FIELD OF INVENTION This invention relates to a process for indigo dyeing of wool and wool blends.

BACKGROUND OF INVENTION It is generally known that indigo is a vat dye which is insoluble in water. However when the vat dye is reduced to the leuco form by addition of sodium hydrosulphide and sodium hydroxide, it is dissolved into a reduced form, but without any colour. Thus, to impart a colour,, the leuco soluble form is subjected to the step of oxidation.

The process of dyeing with indigo is essentially known with respect to cotton yam Such a process of dyeing is carried out with the cotton yam being in an open width or rope form. In the open width form, total no. of ends required are arranged in a spread condition and are dyed and sized in one go to get a weaver's bean In the rope dyeing form the yams are formed into a rope. Generally, a single rope consists of approximately 350 to 400 yams and passed through dyeing vats. Affer dyeing, the rope is opened to cause a separation of the yarns on reels and to provide the yarns in a side by side relationship to get a spread sheet

U. S. Patent no. 5, 361, 438 discloses a method of indigo dyeing so as to allow the yarns to be used in knitting machines. Specifically, U. S. Patent no. 5,361, 438 suggests a method to dye the yarn in skeins or hanks so that the dyed yarn can be wound on a spool rather than on a reel. In such a process, the yarn is in the skein form and placed on a feed and drawn roller and such that the skein is passed through a plurality of indigo dye baths followed by oxidation. The number of dye baths each followed by oxidation depends on the colour intensity.

U. S. Patent no T 100,201 discloses a method for indigo dyeing of polyester fibers. In such a process the fibres are first coated with a polymeric salt so'as to provide washdown and fading properties similar to indigo dyed cotton fibers.

Being of cotton yarn, the process consists in forming the yarns into ropes, each rope cppaisting of a bundle of yarns. Such ropes are introduced into a vat dye bath containing the indigo dye followed by oxidation. A plurality of vat dye baths may be provided and followed each time by the step of oxidation, the number of such repetitive steps of impregnation and oxidation being dependent on the intensity of colour to be dyed on the yarn.

The process of indigo dyeing on wool yarn by a batch process could perhaps be carried out by impregnating wool yarn in a spread form in a vat dye bath. The impregnated yams are then hung in a loose form and subjected to the step of oxidation. Appropriate batch process for the indigo dyeing of woolen yarn has not been described in any literature, though a manner in which such a process could perhaps be carried out has been described hereinabove.

OBJECTS OF THE INVENTION An object of this invention is to propose an indigo dyeing of wool and wool blends.

Another object of this invention is to propose an indigo dyeing of wool and wool blends using the same dyeing apparatus as known with respect to cotton yarn.

Still another object of this invention is to propose an indigo dyeing of wool and wool blends having suitable dyeability factor.

Yet another object of this invention is to propose an indigo dyeing of wool and wool blends, which has dimensional stability.

A further object of this invention is to propose an indigo dyeing of wool and wool blends employing the known dyeing unit but using different parameters.

DETAILED DESCRIPTION OF INVENTION According to this invention there is provided a process for indigo dyeing of wool and wool blends comprising the steps of subjecting the wool and wool blends to a step of pretreatment prior to the spinning of the yarn by impregnation with a shrink resistance agent, subjecting the pretreated wool and wool blend to the step of indigo dyeing, post dyeing and said step of dyeing and post dyeing including a single step or a plurality of steps of impregnation of the pretreated wool and wool blends in a vat dye bath followed each time by the step of oxidation.

The term wool used herein is intended to imply wool in loose tops, hanks, yarn packages etc. (e. g. Cones, Cheeses, Beams etc,) yarn ropes/sheets and fabrics. Further the present , invention may be used as a continuous trough distinct advantages are associated with a continuous process. Still further, the parameters described herein are with respect to a continuous process which are not intended to be implied in a restrictive manner with respect to a batch or continuous process.

