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Why Indigo? Indigo is a dye different than any other. It does not require any mordant. Rather it is dyed through a living fermentation process. The process "reduces" the Indigo, changing it from blue to yellow. In this state, it dissolves in an alkaline solution. The fibre is worked in the solution, or "vat". When brought out to the air, it is a bright green. Slowly the air changes it to the beautiful deep and rich blue of Indigo.
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Indigo in some form is used in all traditional cultures, for it is the only clear and fast natural blue. Indigo dyeing was one of the first speciality professions. Yet it is easy to keep a home pot going, and most colonial homesteads had one. This recipe is the one most commonly used for home dyeing. It contains no harsh chemicals nor toxic metals. It can be used to dye any natural fibre. An additional beauty of dark Indigo is that when ironed or pounded, the blue cloth takes on a beautiful coppery sheen - the same sheen that is seen on the well reduced Indigo vat, when it is ready for dyeing. Indigo: Natural Vermentation Vat NOTE: requires advance preparation of about one week.
4 oz. ground Indigo 2 oz. ground Madder 2 oz. wheat bran (buy at any health food store) 12 oz. washing soda ("soda ash")
(above amounts are by weight ounces, not volume ounces.) Combine in about a three gallon pot of warm water. Always add these amounts in proportion. A larger vat can be made, for example with: 1 lb. ground indigo, 1/2 lb ground madder, 1/2 lb ground bran and 3 lbs washing soda in about a 10 gallon plastic tub. However, I advise starting small, till you are comfortable with the process. The size of the pot is determined by the amount of fobre you need to dye at one time. A three gallon pot is good for yarn skeins of 4 to 6 oz., while a 10 gallon or larger tub will be needed for yards of fabric. WARMTH: It is necessary to keep the vat warm, but not hot, around 100 - 110° Fahrenheit. It is the same temperature for raising bread or making yogurt. It should feel pleasantly warm to the hand.
To keep it warm, a light bulb in a reflector can be put under the vat, with a blanket over it to keep in the heat. (See illustration, next page.) In a warm climate no additional heat is needed, but be sure the vat is out of direct sun so it does not overheat. TIME is very important. It takes time for the vat to ferment and it does no good to try to rush the process. The first time, it takes about a week for the vat to ferment and be ready to dye. With "renewals" the time needed is a bit less, four or five days. It takes time to do the dyeing. The fibre is "dipped" several times to build up a dark color, with airing between each dip. The vat itself lasts a long time. I have had my current vat over fifteen years. In traditional cultures there are vats over 100 years old. The vat is "renewed" with more Indigo and the other ingredients in proportion, whenever the dye value weakens. Then let sit a few days to re-ferment. Indigo dyeing by this natural fermentation method is a slow-steady process. It is good meditation. Stir the vat once a day. The idea is to integrate the undissolved Indigo, madder and bran that settles to the bottom, back into solution. And to do this without incorporating air into the vat. So stir gently. Keep the vat covered. Air is the enemy of a good Indigo vat. The level of liquid in the pot should just allow room for the yarn dyeing, without spilling. The less air between surface and lid the better. I use a domed lid, turned upside down. If you leave more than 2" of air at the top of the vat, it will not reduce properly. The vat is ready for dyeing when:
It develops a coppery film on the top of the vat. The liquid, lifted carefully in a glass jar, will appear green. A test piece of fibre or paper will emerge green and turn blue in the air.
