in a dispersion for coating a paper web so as to obtain such a pattern carrier.

Country Status (30)

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US (1) US6805046B1 (en)
EP (1) EP1125015B1 (en)
JP (1) JP4317979B2 (en)
KR (1) KR100574870B1 (en)
CN (1) CN1138890C (en)
AT (1) ATE236287T1 (en)
AU (1) AU755480B2 (en)
BG (1) BG64961B1 (en)
BR (1) BR9913207B1 (en)
CA (1) CA2341728C (en)
CO (1) CO5100981A1 (en)
DE (1) DE69906563T2 (en)
DK (1) DK1125015T3 (en)
EA (1) EA002519B1 (en)
ES (1) ES2196838T3 (en)
HK (1) HK1041298B (en)
HU (1) HU226431B1 (en)
ID (1) ID29010A (en)
IL (2) IL141608A0 (en)
MX (1) MXPA01001986A (en)
NO (1) NO20010896L (en)
NZ (1) NZ510123A (en)
PL (1) PL200657B1 (en)
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SI (1) SI1125015T1 (en)
TR (1) TR200101263T2 (en)
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WO (1) WO2000012809A1 (en)
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WO2004061200A1 (en) * 2002-12-23 2004-07-22 Kimberly-Clark Worldwide, Inc. Treatment of substrates for improving ink adhesion to the substrates
EP2418090A3 (en) * 2010-08-12 2013-12-25 Transfertex GmbH & Co. Thermodruck KG Transfer paper with a coating for ink jet printing for sublimation transfer printing
JP2016141920A (en) * 2015-02-05 2016-08-08 三菱製紙株式会社 Printing paper used for paper printing method
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CN100344830C (en) * 2006-05-16 2007-10-24 上海迪纺纺织科技有限公司 Pigment release agent for cold transfer printing paper
CN101939376B (en) 2008-02-08 2014-03-19 旭化成化学株式会社 Thermoplastic elastomer composition and method for producing the same
JP5681486B2 (en) 2008-04-14 2015-03-11 旭化成ケミカルズ株式会社 Adhesive composition
WO2010067564A1 (en) 2008-12-10 2010-06-17 旭化成ケミカルズ株式会社 Thermoplastic elastomer composition
CN102259472A (en) * 2011-04-26 2011-11-30 绍兴原色数码科技有限公司 Liquid tansfer printing machine
DK177321B1 (en) * 2011-05-10 2013-01-02 Skandinavisk HTP ApS Paper for transfer pattern printing
CN102220709A (en) * 2011-05-12 2011-10-19 王天友 Multi-color-pattern positioning heat transfer fabric, processing technology and equipment thereof
US8640546B2 (en) * 2011-09-12 2014-02-04 Del Monte Corporation Sensor for high pressure processing of articles
JP6239539B2 (en) * 2015-02-05 2017-11-29 三菱製紙株式会社 Printing paper used for paper printing
CN107921804A (en) 2015-06-12 2018-04-17 科尔登霍夫路浩有限公司 Transfer paper for the improvement of ink jet printing
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WO2021101860A1 (en) * 2019-11-22 2021-05-27 Sun Chemical Corporation Water-based printing ink compositions

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PT1125015E (en) 2003-08-29
JP2002523271A (en) 2002-07-30
IL141608A (en) 2006-12-31
ID29010A (en) 2001-07-26
EP1125015A1 (en) 2001-08-22
NZ510123A (en) 2002-07-26
DE69906563T2 (en) 2004-02-19
NO20010896L (en) 2001-04-25
BG64961B1 (en) 2006-10-31
YU18001A (en) 2003-07-07
AU755480B2 (en) 2002-12-12
BG105288A (en) 2001-11-30
US6805046B1 (en) 2004-10-19
DE69906563D1 (en) 2003-05-08
EA002519B1 (en) 2002-06-27
IL141608A0 (en) 2002-03-10
TW518381B (en) 2003-01-21
KR20010079670A (en) 2001-08-22
ES2196838T3 (en) 2003-12-16
BR9913207A (en) 2001-05-22
BR9913207B1 (en) 2010-03-23
JP4317979B2 (en) 2009-08-19
HUP0103230A2 (en) 2002-01-28
ZA200101467B (en) 2002-06-28
ATE236287T1 (en) 2003-04-15
CN1138890C (en) 2004-02-18
HK1041298A1 (en) 2002-07-05
EA200100279A1 (en) 2001-08-27
HUP0103230A3 (en) 2005-11-28
CA2341728C (en) 2007-11-27
DK1125015T3 (en) 2003-07-28
EP1125015B1 (en) 2003-04-02
CN1324418A (en) 2001-11-28
PL200657B1 (en) 2009-01-30
NO20010896D0 (en) 2001-02-22
AU5153599A (en) 2000-03-21
HU226431B1 (en) 2008-12-29
CA2341728A1 (en) 2000-03-09
TR200101263T2 (en) 2002-07-22
SI1125015T1 (en) 2003-10-31
HK1041298B (en) 2004-12-17
PL346304A1 (en) 2002-01-28
MXPA01001986A (en) 2002-04-24
KR100574870B1 (en) 2006-04-27

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