One of the aspects of this invention resides in subjecting woolen and woolen blends to a shrink resist treatment prior to the step of dyeing. The shrink resist treatment may be effected in the spun yarn itself. However, the homogeneity is reduced on a spun yarn in comparison to effecting the shrink resist treatment to the fibre or wool top. The yarn is in a twisted form, and therefore the homogeneity is considerably reduced if such a shrink resist treatment is effected on the yarn. However, in effecting such a treatment prior to the step of spinning, the separated fibres are disposed along the longitudinal axis and spaced from each other, and whereby the absorbality is improved in comparison to a yarn. Such an absorbality provides a better dye uptake.

The shrink treatment composition and operating temperatures and time period are described hereinabelow. However, such operating temperatures and time period are only exemplary in nature and in no instance tp be construed in a restrictive manner.

Treatment Procedure: Set the bath at 15°C with a composition of Acetic acid 0.3-0. 5 gpl Sodium Sulphate 1.5-3. 0 gpl Basolan DC (Sodium dichloro iso cynuric Dehydrate, 3.0-5. 0 gpl Shrink Resist Chemical) pH 3.5 to 4.0 gpl The temperature is raised to 50°C at 1°C per minute maintaining a pH of 3.50 to 4.0 and held 60 minutes.

Then sodium metabisulphite of 1.5-3. 0 gpl is added. The bath is run for 35 minutes and drained. The tops are then washed twice cold, once hot (60°C) and finally cold.

The flow chart of the process for the present invention is shown hereinbelow with respect to wool being in the form of a rope and the process is continuous in nature. However, the flow chart does not show the pretreatment steps and the shrink resist treatment steps. The flow chart essentially shows certain of the operating parameters of the known machine for a continuous process, but having operating parameters for dyeing of wool in rope form. It is considered that the impregnation period and that of oxidation is inversely proportionate to the speed of the machine.

FLOW CHART 100% WOOL BALL-WARPING LONGFORMING (M/c. Speed 75-100 mpm) Creel Tension 25-30 gms) ROPE-DYEING INDIGO DYEING REBEAMING (ON LCB M/C) (M/s. Speed 75-100 mpm) Rope Tension 5-10 psi) SIZING WEAVING FABRIC SETTING v FINISHING

A typical dye bath is as follows: Caustic soda-1. 5 to 3. 0 gpl Sodium hydrosulphite 1.8 to 3.0 gpl Indigo-0. 5-5.0 gpl An ionic Wetting agent (Primasol NF-Salt of phosphoric acid ester) 0.05 to 0.5 gpl An ionic Dispersing Agent (Setamol WS-Condensation product of an aromatic 0.05 to 0.5 gpl sulphonic acid) Dye-bath temperature 25°C-35°C pH 11. 2-12.5 The flow chart for the slasher process for the dyeing of wool is as follows, but without showing the shrink resist tF¢tXnent and ten pretreatment.

SLASHER DYEING PROCESS FLOW 100% Wool Yarn Direct Warping Indigo Dyeing cum sizing Weaving Finishing A typical dye bath for the slasher process is Caustic soda-1. 5 to 3.0 gpl Sodium hydrosulphite 1.8 to 3.0 gpl Indigo-0. 5-5.0 gpl An ionic Wetting agent (Primasol NF-Salt of phosphoric acid ester) 0.05 to 0.5 gpl An ionic Dispersing Agent (Setamol WS-Condensation product of an aromatic 0.05 to 0.5 gpl sulphonic acid) Dye-bath temperature 25°C-35°C pH 11. 2-12.5 The flow chart for hank indigo dyeing of woolen material is as follows.

