EP0856078B1 - Procede de teinture d'un substrat textile dans au moins un fluide surcritique - Google Patents

Procede de teinture d'un substrat textile dans au moins un fluide surcritique Download PDF

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Publication number
EP0856078B1
EP0856078B1 EP96934333A EP96934333A EP0856078B1 EP 0856078 B1 EP0856078 B1 EP 0856078B1 EP 96934333 A EP96934333 A EP 96934333A EP 96934333 A EP96934333 A EP 96934333A EP 0856078 B1 EP0856078 B1 EP 0856078B1
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EP
European Patent Office
Prior art keywords
dye
supercritical fluid
dispersion
supercritical
bulk
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP96934333A
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German (de)
English (en)
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EP0856078A1 (fr
Inventor
Rudolf Eggers
Joachim Von Schnitzler
Gottlob Wörner
Richard Huber
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.)
Amann and Soehne GmbH and Co KG
Original Assignee
Amann and Soehne GmbH and Co KG
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Publication date
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Publication of EP0856078A1 publication Critical patent/EP0856078A1/fr
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Publication of EP0856078B1 publication Critical patent/EP0856078B1/fr
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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
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34—Material containing ester groups
    • D06P3/52—Polyesters
    • D06P3/54—Polyesters using dispersed dyestuffs
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
    • 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
    • D06P1/94—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 dyes dissolved in solvents which are in the supercritical state
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
    • D06B23/205—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation for adding or mixing constituents of the treating material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/92—Synthetic fiber dyeing
    • Y10S8/922—Polyester fiber