Now is the exciting time to begin Indigo dyeing! 1. Wet your fibre out very well in warm water. It must be well wet out. Any air remaining in the fibre will oxidize Indigo in the vat, and this must be avoided. 2. Put on rubber gloves! You don't want to scare people with blue hands; also the strongly alkaline vat may irritate your skin. 3. Enter the fibre (yarn/fabric) into the vat very carefully, to avoid adding any air to the vat. Now the fibre must be "worked" in the vat, under the surface. It should not be stirred, but with your gloved hands, gently, slowly and deliberately squeeze the liquid through the fibre while you hold it under the surface. Any time you break the surface you introduce
air into the vat and this you do not want to do. 4. After you have worked it several minutes, carefully and slowly raise it out of the vat, squeezing the excess Indigo solution back into the vat. Do this squeezing as close to the surface as you can, as dropping liquid will bring air into the vat. 5. The fibre should be a bright clear green. It will start to turn blue in the air immediately. Lay it out on newspaper and let it air for 20 minutes. Repeat the dips up to five times for dark Indigo Blue. Air between each dip. For lighter shades, fewer dips are needed. 6. Rinse well. Then leave the fibre to air overnight. Soak and do a final rinse in the morning. The vat lasts indefinitely. It is begun with a certain amount of Indigo, and all other ingredients as given, in proportion. Dyeing is begun, with the darkest color dyed first, then medium, then lights. Between dyeings the vat must rest overnight or an extra day. This is because, during dyeing a certain amount of the Indigo is oxidized in the vat. Allowing it to rest lets it re-reduce that Indigo. An oxidized (blue colored) vat won't dye well. The Indigo color will only wash out and rub off too quickly. When the vat is "exhausted", and will only dye light shades, it is time to renew it. All ingredients are again added, again in correct proportion. The vat is let to ferment for several days, and is ready to dye when it shows the proper signs. In this way a vat can be kept going for many years. If one wishes to rest from dyeing for several weeks, simply turn off the heat source, and keep the vat cool for that period. Stir it vigorously on occasion. When ready to dye again, warm it up, renew it with the ingredients, and proceed as before. It is not good to leave a vat unused for too long, as it is a living process and may then get cranky about starting up again. Also it is important to exhaust the vat before leaving it, or it may over-ferment and ruin any Indigo remaining in it. Over time a deposit of sludge will develop at the bottom of the vat. You may want to gently lower a screen into the vat before dyeing, to keep your fibre from pickinging itup during the dye process. Be sure to remove the screen after the day's dyeing, so you can stir the vat before closing it. For greens, dye you fibre Indigo first, then rinse well and overdye with alum mordant and your chosen yellow dye. For purples, dye the Indigo first, rinse well, then mordant and dye over with any red dye. The indigo vat is very alkaline. It is important to rinse out all the alkalinity. Just to be on the safe side, I always double rinse my indigo dyed textiles. First I rinse well just after dyeing, then I let air overnight. Next day I soak in two successive waters for about an hour each time, rinse again, wring and dry.
Squeeze solution through yarn for best penetration. Always work under the surface of the vat. Always wear rubber gloves. More About Indigo Indigofera is a legume. The plant looks similar to alfalfa, but is usually larger. It is an excellent rotational crop for increasing soil fertility. In southern Mexico, where some of the current Indigo of commerce originates, it is naturalized and grows in fallow fields, so no effort is spent cultivating it. Indigo dye must be prepared from the fresh plant in an exacting and elaborate process that takes about a month. The Indigo plants are harvested and brought to a central location. They are soaked in water and allowed to ferment. This separates the dyestuff from the plant. The solution is then beaten to oxidize and precipitate the Indigo. Excess water is poured off and the sludge is dried. This sludge, packed into balls or patties and fully dried, is the Indigo dye of commerce. This Indigo comes to us in the form of a hard, dark blue colored cake. It must be ground to be used for dyeing. Very small amounts can be ground in a mortar and pestle. Use a bit of water to facilitate grinding and keep down the dust. A Corona Corn mill is what I use. Meat grinders also work. A zip-loc baggie cinched over the grinding plates catches all the powder and keeps blue dust from getting everywhere. In most traditional cultures, the color(s) of ones clothing indicates ones status or class. Indigo blue has long been associated with the less than aristocratic classes. Indigo blue has still the association of "The Working Class". We use the distinction as "Blue Collar Workers" and "Blue Jeans". These clothes were originally dyed with indigo. In the past, Indigo has been a prolific dyestuff. It is relatively easy to grow and dye, and is quite fast. It withstands well the many washings that work clothes require. In most cultures, Indigo dyeing is or was a specialty. The dye process is unique, and the facilities require a stable set-up. Vats made of great clay pots set in the ground are commonly used in warmer climates. If more heat is needed, pits for burning charcoal are placed between clusters of the vats. Indigo dyeing is practiced today in Japan, Southern China, Tibet, India, Indonesia, Indo China, Africa, especially Nigeria, Southern Mexico and Guatemala, and it has recently been reintroduced to Turkey. Traditional fermentation methods are used. However, many of these cultures now use synthetic Indigo, manufactured from coal tar or petroleum. Natural Indigo contains several related dye chemicals that give different shades of blue. As much as twenty percent of the dye may be a violet tone called Indigo Red. These complexities give Natural Indigo nuances and depths that cannot be
achieved with the synthetic substitute. Here is a page with more about the chemical properties of indigo. An additional beauty of dark Indigo Blue, is that when ironed or pounded, cloth so dyed takes a coppery sheen - the same sheen we see on the top of the well reduced Indigo vat.
