(19)
(11) EP 3 377 693 B1

(12) EUROPEAN PATENT SPECIFICATION

(45) Mention of the grant of the patent:
18.03.2020 Bulletin 2020/12

(21) Application number: 16733690.8

(22) Date of filing: 16.05.2016
(51) International Patent Classification (IPC): 
D06P 3/66(2006.01)
D06P 5/30(2006.01)
D06P 1/642(2006.01)
D06P 5/00(2006.01)
D06P 1/52(2006.01)
D06P 1/649(2006.01)
(86) International application number:
PCT/IB2016/052823
(87) International publication number:
WO 2017/085567 (26.05.2017 Gazette 2017/21)

(54)

COMPOSITION FOR THE TREATMENT OF A CELLULOSIC SUBSTRATE AND METHOD FOR COLOURING THE CELLULOSIC SUBSTRATE

ZUSAMMENSETZUNG ZUR BEHANDLUNG EINES CELLULOSESUBSTRATS UND VERFAHREN ZUM FÄRBEN DES CELLULOSESUBSTRATS

COMPOSITION DESTINÉE AU TRAITEMENT D'UN SUBSTRAT CELLULOSIQUE ET PROCÉDÉ POUR COLORER LE SUBSTRAT CELLULOSIQUE


(84) Designated Contracting States:
AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

(30) Priority: 20.11.2015 IT UB20155790

(43) Date of publication of application:
26.09.2018 Bulletin 2018/39

(73) Proprietor: ICS Tech SRL
20123 Milan (IT)

(72) Inventor:
  • CACCIA DOMINIONI, Ambrogio
    20123 Milan (IT)

(74) Representative: Manfredi, Irene 
Giambrocono & C. S.p.A. Via Rosolino Pilo, 19/b
20129 Milano
20129 Milano (IT)


(56) References cited: : 
WO-A1-99/20405
US-A1- 2002 025 379
US-A- 3 653 952
   
     
    Remarks:
    The file contains technical information submitted after the application was filed and not included in this specification
     
    Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


    Description


    [0001] This invention relates to a composition for the treatment of a cellulosic substrate with a view to colouring it by printing, and a kit for that treatment, a method for colouring the cellulosic substrate and use associated with that method.

    [0002] More particularly it relates to a composition and kit for the treatment of cellulosic fibres in order to colour them by means of printing, and a method and a use for the colouring of cellulosic fibres using monochlorotriazine dyes.

    [0003] It has been known for a long time that fabrics can be coloured using any digital printing method to apply the dye to the fabric, such as for example by ink-jet or rotary printing.
    US2002/025379 discloses a composition for the treatment of cellulosic substrates for the colouring thereof by means of reactive dyes comprising a cellulose reactive compound which can be nicotinamide. The composition can further comprise hydrotropes such as urea, polyethylene glycol and thiourea and antifoamers. US3653952 focuses on improved printing of fibrous substrates by coating with amino organosiloxane.
    WO 99/20405 relates to pre-treatment of fabric, including cellulose natural fabric, prior to ink dyeing and discloses the use of a compound including a functional polysiloxane.

    [0004] When a printing method is used to colour the fabrics, the quality of the coloured fabric also depends on the fixing method used after the colouring stage.

    [0005] Excellent results are obtained through fixing by means of steaming, although it is known that steaming gives rise to a number of disadvantages, such for example great consumption of water, time and logistics; an increased risk of defects associated with the repeatability of tones and migration of the dyes which takes place during the steaming stage; also the repeatability of the percentage of dye fixed varies on the basis of the settings; steaming gives rise to different kinetics in the dye fixing reaction, subsequently causing migration of the unreacted dye during subsequent washing, with consequent contamination of the printed areas and unprinted white areas.

    [0006] A known alternative method of fixing is thermofixing, which consists in fixing the dyes through the application of dry heat. This process proves more advantageous in terms of water consumption, application times, washing efficiency and reduced plant size. It has also been found that after thermofixing the quantity of dye lost during the washing stage is less than in comparison with steaming.

    [0007] However it is known that thermofixing has an adverse effect on the final appearance of the dyed fabric. In particular the colours obtained are visibly less intense, and the fabric has a slightly rough feel to the touch.