Definitions

  • the present invention relates to a method for dyeing of a textile substrate in at least one supercritical one Fluid, preferably for dyeing spools of thread in supercritical carbon dioxide, with the characteristics of the generic term of claim 1.
  • Textile substrates are still used in practice today colored in the aqueous system, for this purpose each textile substrate to be dyed arranged in an autoclave and there with the watery, at least one Dye-containing liquor flowed through or through becomes.
  • this dye liquor is usually used made that a concentrated aqueous dye solution or dye dispersion from the solid dye initially is created using this concentrated dye solution or dye dispersion with that in the autoclave Fleet is successively diluted.
  • the direct use of solid dye bypassing the previously described concentrated dye solution or dye dispersion is not possible as this inevitably leads to training of color spots as a result of undissolved or. undispersed Lead dyes on the textile substrate would.
  • WO 93/14259 A names light stabilizers for such a substance, Plasticizers, water repellents, Sizing, finishing agents, preparations, flame retardants, pharmaceutical Active ingredients, antistatic agents, anti-pest agents, Bactericides, bacteriostatics, perfumes, adhesives, flavor or fragrances, while DE 42 37 823 A mainly on directed the production of a dye freed from additives with which a corresponding textile Substrate is colored in supercritical fluids.
  • the present invention is based on the object Process for dyeing a textile substrate in at least a supercritical fluid of the type specified with which the respective textile substrate to be dyed can be dyed particularly safely and without interference.
  • the method according to the invention for dyeing a textile substrate in at least one supercritical fluid preferably for dyeing bobbins in supercritical carbon dioxide before placing the textile substrate in an autoclave and there with the at least one dye flows on or through supercritical fluid.
  • the supercritical so mixed with the dispersed dye Fluid is filtered through in the process according to the invention a filter whose pore size is less than or equal to 30 ⁇ m.
  • the method according to the invention such a dispersion of the dye in the supercritical Fluid used that has no dye dispersgate or multimolecular dye agglomerates whose size is 30 ⁇ m. This is done, as already stated above is achieved in the method according to the invention in that the supercritical mixed with the dispersed dye Fluid before and / or during staining through a filter filtered, the pore size is less than or equal to 30 microns.
  • the method according to the invention has a number of advantages on. It was surprisingly found that incorrect coloring, in particular by the method according to the invention the previously described color spots or uneven Discolorations, which is attributed to that only in the supercritical dyeing liquor multimolecular dye agglomerates the aforementioned maximum particle size available. This also leads to the fact that Process according to the invention with a high reproducibility color loss, i.e. both in terms of color depth as well as the color tone. They are too created using the inventive method Color fastness, especially wet fastness, such as the perspiration fastness, the fastness to rubbing, the water and / or fastness to washing, excellent.
  • Another embodiment of the method according to the invention provides that the dye fill with inert particles, especially with glass and / or steel balls, provides so that in this embodiment of the invention Procedure from the outset the risk of clumping of the dye to be dispersed is prevented, since the dye particles to be dispersed are then largely not in contact with each other, but in the gaps, which exist between the inert particles are, which in turn is the previously mentioned Reduction in the dispersing time of the dye to be dispersed is understandable becomes. In addition, the flow conditions uniform.
  • the inert particles of the method according to the invention so that their geometric shape and / or their Mass of the geometric shape and / or mass of each used dyes corresponds, so by this measure it is ensured that the fluid flows through none of the dye bed mixed with inert particles Separation of dyes and inert particles brings about.
  • a further acceleration of the dispersing process of the at least one dye in the supercritical fluid used in each case is achieved in another embodiment of the process according to the invention by providing granules of the at least one dye in the fluidized bed and / or the fixed bed described above. It was found here that a particularly great acceleration of the dispersing of the at least one dye results in the process according to the invention if granular dye material is selected which has an average particle diameter between 0.5 mm and 5 mm, preferably between 1.5 mm and 3 mm.
  • Dye bed opened up as a fluidized bed so can then a particularly reproducible dispersion of the at least a dye or the at least one dye granulate thereby brought about within a very short time be that the dye or the dye granules with a minimal fluidization rate between 0.02 m / s and 0.12 m / s, preferably between 0.04 m / s and 0.06 m / s, swirled in the fluidized bed.
  • Another embodiment of the method according to the invention provides that to disperse the at least one Dye forms the bed of dye as such bed, whose axial length is much greater than their radial dimension and that one for dispersing the at least a dye used in supercritical fluid directs axial direction through the bulk material. This leads to an optimized mass transfer and further reduces the dispersion time required in each case.
  • Dye fill in particular cylindrical or cylindrical is formed, such a fill of dye from, the axial length of two to ten times, preferably four to seven times larger than their radial dimension.
  • Another embodiment of the method according to the invention provides that the at least one to be dispersed Dye in a chambered or channeled one Arranging inert material, whereby the chambers or the channels to the flow direction of the supercritical Fluid aligns that these chambers or channels from the flow through supercritical fluid.