PO Box 14 • Somerset, MA 02726 orders 1-800-2-BUY-DYE technical support 508-676-3838 fax 508-676-3980 e-mail • email@example.com www.prochemical.com
Please read the directions carefully before starting. Indigo belongs to a class of dyes called vat dyes, which are among the oldest natural coloring substances used for textiles. Until the beginning of this century, indigo could be obtained only from plants. Two things are required to make indigo work, Thiox, the reducing agent, and Lye, the alkali. The dye vat is prepared in two steps: The stock solution and the dye vat. The stock solution then added to the dye vat. Always do test samples before working on a large project.
While Indigo and the chemicals used are comparatively safe and non-toxic, it is best to treat them all with caution. Wear rubber gloves to minimize contact with hands. Eye protection is urged as you are working with alkalies and strong reducing agents. Always work in a well ventilated area. Good house-keeping is essential to good results. Utensils used for dyeing should never be used for food preparation. See caution for Lye (Sodium Hydroxide) below.
Supplies: For Cotton, linen, rayon, and silk PRO Indigo grains For Wool PRO Indigo grains
5. add the Thiox to 1 cup (250 ml) of warm water (Mini Vat use ½ cup (125 ml) water). Measure the COLD water into a separate container. until reduction is complete. . 6. Set the jar of stock solution in a pan of HOT Water. slowly add the thiox solution. linen. Slowly add the lye solution to the pasted Indigo and stir to make a smooth mixture.5 liters) Lye 1 cup (215 gm) Thiox 2 Tbl (25 gm) Mini vat 3 Tbl (15 gm) 1½ cups (375 ml) 5 tsp (23 gm) 1 tsp (4 gm) 2. Otherwise the surface is a deep blue from oxygen coming in contact with the dye. Full size vat PRO Indigo 1 cup (70 gm) Cold water 6 cups (1. if necessary. Stir this mixture gently from time to time. rayon and silk 1. Raise the temperature no higher than 135oF (57oC) for 15 to 30 minutes or until reduction takes place. Avoid creating air bubbles. In a third container. Reduction is complete when the stock solution turns yellow. Determine whether you wish to make a 20 gallon (80 liter) full size vat or 4 gallon (16 liter) mini vat and prepare the stock solution. 3. 7. Stir gently to dissolve. Carefully add the lye and set aside to cool. Next. 4.Lye (Sodium Hydroxide) Thiox (Thiourea Dioxide) Metaphos Non-Iodized Salt Distilled White Vinegar Ivory Bar Soap or Ivory Flakes Lye (Sodium Hydroxide) Thiox (Thiourea Dioxide) Synthrapol SP Unflavored Gelatin Clear Household Ammonia Distilled White Vinegar Ivory Bar Soap or Ivory Flakes Procedure for dyeing cotton. Mix Indigo with enough luke warm water to make a lump free paste.