    [0008] The object of this invention is therefore that of providing a composition and a kit for the treatment of a cellulosic substrate which allows the latter to be coloured by means of printing and which makes it possible to obtain an optimum final product even after thermofixing.

    [0009] Another object of the invention is that of providing a method for colouring a cellulosic substrate in which colouring of the cellulosic substrate can be performed by ink-jet printing or rotary printing.

    [0010] This and other objects will be accomplished by means of a composition, a kit, a use and a method performed in accordance with the technical teachings in the appended claims.

    [0011] This invention relates to a composition for the treatment of a cellulosic substrate for colouring it through printing. In the present context printing is to be understood to mean any type of printing suitable for the application of a dye onto a cellulosic substrate using digital printing methods such as for example ink-jet printing, rotary printing, screen printing or others.

    [0012] In the context of this invention cellulosic substrate means cellulosic fibres in the form of fabrics and yarns in general.

    [0013] In accordance with the invention the composition comprises nicotinamide, a polydimethylsiloxane and urea.

    [0014] The nicotinamide acts as an activator or catalyst of the colouring reaction with the cellulosic substrate. This activator function is more efficient with monochlorotriazine dyes.

    [0015] The polydimethylsiloxane on the other hand has a corrective function in that it closes off much of the porosity in the cellulosic substrate, rendering it smoother. This brings about various advantages, such as better optical density of the inks. It has also been found that using polydimethylsiloxane together with nicotinamide it is possible to obtain a better colour yield on the fabric, with more intense tones and brighter colours, even in the situation where a printing process combined with thermofixing is used. In addition to this, the fabric obtained is softer to the touch in comparison with fabric which has only been treated with nicotinamide. This reactive polydimethylsiloxane is permanent and can therefore not be washed out in subsequent washes and does not in any way affect the final fastness of the applied dyes.

    [0016] Urea acts as a hydrating agent for the thermofixing stage. More specifically, during the application of heat associated with fixing, the urea creates a network on the cellulosic substrate which contains the dye in a non-aggregated form and maintains it in that state until temperatures are high, in addition to the function of retaining the water which is necessary for the reaction between the dye and the cellulosic substrate at the abovementioned high temperatures.

    [0017] Preferably the polydimethylsiloxane is of the hydrophilic type, is reactive with the substrate, is permanent and has a low refractive index. By permanent is meant that the polydimethylsiloxane remains on the cellulosic substrate even after washing. By low refractive index is meant a refractive index of less than 1.4, so that the dye has greater intensity and brightness. For this purpose it is useful also to add an oil to the polydimethylsiloxane in order to have a second refractive index which is different from that of the polydimethylsiloxane, and thus further improve the brilliance and intensity of the dye.

    [0018] Even more preferably the polydimethylsiloxane is of the amine type, that is it comprises at least one amine functional group.

    [0019] It is particularly advantageous to provide that the polydimethylsiloxane should be in a macroemulsion, so as to render the cellulosic substrate less porous, with the result of achieving a better optical density for the inks.

    [0020] Preferably the nicotinamide is present in a concentration of between 5 and 25 g/kg, the polydimethylsiloxane between 30 and 90 g/kg, and the urea between 50 and 400 g/kg with respect to the total weight of the composition. Even more preferably the composition comprises between 10 and 20 g/kg of nicotinamide, between 40 and 80 g/kg of polydimethylsiloxane, and between 200 and 300 g/kg of urea with respect to the total weight of the composition.

    [0021] Preferably the composition also comprises a thickener, which may be of natural or synthetic origin. In accordance with a preferred embodiment of the invention the thickener is selected from alginates, polyacrylates or carboxymethylcellulose. These compounds have the advantage that they do not contain OH groups which are likely to react with the dye, and therefore enter into competition with the OH groups in the cellulosic substrate, which would result in less dye being available for reaction with the cellulosic substrate.

    [0022] The alginates may be of the high, medium or low viscosity type, and the carboxymethylcellulose may have various degrees of substitution.

    [0023] In a preferred manner the thickener comprises medium/high viscosity alginates which have the advantage of giving rise to a porous structure on the cellulosic substrate which is more regular than acrylates and carboxymethylcellulose, with regard to their thermal stability, that is they maintain a suitable viscosity and a suitably porous structure, above all in the temperature range required for thermofixing.