  • the dye as a fixed bed in the previously described specially designed inert material so that then when flowing through the chambers or channels at least one dye from the supercritical arranged therein Fluid is dispersed.
  • Embodiment of the method according to the invention provides the inert material with honeycomb-like chambers or channels, which enables the greatest possible concentration of the dye to be dispersed on a relative small area can be arranged without this to undesirable clumping or sintering of the material to be dispersed Dye can come.
  • Embodiments of the invention have been described above Processes described in which the at least to be dispersed opens up a dye as a bed of dye.
  • a fundamentally different solution of the method according to the invention provides that the at least one to be dispersed Dye as a dye melt and / or as a dye dispersion in the supercritical fluid injected so as to disperse the at least previously described produce a dye in the supercritical fluid, this dispersion then the multimolecular dye, but none Contains dye agglomerates, their average particle size is larger than 30 ⁇ m, preferably larger than 15 ⁇ m.
  • the ones described below Developments of the method according to the invention are not fixed Dye but a liquid dye with each brought into contact to use supercritical fluid. To ensure that the liquid formulation of each in to achieve the supercritical fluid to be dispersed, there are several options.
  • the at least one liquid dye, which as Dye melt is present in the respective by means of a nozzle used supercritical fluid, such allows Working method a particularly precise addition of the required Amount of dye, which in turn is reproducible that according to the inventive method expresses created coloring.
  • the inventive method expresses created coloring.
  • the amount of dye to be dispersed on the Dispersibility of the supercritical fluid for each used dye via an adjustable time-quantity control vote so that in no time a dispersion of the dye in the supercritical fluid arises.
  • this Dispersion then dye agglomerates of a maximum size of less than 30 ⁇ m, preferably of a maximum Has a size of less than 15 ⁇ m, sees further training of the inventive method before that supercritical fluid provided with the dispersed dye filtered through a filter before it is dyed supercritical fluid then with the textile to be dyed Comes into contact with the substrate.
  • the dyeing autoclave 1 has a first circulation system provided, the first circulation system corresponding piping system 2 includes. Within this Pipe system 2 of the first circulation system a circulation pump 3 is arranged.
  • the piping system 2 has a not shown Feed for carbon dioxide and a heat exchanger (also not shown).
  • the in 1 schematically shown a second plant Circulation system, which is designated overall by 11, available.
  • valves 4 and 7 of the bypass are opened, so that the supercritical carbon dioxide through the Ink set pot 5 flows and there still listed below Marine dye dispersed. At this time the valve 6 closed.
  • the autoclave 12 is filled with a silica gel, type Trysil.
  • This silica gel has a particle size between 2 mm and 8 mm, a density of 2,200 kg / m 3 , a bulk density of 550 kg / m 3 , a porosity of 0.55, an inner surface of approx. 450 m 2 / g, a pore volume of 0.4 cm 3 / g, an average pore diameter between 4 nm and 10 nm and a tortuosity factor of 5.0.
  • the first embodiment of the Paint batch pot 5 is a fluidized bed paint batch pot 5 formed, this paint approach pot an inner has cylindrical container 10, the top and is closed on the foot side with a sintered metal plate 9, wherein the sintered metal plates 9 are designed as filters and have a maximum pore size of 30 ⁇ m.
  • the second embodiment of the paint batch pot shown in FIG. 3 5 has a cylindrical container 15, wherein the cylindrical container 15 at a distance from the inner wall of the paint batch pot 5 is arranged. in this connection the cylindrical container 15 takes the one to be dispersed Dye 13 in the form of a fixed bed.
  • the flowing into the cylindrical container 15 supercritical carbon dioxide flows through the inside of the Container 15 arranged as a fixed bed dye 13 radially to the outside, so that the supercritical provided with dye Fluid in the direction of arrow 12 leaves the ink set pot 5.
  • the third embodiment of the Paint batch pot 5 is a fluidized bed paint batch pot 5 formed, this paint approach pot an inner has cylindrical container 10, the top and is closed on the foot side with a sintered metal plate 9, wherein the sintered metal plates 9 are designed as filters and have a maximum pore size of 30 ⁇ m.
  • the disperse dye 13 is inside the container 10 arranged such that this disperse dye 13 by the supercritical flowing into the paint batch pot 5 Fluid (flow direction 11) is swirled. That with the dispersed dye provided supercritical fluid leaves then in the direction of arrow 12 the ink set pot 5.
  • the color approach pot 5 shown in Figure 4 four, evenly distributed over the circumference of the paint set pot Outlet connector 30 on.
  • the ratio of the axial Length of the container 10 to its diameter is the embodiment 1: 2.5 shown in FIG. 4.
  • the paint approach pot 5 shown in Figure 4 has a jacket heater 31 on.
  • the ink set pot 5 shown in Figure 2 is in the following described dyeing test 2 and the one shown in FIG. 3 Color approach pot 5 is in the following described coloring test 3 used.
  • the navy blue disperse dye used was a pure dye, i.e. he showed no means of positioning or other Additions on.
  • the dye was on the bottom arranged in a cotton sack inside the dye autoclave, so that the dye in this experiment 1 not undesirably discharged from the autoclave could.
  • the bobbins dyed after dyeing tests 2 and 3 were all colored no matter what, in the case of color loss (color tone and color depth) about the axial lengths and the radial dimensions no difference can be found in the colored coils could.
  • the measured wet fastness properties (fastness to rubbing, fastness to washing, Water fastness and perspiration fastness) after the dyeing test 1 created coloring were between 1 and 2 and were therefore unacceptable, while the aforementioned fastness properties the dyeings made after dyeing tests 2 and 3 were between 4 and 5 and therefore very good are.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Coloring (AREA)

