EP0514337B1 - Procédé de teinture de matériaux textile avec des colorants dispersés dans du CO2 supercritique - Google Patents

Procédé de teinture de matériaux textile avec des colorants dispersés dans du CO2 supercritique Download PDF

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Publication number
EP0514337B1
EP0514337B1 EP92810343A EP92810343A EP0514337B1 EP 0514337 B1 EP0514337 B1 EP 0514337B1 EP 92810343 A EP92810343 A EP 92810343A EP 92810343 A EP92810343 A EP 92810343A EP 0514337 B1 EP0514337 B1 EP 0514337B1
Authority
EP
European Patent Office
Prior art keywords
pressure
process according
bar
dyeing
textile material
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
EP92810343A
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German (de)
English (en)
Other versions
EP0514337A1 (fr
Inventor
Wolfgang Saus
Dierk Dr. Knittel
Eckhard Prof. Dr. Schollmeyer
Hans-Jürgen Dr. Buschmann
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.)
Novartis AG
Original Assignee
Ciba Geigy AG
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 Ciba Geigy AG filed Critical Ciba Geigy AG
Publication of EP0514337A1 publication Critical patent/EP0514337A1/fr
Application granted granted Critical
Publication of EP0514337B1 publication Critical patent/EP0514337B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/94General 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/10Processes in which the treating agent is dissolved or dispersed in organic solvents; Processes for the recovery of organic solvents thereof
    • D06M23/105Processes in which the solvent is in a supercritical state
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/0004General aspects of dyeing
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/90General 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 organic solvents or aqueous emulsions thereof
    • D06P1/92General 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 organic solvents or aqueous emulsions thereof in organic solvents
    • D06P1/928Solvents other than hydrocarbons
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34Material containing ester groups
    • D06P3/52Polyesters
    • D06P3/54Polyesters using dispersed dyestuffs
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/92Synthetic fiber dyeing
    • Y10S8/922Polyester fiber