    [0024] As is known, regularity of the porous structure is an advantage for the regularity of the optical density of the ink deposited on the substrate. Correct pore size at the high temperatures in use makes the ink pass through correctly without creating steric hindrance interferences because of the dimensions of the dye molecules, but not pore sizes which are sufficiently high to sufficiently impede migration of the ink. It is furthermore obvious that an increase in the surface area of the porous structure will result in an increase in its porosity, and greater porosity results in less coalescence of the drops of ink on the substrate, and therefore a more regular optical density. Furthermore it has been observed that thickening agents based on alginates make optimum control of dye migration possible even at high temperatures, in that their cross-linked structure, and therefore their viscosity, also persists as temperature rises, and therefore, by not decomposing their porous structure and reducing only their viscosity, they favour migration of dye from the thickener to the cellulose, maintaining the desired definition of the printing, thanks to the residual viscosity, as well as the necessary contact with the cellulosic substrate, thanks to the reduced migration, so that the dye-fibre reaction can take place.

    [0025] Among the alginates, medium/high viscosity alginates give the best results in terms of the optical density of printing and colour yield. It will also be noted that medium/high viscosity alginates maintain a regular porous network, above all even under alkaline conditions, in particular at pH 8 - 9.

    [0026] Preferably the composition according to the invention also comprises at least one rheological stabiliser selected from the terpenes. Even more preferably the terpene is pinene. Advantageously it is possible for the pinene to be provided in the form of pine oil, and incorporated in the composition through an aqueous emulsion of nicotinamide in the pine oil; this terpene has the ability to modify the rheology of the printing paste, rendering it less pseudoplastic, and therefore more newtonian, and increasing the transfer capacity of the printing paste onto the substrate during the stage of preparation for ink-jet printing or direct printing using rolls and silk screen.

    [0027] In accordance with a preferred aspect of the invention the composition also comprises a hydrophilic polydimethylsiloxane having a low refractive index. As already mentioned, by a low refractive index is meant a refractive index of less than 1.4.

    [0028] The presence of the polydimethylsiloxane having a low refractive index makes it possible to reduce the refractive index of the substrate, thus increasing the optical path of the light incident within the fibre on which the ink is deposited. This results in a decrease in the white reflection of the substrate, and therefore in a relative increase in the optical density of the printed colour.

    [0029] Preferably the composition comprises nicotinamide, the hydrophilic and reactive polydimethylsiloxane having a low refractive index, an increased quantity of urea, a thickener selected from alginates, carboxymethylcellulose and polyacrylates, sodium bicarbonate and an anti-reducing agent based on meta-nitrobenzene-sulfonate.

    [0030] The composition may also form part of a kit for preparation of the cellulosic substrate. This kit is to be intended as being part of this invention.

    [0031] The above composition may be applied directly to the cellulosic substrate before the printing stage and that stage of the process is described as "preparation" in the case where ink-jet printing is intended.

    [0032] If instead rotary printing is used, the composition should be provided in the form of a paste which also comprises at least one dye. This paste for colouring a cellulosic substrate is also intended to be protected by this application.

    [0033] In the paste the dye is preferably a monochlorotriazine dye and even more preferably a monofunctional monochlorotriazine dye. It has been found that when undergoing thermofixing monofunctional monochlorotriazine dyes are fixed to a greater extent than bifunctional monochlorotriazine dyes.

    [0034] This invention also relates to a method for dyeing a cellulosic substrate, comprising, but not necessarily in the order indicated, the stages of:
    1. a) applying a composition according to the invention to the cellulosic substrate;
    2. b) drying the cellulosic substrate;
    3. c) applying at least one dye by means of printing;
    4. d) fixing the dye by thermofixing; and
    5. e) washing the cellulosic substrate.


    [0035] Through using a composition comprising nicotinamide, polydimethylsiloxane and urea it is possible to avoid fixing stage d) being performed by steaming, and to maintain a high quality of the dyed cellulosic substrate in both colour yield, maintenance of the white (unprinted parts) and the softness of the fabric.

    [0036] Preferably the dye is a monochlorotriazine dye. Even more preferably the dye is a monofunctional monochlorotriazine dye. It has been found that when they undergo thermofixing monofunctional monochlorotriazine dyes are fixed more quickly than in the steaming process, resulting in an improvement in production times and energy expenditure, but comparable as regards the quantity of reacted dye. Bifunctional monochlorotriazine dyes on the other hand are fixed less effectively by thermofixing.