Claims (20)

  1. Procédé de teinture d'un substrat textile dans au moins un fluide supercritique, dans lequel on dispose le substrat textile dans un autoclave et on l'y expose à un afflux ou à une traversée du fluide supercritique comprenant au moins un colorant, dans lequel on met en contact ledit au moins un colorant sous forme de charge, sous forme de masse fondue et / ou sous forme de dispersion avec le fluide supercritique avec formation d'une dispersion du colorant dans le fluide supercritique, caractérisé en ce que l'on filtre le fluide supercritique mélangé avec le colorant dispersé à travers un filtre dont la taille des pores est inférieure ou égale à 30 µm.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on filtre le fluide supercritique mélangé avec le colorant dispersé à travers un filtre dont la taille des pores est inférieure ou égale à 15 µm.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on présente la charge de colorant comme un lit fluidisé et / ou comme un lit fixe submergé ou traversé par le fluide supercritique.
  4. Procédé selon la revendication 3, caractérisé en ce que l'on prévoit des particules inertes dans la charge de colorant.
  5. Procédé selon la revendication 4, caractérisé en ce que la charge de colorant est constituée des particules inertes enrobées d'au moins un colorant.
  6. Procédé selon une des revendications précédentes, caractérisé en ce que l'on prévoit dans le lit fluidisé et / ou le lit fixe un granulat dudit au moins un colorant.
  7. Procédé selon la revendication 6, caractérisé en ce que l'on sélectionne comme granulat un granulat de colorant qui présente un diamètre moyen de particule entre 0,5 mm et 5 mm, de préférence entre 1,5 mm et 3 mm.
  8. Procédé selon une des revendications précédentes, caractérisé en ce que l'on fait tourbillonner le colorant ou le granulat de colorant à une vitesse de fluidisation minimale entre 0,02 m/s et 0,12 m/s, de préférence entre 0,04 m/s et 0,06 m/s dans le lit fluidisé.
  9. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on conforme la charge de colorant comme une charge dont la longueur axiale est nettement plus grande que sa dimension radiale et que l'on guide le fluide supercritique à travers la matière en vrac de manière essentiellement axiale.
  10. Procédé selon la revendication 9, caractérisé en ce que l'on choisit une charge de colorant dont la longueur axiale est deux à dix fois, de préférence quatre à sept fois, plus grande que sa dimension radiale.
  11. Procédé selon une des revendications 1 à 8, caractérisé en ce que l'on dispose ledit au moins un colorant dans un matériau inerte pourvu de chambres ou de canaux de telle manière que l'on verse ledit au moins un colorant dans les chambres ou les canaux et que l'on oriente le matériau inerte par rapport au sens du courant du fluide supercritique de telle manière que les chambres ou les canaux sont traversés par le fluide supercritique.
  12. Procédé selon la revendication 11, caractérisé en ce que le matériau inerte est pourvu de chambres ou de canaux à alvéoles.
  13. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on injecte ledit au moins un colorant sous forme de masse fondue et / ou de dispersion dans le fluide supercritique.
  14. Procédé selon la revendication 13, caractérisé en ce que l'on injecte ledit au moins un colorant sous forme de masse fondue, le colorant étant au préalable fondu en présence de gaz inerte.
  15. Procédé selon la revendication 13 ou 14, caractérisé en ce que l'on injecte ledit au moins un colorant au moyen d'un ajutage dans le fluide supercritique.
  16. Procédé selon la revendication 13 à 15, caractérisé en ce que l'on dose la masse fondue de colorant et / ou la dispersion de colorant dans le fluide critique utilisé concerné par l'intermédiaire d'une zone de mélange parcourue par le fluide supercritique.
  17. Procédé selon une des revendications 13, 15, ou 16, caractérisé en ce que l'on utilise de l'acétone, du chloroforme, du diméthylformamide, de l'éthylène glycol, du propylène glycol, une huile et / ou un alcool inférieur, en particulier de l'éthanol, du propanol-2, du propanol-1, du butanol-1 et / ou du butanol-2 comme moyen de dispersion pour la production de la dispersion de colorant.
  18. Procédé selon la revendication 15, caractérisé en ce que l'on injecte une dispersion de colorant, de préférence une dispersion de colorant aqueuse, dans le fluide supercritique.
  19. Procédé selon une des revendications précédentes, caractérisé en ce que l'on choisit comme substrat textile à teinter une bobine X d'un fil à coudre en fibres polyester.
  20. Procédé selon une des revendications précédentes, caractérisé en ce que l'on choisit comme fluide supercritique un dioxyde de carbone supercritique et au moins comme colorant un colorant de dispersion.
EP96934333A 1995-10-17 1996-08-05 Procede de teinture d'un substrat textile dans au moins un fluide surcritique Expired - Lifetime EP0856078B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19540227 1995-10-17
DE19540227 1995-10-17
PCT/DE1996/001456 WO1997014843A1 (fr) 1995-10-17 1996-08-05 Procede de teinture d'un substrat textile dans au moins un fluide surcritique