Definitions

  • the present invention relates to a method for dyeing from supercritical CO2.
  • the object of the present invention was to improve this known method. This object is achieved by the method according to the invention.
  • the present invention thus relates to a process for dyeing hydrophobic textile material with disperse dyes by heating the textile material and the disperse dye in supercritical carbon dioxide at a pressure of 73 to 400 bar to a temperature of 80 to 300 ° C and then the pressure and the temperature lowered to below the critical pressure and the critical temperature, characterized in that the pressure reduction is carried out in several stages and the pressure in each stage is reduced by 0.1 to 20 bar and after each stage is waited until a practically constant pressure has stopped.
  • the dyeing of textile substrates from supercritical CO2 has a number of advantages over dyeing processes from an aqueous liquor. Due to the fact that the CO2 used does not get into the wastewater, but is preferably used again after dyeing, no wastewater pollution occurs. Furthermore, the dyeing of supercritical CO2 required for dyeing the textile substrate Mass transfer processes take place much faster compared to aqueous systems. This in turn means that the textile substrate to be dyed can be flowed through particularly well and quickly. When using dyeing from supercritical CO2, there are no irregularities with regard to the flow through the winding body during the coloring of winding bodies, which are to be regarded as causes for edge runs or length runs, for example, in the conventional method for tree coloring of flat structures.
  • no disperse dyes can undesirably agglomerate, as is sometimes the case with conventional dispersion dyeings, so that the use of dyeing from supercritical CO2 avoids the brightening of disperse dyes known in conventional dyeing processes in aqueous systems, and thus the formation of corresponding stains.
  • Another advantage of dyeing from supercritical CO2 is that you can use disperse dyes that consist exclusively of the actual dye and do not contain the usual dispersants and agents. For many dyes, there is also no need to grind the dyes.
  • supercritical CO2 means CO2 in which the pressure and the temperature of the CO2 are above the critical pressure and the critical temperature.
  • the supercritical CO2 has approximately the viscosity of the corresponding gas and a density that is approximately comparable with the density of the correspondingly liquefied gas.
  • the dyeing process according to the invention is carried out, for example, in such a way that the textile material to be dyed is placed together with the disperse dye in a pressure-resistant dyeing apparatus and heated to the dyeing temperature under CO2 pressure or by heating and then adjusting the desired CO2 pressure.
  • the dyeing temperature used in the process according to the invention depends essentially on the substrate to be dyed. Usually it is between about 80 and 300 ° C, preferably between about 100 and 150 ° C.
  • the pressure to be applied must be at least so high that the CO2 is in a supercritical state. The higher the pressure, the greater the solubility of the dyes in CO2 in general, but the greater the expenditure on equipment.
  • the pressure is preferably between about 73 and 400 bar, in particular between about 150 and 250 bar. At the preferred dyeing temperature for polyester material of approximately 130 ° C., the pressure is approximately 200 bar.
  • the liquor ratio (mass ratio of textile material: CO2) when dyeing by the process according to the invention depends on the goods to be treated and their presentation.
  • polyester yarns which are wound onto corresponding packages are to be dyed using the process according to the invention, this is preferably done with relatively short liquor ratios, i.e. Fleet ratios between 1: 2 to 1: 5.
  • Such short liquor ratios generally cause difficulties in the conventional dyeing process in the aqueous system, since there is often the risk that the finely dispersed systems agglomerate due to the high dye concentration. However, this does not occur in the method according to the invention.
  • the desired pressure is set, if this has not already been reached due to the temperature increase.
  • the temperature and pressure are then kept for some time, e.g. Kept constant for 1 to 60 minutes, taking suitable measures, e.g. Stirring or shaking, or above all by circulation of the "dye liquor" ensures intensive mixing of the textile material and "dye liquor".
  • the length of time is generally not critical, but it has been shown that times of more than 10 minutes usually do not improve the dyeing yield.
  • the pressure is then reduced in several stages, preferably in 2 to 100 stages, which is done most simply by opening a valve and releasing a portion of CO2.
  • the rapid expansion results in cooling, that is, it is quasi-adiabatically expanded.
  • the density of the CO2 is changed by lowering the pressure. After closing the valve, heating to the Ambient temperature instead, the pressure rises isochorically again. After approx. 30 seconds to a few minutes, when the pressure and temperature practically no longer rise, the pressure is reduced again and the process described above is repeated.
  • This mode of operation is preferably controlled automatically by a pressure and / or density and / or temperature program.
  • the pressure in each stage is preferably reduced by 1 to 10 bar and especially by 2 to 5 bar.
  • the textile material is then removed from the dyeing machine and can often be used without further cleaning. In particular, it should be noted that no drying is required.
  • the CO2 can then be collected and used again after coloring to the supercritical state for the coloring of other substrates.
  • the dyes separate out as liquid or solid dyes, which can be collected accordingly and used for further dyeings.
  • the method according to the invention is suitable for dyeing semi-synthetic and in particular synthetic hydrophobic fiber materials, especially textile materials.
  • Textile materials from blended fabrics which contain such semi-synthetic or synthetic hydrophobic textile materials can also be dyed by the process according to the invention.
  • Cellulose-21 ⁇ 2-acetate and cellulose triacetate are particularly suitable as semi-synthetic textile materials.
  • Synthetic hydrophobic textile materials consist primarily of linear, aromatic polyesters, for example those made of terephthalic acid and glycols, especially ethylene glycol or condensation products made of terephthalic acid and 1,4-bis (hydroxymethyl) cyclohexane; from polycarbonates, e.g. from ⁇ , ⁇ -dimethyl-4,4'-dihydroxy-diphenylmethane and phosgene, from fibers based on polyvinyl chloride, polypropylene or polyamide, e.g. Polyamide 6.6, polamide 6.10, polyamide 6, polyamide 11 or poly (1,4-phenylene terephthalamide).
  • Microfilament fibers made of polyester e.g. Color polyethylene terephthalate with very good levelness.
  • Suitable dyes for the process according to the invention are, above all, dispersion dyes, i.e. dyes which are sparingly soluble or almost insoluble in water.
  • dyes from the following classes are possible: Nitro dyes, for example nitrodiphenylamine dyes, methine dyes, quinoline dyes, amino naphthoquinone dyes, coumarin dyes and in particular anthraquinone dyes, tricyanovinyl dyes and azo dyes such as monoazo and disazo dyes.
  • Nitro dyes for example nitrodiphenylamine dyes, methine dyes, quinoline dyes, amino naphthoquinone dyes, coumarin dyes and in particular anthraquinone dyes, tricyanovinyl dyes and azo dyes such as monoazo and disazo dyes.
  • a strip of polyester fabric and 1.5% by weight, based on the polyester fabric, of the dye of the formula are placed in an autoclave
  • the autoclave is flushed with CO2 gas and heated to 130 ° C under 10 bar CO2 pressure at a heating rate of 2 ° C per minute, the stirrer running at approx. 100 revolutions per minute. Then the pressure is increased to 250 bar within 1.5 to 2.5 minutes and the stirrer speed is increased to about 700 revolutions per minute.
  • the pressure is reduced by 5 bar within 5 to 15 seconds by releasing CO2, the temperature in the autoclave falling by about 2 ° C. After closing the valve, the pressure rises again by about 2 bar within the next minute and the temperature returns to the original value.
  • the pressure is again reduced by 7 bar within 5 to 15 seconds by releasing CO2, the valve is closed and the system waits for 1 minute to set a constant temperature and pressure. This process is repeated until the pressure has dropped to 180 bar. (approx. 15 minutes) The residual pressure in the autoclave is then released and the polyester fabric is removed from the hot autoclave.
  • a red-dyed polyester fabric of similar quality to that obtained by dyeing by customary methods from an aqueous liquor is obtained.
  • Example 1 If one works as described in Example 1, but after reaching 130 ° C. and a pressure of 250 bar and a stirrer speed of 700 revolutions per minute, these conditions are kept constant for 25 minutes, then the pressure in the autoclave is released within 30 seconds, cools and removes the dyed polyester fabric, the color depth is only approx. 1 10th the color depth obtained in Example 1.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Coloring (AREA)