    [0037] In accordance with a first variant of the method, stage c) of applying the dye is carried out by ink-jet printing of the dye onto the cellulosic substrate.

    [0038] In this case stages a), b) and c) are performed in succession, and in the order indicated, that is after the substrate has been treated with the composition according to the invention the treated substrate is dried and then coloured by ink-jet printing.

    [0039] In accordance with a second variant of the method, stage c) of applying the dye is carried out by rotary printing.

    [0040] In this case however the paste mentioned above, which comprises both the composition according to the invention and the dye, has to be used. It is pointed out that the stages a) of applying the composition and c) of applying the dye are simultaneous, and that these take place before stage b) of drying the cellulose substrate.

    [0041] In accordance with a preferred aspect of the invention, stage a) of treating the cellulosic substrate takes place through a procedure of impregnating the substrate, in particular through a pad batch or rotary printing process.

    [0042] Washing stage e) is preferably carried out using at least one fatty amine, preferably ethoxylated. This surfactant has a dye inhibitor function during the stage of washing the dyed cellulosic substrate.

    [0043] According to a preferred aspect of the invention washing is also carried out using sodium dodecylbenzene sulfonate, mixed with the fatty amine. It has in fact been found that in the presence of the ethoxylated fatty amine this compound produces a synergistic effect in washing efficiency and inhibition of dye redeposition, thus resulting in better efficiency in washing the unfixed dyes and optimum maintenance of the white and the original printed tones due to contamination of the unfixed dye. It has been found that this washing kit reduces the washing tanks in continuous washing to only three in comparison with the six normally used, thus improving water consumption.

    [0044] Advantageously the ethoxylated fatty amine or the mixture of fatty amine with sodium dodecylbenzene sulfonate is sold in the form of a kit for washing a cellulosic substrate following printing and thermofixing.


    Claims

    1. Composition for the treatment of a cellulosic substrate for colouring it with monochlorotriazine dyes, comprising
    nicotinamide as activator,
    polydimethylsiloxane, and
    urea.
     
    2. Composition according to claim 1, wherein the polydimethylsiloxane comprises at least one amine functional group.
     
    3. Composition according to any one of the preceding claims, wherein the polydimethylsiloxane is provided as a macroemulsion.
     
    4. Composition according to one or more of the preceding claims, comprising between 5 and 25 g/kg of nicotinamide, between 30 and 90 g/kg of polydimethylsiloxane, and between 50 and 400 g/kg of urea in relation to the total weight of the composition, preferably comprising between 10 and 20 g/kg of nicotinamide, between 40 and 80 g/kg of polydimethylsiloxane, and between 200 and 300 g/kg of urea in relation to the total weight of the composition.
     
    5. Composition according to one or more of the preceding claims, comprising at least one thickener selected from an alginate, a polyacrylate or a carboxymethylcellulose, preferably further comprising a rheological stabiliser based on pinene.
     
    6. Paste for colouring a cellulosic substrate by printing, comprising the composition according to one or more of the preceding claims, and at least one dye.
     
    7. Kit for the treatment of a cellulosic substrate in order to colour it by means of monochlorotriazine dyes, comprising the composition according to one or more of claims 1 to 6.
     
    8. Use of a polydimethylsiloxane together with nicotinamide to treat a cellulosic substrate in order to colour it by printing.
     
    9. Method for colouring a cellulosic substrate, comprising, not necessarily in the following order, the stages of:

    a) applying a composition according to one of claims 1 to 5 to said cellulosic substrate;

    b) drying said cellulosic substrate;

    c) applying at least one dye to said cellulosic substrate by printing;

    d) fixing said dye by thermofixing; and

    e) washing said cellulosic substrate.


     
    10. Method according to the preceding claim, wherein stage c) of applying the dye is carried out by ink-jet printing, stages a) and c) being performed one after the other, or wherein stage c) of applying the dye is carried out by rotary printing, stages a) and c) being carried out simultaneously, and before stage b) of drying the cellulosic substrate.
     
    11. Method according to one of claims 9 to 10, wherein the dye is a monochlorotriazine dye, preferably wherein the dye is a monofunctional monochlorotriazine dye, more preferably wherein the dye is applied by ink-jet printing.
     