TOP INDIGO DYEING AND HANK INDIGO DYEING OF WOOLEN MATERIAL: SR Treatment of Woolen Tops . Dyeing of Tops in Batch Reduced Form Oxidation Washing Drying A typical dye bath is as follows : Caustic soda-1. 5 to 3. 0 gpl Sodium hydrosulphite-1. 8 to 3. 0 gpl Indigo-0. 5-5.0 gpl An ionic Wetting agent (Primasol NF-Salt of phosphoric acid ester) 0.05 to 0.5 gpl An ionic Dispersing Agent (Setamol WS-Condensation product of an aromatic 0.05 to 0.5 gpl sulphonic acid) Dye-bath temperature 25°C-35°C pH 11. 2-12.5 Reference is made hereinafter to process parameters for indigo dyeing of wool in the form of rope. However, the flow chart and the parameters are only illustrative. Further, the resist shrink treatment is not shown.

CRITICAL PROCESS PARAMETERS WITH DYEING RECIPE FOR ROPE DYEING OF WOOLLEN TARN.

Critical process parameters for indigo Dyeing of woolen yarn on Rope Dyeing PROCESS FLOW CHART CREEL SECTION M/C SPEED-23 MPM (Speed Range 16mpm-28Km) 4. WASHBOX-1 (SCOURING : 02 GPL. PRIMASOLNF (WETTING AGENT), 80°C) 1 WASHBOX-1 (HOTWASH) 50°C 1 WASH BOX-3 (COLD WASH, ROOM TEMR.'} 4. Fer 16 ~w For28 DYE BOX-1 ( ! NDIGO DYEING) DIPPING TOME-23. S SEC. 33. 78 SEC. 19. 3 SEC. AIROXIDAnON OXCDN. TEME-102SEC. 146. 6 SEC 83. 7SSEC. 4 DYE BOX-2 (NDIGO DYEING) DIPPING TIME-23. 5 SEC. 33. 78 SEC. 19. 3 SEC. AIR MION O} SN. llME-102 BEC, 146. 6 SEC. 3. 78 SEC. 4 DYEBOX-30NDIGO DYEING) DIPPING TEME-23. S SEC. 33. 78 SEC. 19. 3 SEC. AIROXiDA'nON OXIDN. TIME-102 SEC. 146. 6 SEC. 83. 78 SEC. ir DYEBOXONDIGODYEMG) DIPPING TIME. 23. 5 SEC. 33. 78 SEC. 19. 3 SEC. AIROXIDAnON OXBDN. TEME-102SEC. 146. 6 SEC. 83. 78 SEC. 4. DYEBOX-S (INDIGO DYEMG) DIPPING TIME-23. 5 SEC. 33. 78 SEC. 19. 3 SEC. AlRQzAlIoN OnK, 102SEC. 146. 6 Y. 7BSEC, QX 6 XIGQ] PING TM-23, 5 SEC, 33. 78 9EC. 19. 3 SEC. AR OBAnON ODN. SE-102 SEC. 146. 6 SEC. 83. 78 SEC. 4. DYE BOX-7 (INDIGO DYEING) DIPPING 7IM-23. 5 SEC, 33. 78 SEC. 19, 3 SEC. AIR OXIDAMON OXDN. TIME-102 SEC. 146. 6 SEC. 83. 78 SEC. 4 DYE BOX-8 (INDIGO DYEING) DIPPING TIME-23. 5 SEC. 33. 78 SEC. 19. 3 SEC. AIR ? ATION N. TliE-102 SEC, 146, 6 EC, 83, 7 9C. I WASHBOX-4 (HOTWAw 50°e 41 WASH BOX-s (HOTWASH) s0°C 4, WASHBOX-6 (ACETICACmiOGPL, WASH60°C, P-6) 4 WAS BOX-7 (ACErIC ACED 10 GPLs WASH 4PC, M 5} DRYTNG (STEAM HEATED CYLINDER, STEAM PRESSURE UPTO 4. 5 BAR). Reference is made hereinabove to the step of scouring Though sodium hydroxide is the normal scouring agent for çoVonf it has been found that sodium hydroxide cannot be used for wool, and that a preferable agent is a detergent and a wetting agent.

Further, subsequent to the step of dyeing, the hot washed dyed wool is washed with acetic acid as it helps in reversing any elongation loss.