Publications (2)

Publication Number Publication Date
EP0856078A1 EP0856078A1 (fr) 1998-08-05
EP0856078B1 true EP0856078B1 (fr) 2002-07-31

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EP96934333A Expired - Lifetime EP0856078B1 (fr) 1995-10-17 1996-08-05 Procede de teinture d'un substrat textile dans au moins un fluide surcritique

Country Status (6)

Country Link
US (1) US5958085A (fr)
EP (1) EP0856078B1 (fr)
AT (1) ATE221592T1 (fr)
DE (2) DE59609515D1 (fr)
ES (1) ES2179951T3 (fr)
WO (1) WO1997014843A1 (fr)

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CN105926210B (zh) * 2016-05-27 2018-07-13 南通纺织丝绸产业技术研究院 一种超临界流体无水染整的一种移动式染杯
CN105926220B (zh) * 2016-05-27 2018-05-04 南通纺织丝绸产业技术研究院 一种超临界流体无水染整的打样染杯
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TW202001038A (zh) * 2018-06-21 2020-01-01 遠東新世紀股份有限公司 含有殘留寡聚物之織物基材的染色方法
CN114606692B (zh) * 2022-03-25 2022-12-06 东华大学 提高超临界二氧化碳流体中染化料的溶解度和溶解速率的方法
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EP0514337B1 (fr) * 1991-05-17 1995-11-22 Ciba-Geigy Ag Procédé de teinture de matériaux textile avec des colorants dispersés dans du CO2 supercritique
EP0543779A1 (fr) * 1991-11-20 1993-05-26 Ciba-Geigy Ag Procédé d'azurage optique de matériau textile hydrophobe avec des azurants optiques dispersés dans du CO2 supercritique
DE4200352A1 (de) * 1992-01-09 1993-08-19 Deutsches Textilforschzentrum Verfahren zum aufbringen von substanzen auf fasermaterialien und textile substrate
DE4237823A1 (de) * 1992-10-08 1994-04-14 Amann & Soehne Verfahren zum Färben eines Substrates in einem überkritischen Fluid
DE4238622C2 (de) * 1992-11-16 2002-10-24 Amann & Soehne Vorrichtung zur Behandlung von textilen Gütern
DE4238621C2 (de) * 1992-11-16 2002-10-24 Amann & Soehne Vorrichtung zur Behandlung von textilen Gütern
US5340614A (en) * 1993-02-11 1994-08-23 Minnesota Mining And Manufacturing Company Methods of polymer impregnation

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DE19631604A1 (de) 1997-04-24
ATE221592T1 (de) 2002-08-15
ES2179951T3 (es) 2003-02-01
WO1997014843A1 (fr) 1997-04-24
DE59609515D1 (de) 2002-09-05
EP0856078A1 (fr) 1998-08-05
US5958085A (en) 1999-09-28

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