    12. Method according to one or more of claims 9 to 11 wherein stage a) of treating the cellulosic substrate is performed using an impregnation or rotary printing process.
     
    13. Method according to one or more of claims 9 to 12 wherein washing stage e) is performed with an ethoxylated fatty amine.
     
    14. Method according to the preceding claim, wherein washing stage e) is carried out with sodium dodecylbenzene sulfonate mixed with the ethoxylated fatty amine.
     


    Ansprüche

    1. Zusammensetzung zur Behandlung eines Cellulosesubstrats, um es mit Monochlortriazin-Farbstoffen zu färben, umfassend
    Nicotinamid als Aktivator,
    Polydimethylsiloxan, und
    Harnstoff.
     
    2. Zusammensetzung nach Anspruch 1, wobei das Polydimethylsiloxan mindestens eine funktionelle Aminogruppe umfasst.
     
    3. Zusammensetzung nach einem der vorherigen Ansprüche, wobei das Polydimethylsiloxan als Makroemulsion bereitgestellt ist.
     
    4. Zusammensetzung nach einem oder mehreren der vorherigen Ansprüche, umfassend zwischen 5 und 25 g/kg Nicotinamid, zwischen 30 und 90 g/kg Polydimethylsiloxan und zwischen 50 und 400 g/kg Harnstoff, bezogen auf das Gesamtgewicht der Zusammensetzung, vorzugsweise umfassend zwischen 10 und 20 g/kg Nicotinamid, zwischen 40 und 80 g/kg Polydimethylsiloxan und zwischen 200 und 300 g/kg Harnstoff, bezogen auf das Gesamtgewicht der Zusammensetzung.
     
    5. Zusammensetzung nach einem oder mehreren der vorherigen Ansprüche, umfassend mindestens ein Verdickungsmittel, ausgewählt aus einem Alginat, einem Polyacrylat oder einer Carboxymethylcellulose, vorzugsweise ferner umfassend einen rheologischen Stabilisator basierend auf Pinen.
     
    6. Paste zum Färben eines Cellulosesubstrats durch Drucken, umfassend die Zusammensetzung nach einem oder mehreren der vorherigen Ansprüche und mindestens einen Farbstoff.
     
    7. Kit zur Behandlung eines Cellulosesubstrats, um es mittels Monochlortriazin-Farbstoffen zu färben, umfassend die Zusammensetzung nach einem oder mehreren der Ansprüche 1 bis 6.
     
    8. Verwendung eines Polydimethylsiloxans zusammen mit Nicotinamid, um ein Cellulosesubstrat zu behandeln, um es durch Drucken zu färben.
     
    9. Verfahren zum Färben eines Cellulosesubstrats, umfassend, nicht notwendigerweise in der folgenden Reihenfolge, die folgenden Stufen:

    a) Anwenden einer Zusammensetzung nach einem der Ansprüche 1 bis 5 auf das Cellulosesubstrat;

    b) Trocknen des Cellulosesubstrats;

    c) Anwenden mindestens eines Farbstoffs auf das Cellulosesubstrat durch Drucken;

    d) Fixieren des Farbstoffs durch Thermofixieren; und

    e) Waschen des Cellulosesubstrats.


     
    10. Verfahren nach dem vorherigen Anspruch, wobei Stufe c) eines Anwendens des Farbstoffs durch Tintenstrahldrucken durchgeführt wird, die Stufen a) und c) nacheinander ausgeführt werden, oder
    wobei Stufe c) eines Anwendens des Farbstoffs durch Rotationsdruck durchgeführt wird, Stufen a) und c) gleichzeitig und vor Stufe b) eines Trocknens des Cellulosesubstrats durchgeführt werden.
     
    11. Verfahren nach einem der Ansprüche 9 bis 10, wobei der Farbstoff ein Monochlortriazin-Farbstoff ist, vorzugsweise ein monofunktioneller Monochlortriazin-Farbstoff, wobei der Farbstoff vorzugsweise durch Tintenstrahldrucken angewendet wird.
     
    12. Verfahren nach einem oder mehreren der Ansprüche 9 bis 11, wobei Stufe a) eines Behandelns des Cellulosesubstrats unter Verwendung eines Imprägnierungs- oder Rotationsdruckverfahrens ausgeführt wird.
     