Claims (12)

  1. Procédé de teinture de matériaux textiles hydrophobes par des colorants dispersés, en chauffant le matériau textile et le colorant dispersé dans le dioxyde de carbone supercritique, à une pression de 73 à 400 bar et à une température de 80 à 300°C et en diminuant ensuite la pression et la température en dessous de la pression critique et de la température critique, caractérisé en ce que l'on effectue la diminution de pression en plusieurs étapes et que, au cours de chaque étape, l'on diminue la pression de 0,1 à 20 bar et que l'on attend après chaque étape, jusqu'à ce qu'une pression pratiquement constante se soit établie.
  2. Procédé selon la revendication 1, caractérisé en ce que l'on effectue la diminution de pression en 2 à 100 étapes.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on diminue la pression au cours de chaque étape de 1 à 10 bar et, de préférence, de 2 à 5 bar.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que l'on diminue la pression par étapes d'une pression entre 200 et 300 bar jusqu'à 100 à 130 bar et que l'on supprime ensuite en une seule étape la pression résiduelle.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que l'on règle la diminution de pression au moyen d'un programme de pression et/ou densité et/ou température.
  6. Procédé selon la revendication 5, caractérisé en ce que l'on règle la diminution de pression de façon que la diminution de la densité se produise sous forme d'étapes constantes.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que l'on utilise un colorant dispersé qui est exempt d'additifs et, en particulier, d'agents de fixation et d'agents de dispersion.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce que l'on chauffe le matériau textile à des températures entre environ 100°C et environ 150°C.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que l'on opère sous une pression comprise entre environ 150 bar et environ 250 bar.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que l'on effectue la teinture du support avec un rapport de bain compris entre environ 1:2 et environ 1:100 et, de préférence, entre environ 1:5 et environ 1:75.
  11. Procédé selon l'une des revendications 1 à 10, caractérisé en ce que l'on utilise à nouveau après teinture le colorant non consommé, en vue d'une nouvelle opération de teinture.
  12. Utilisation du procédé selon l'une des revendications 1 à 11, pour la teinture de matériaux textiles à base de polyester.
EP92810343A 1991-05-17 1992-05-08 Procédé de teinture de matériaux textile avec des colorants dispersés dans du CO2 supercritique Expired - Lifetime EP0514337B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH147591 1991-05-17
CH1475/91 1991-05-17

Publications (2)

Publication Number Publication Date
EP0514337A1 EP0514337A1 (fr) 1992-11-19
EP0514337B1 true EP0514337B1 (fr) 1995-11-22

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EP92810343A Expired - Lifetime EP0514337B1 (fr) 1991-05-17 1992-05-08 Procédé de teinture de matériaux textile avec des colorants dispersés dans du CO2 supercritique

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Country Link
US (1) US5250078A (fr)
EP (1) EP0514337B1 (fr)
JP (1) JPH05132880A (fr)
DE (1) DE59204395D1 (fr)

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Also Published As

Publication number Publication date
US5250078A (en) 1993-10-05
EP0514337A1 (fr) 1992-11-19
JPH05132880A (ja) 1993-05-28
DE59204395D1 (de) 1996-01-04

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