    13. Verfahren nach einem oder mehreren der Ansprüche 9 bis 12, wobei Waschstufe e) mit einem ethoxylierten Fettamin ausgeführt wird.
     
    14. Verfahren nach dem vorherigen Anspruch, wobei Waschstufe e) mit Natriumdodecylbenzolsulfonat gemischt mit dem ethoxylierten Fettamin durchgeführt wird.
     


    Revendications

    1. Composition pour le traitement d'un substrat cellulosique pour le colorer avec des colorants de monochlorotriazine, comprenant
    du nicotinamide en tant qu'activateur
    du polydiméthylsiloxane, et
    de l'urée.
     
    2. Composition selon la revendication 1, dans laquelle le polydiméthylsiloxane comprend au moins un groupe fonctionnel amine.
     
    3. Composition selon l'une quelconque des revendications précédentes, dans laquelle le polydiméthylsiloxane est fourni en tant que macroémulsion.
     
    4. Composition selon l'une ou plusieurs des revendications précédentes, comprenant entre 5 et 25 g/kg de nicotinamide, entre 30 et 90 g/kg de polydiméthylsiloxane et entre 50 et 400 g/kg d'urée par rapport au poids total de la composition, de préférence comprenant entre 10 et 20 g/kg de nicotinamide, entre 40 et 80 g/kg de polydiméthylsiloxane et entre 200 et 300 g/kg d'urée par rapport au poids total de la composition.
     
    5. Composition selon l'une ou plusieurs des revendications précédentes, comprenant au moins un épaississant sélectionné parmi un alginate, un polyacrylate ou une carboxyméthylcellulose, de préférence comprenant également un stabilisant rhéologique à base de pinène.
     
    6. Pâte pour la coloration d'un substrat cellulosique par impression, comprenant la composition selon l'une ou plusieurs des revendications précédentes et au moins un colorant.
     
    7. Kit pour le traitement d'un substrat cellulosique afin de le colorer au moyen de colorants de monochlorotriazine, comprenant la composition selon l'une ou plusieurs des revendications 1 à 6.
     
    8. Utilisation d'un polydiméthylsiloxane avec du nicotinamide pour traiter un substrat cellulosique afin de le colorer par impression.
     
    9. Méthode pour la coloration d'un substrat cellulosique, comprenant, non nécessairement dans l'ordre suivant, les étapes suivantes :

    a) application d'une composition selon l'une des revendications 1 à 5 audit substrat cellulosique ;

    b) séchage dudit substrat cellulosique ;

    c) application d'au moins un colorant audit substrat cellulosique par impression ;

    d) fixation dudit colorant par thermofixation ; et

    e) lavage dudit substrat cellulosique.


     
    10. Méthode selon la revendication précédente, dans laquelle l'étape c) d'application du colorant est effectuée par une impression à jet d'encre, les étapes a) et c) étant effectuées l'une après l'autre, ou
    dans laquelle l'étape c) d'application du colorant est effectuée par une impression rotative, les étapes a) et c) étant effectuée de façon simultanée et avant l'étape b) de séchage du substrat cellulosique.
     
    11. Méthode selon l'une des revendications 9 à 10, dans laquelle le colorant est un colorant de monochlorotriazine, de préférence dans laquelle le colorant est un colorant de monochlorotriazine monofonctionnel, idéalement dans laquelle le colorant est appliqué par une impression à jet d'encre.
     
    12. Méthode selon l'une ou plusieurs des revendications 9 à 11, dans laquelle l'étape a) de traitement du substrat cellulosique est effectuée à l'aide d'un processus d'impression rotative ou d'imprégnation.
     
    13. Méthode selon l'une ou plusieurs des revendications 9 à 12, dans laquelle l'étape de lavage e) est effectuée avec une amine grasse éthoxylée.
     
    14. Méthode selon la revendication précédente, dans laquelle l'étape de lavage e) est réalisée avec du dodécylbenzène sulfonate de sodium mélangé à l'amine grasse éthoxylée.
     






    Cited references

    REFERENCES CITED IN THE DESCRIPTION



    This list of references cited by the applicant is for the reader's convenience only. It does not form part of the European patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be excluded and the EPO disclaims all liability in this regard.

    Patent documents cited in the description