Lower the container into the vat and slide the liquid out at an angle. Add reduced stock solution by carefully lowering the container into the Dye Vat and sliding the liquid out at an angle. 13. use a deep vessel with a narrow top to minimize exposure to air. Make the dye vat.5 ml) Synthrapol per pound (454 gm) of fabric. Full Size Vat Warm Water 120oF(49oC) 20 gallons (80 liters) Metaphos 3 Tbl (63 gm) Salt 2 cups (600 gm) Thiox 4 tsp (15 gm) Mini Vat 3 gallons (12 liters) 1 tsp (7 gm) 1/4 cup (75 gm) ½ tsp (2 gm) 9. The vat is then ready to use. do not pour them in. 10. Stir in the Metaphos and salt. If the vat is not clear and greenishyellow in color wait an additional 30 to 60 minutes. It can take as long as 6 hours for proper reduction. dark blue metallic surface. . Stir gently. Measure warm water into dye vat container.8. After 30 to 60 minutes the vat should be clear greenish-yellow with a shiny. * When adding additional Stock Solution or dissolved chemicals to the vat. Maintaining the Indigo vat * Every precaution MUST be taken to keep oxygen out of an Indigo vat!!! * For your vat. machine wash the fabric on HOT cycle with a minimum temperature of 140oF (60oC) water OR by hand in a pot on the stove with ½ tsp (2 gm) PRO Dye Activator or Soda Ash and ½ tsp (2. 11. Dissolve the Thiox in a small amount of warm water and add it to the dye vat. Using the Indigo vat *Before dyeing. 12. Rinse thoroughly.
DO NOT SWISH the fabric around in the vat. Troubleshooting the dye vat * If the vat appears grayish and watery. Wait 15 minutes and check vat again before dyeing. This helps the dye penetrate. If you’ve done a bound resist dyed fabric it’s best to let the fabric dry completely before untying so the threads won’t rip the fabric. Hang cotton and rayon to dry. Then rinse the silk thoroughly in plain water. Let the fabric air dry before washing. Where scum clings to the cloth it will look dark blue. squeeze out excess water evenly. Repeat dipping and oxidizing until you’ve reached the desired depth of blue. With a knife. . it is exhausted.* Thoroughly wet fabrics before dipping in vat. or if blue specks appear. * Gently push the dark blue scum aside before entering fabric in the vat. * Gently squeeze out excess dye BELOW the surface and remove fabric from the dye vat. Add a small amount (½ tsp (2 gm) for full size vat) Thiox. 2 to 3 minutes. Stir the wash bath occasionally and rinse the fabric until the water runs clear. without splashing. leaving a light undyed spot. Remember that after washing. it’s easy to flake off a 1/8 inch thick peel of soap. This means that all the indigo has been used. more Thiox is needed. DO NOT allow fabric to drip into the vat after dyeing. Washing the fabric Wash the fabric in hot 135oF to140oF (57oC to 60oC) water for 10 minutes in a generous bath of Ivory bar soap or Ivory Flakes. after dyeing is finished the spot will wash off the surface. * Lower fabric into the vat very gently. dissolved in water. Make the acid soak by mixing 2 Tbl (30 ml) of White Distilled Vinegar in 1 gallon (4 liters) of room temperature water. the final color will be one to two shades lighter. An addition of Stock Solution is needed. Keep fabric submerged for the duration of each dip. * If the vat changes from yellow-green to blue. Stir gently. dissolved in water. * Slowly manipulate the cloth while working below the surface of the vat. A warm water soak for 15 to 30 minutes is recommended. * If the vat has been left for a few days. However. If you’ve gotten some of the dark blue scum on your fabric. *Let fabric oxidize (turn blue) for approximately 15 minutes. If you’re dyeing silk then soak it for 10 minutes in a bucket of acid soak. This way the fabric that is underneath the scum can oxidize. Wearing gloves. it may need to be "Sharpened" with a small amount (½ tsp (2 gm) for full size vat) Thiox. then give it a rinse in plain room temperature water.
Excess alkali or reducing agent can unbalance the vat. Stir gently from time to time until reduction is complete. Be patient. Slowly add the Lye solution to the pasted Indigo and stir to make a smooth mixture. Reduction is complete when the stock solution turns yellow. and the vat will have a long life. 5. Troubleshooting fabric * Dye washes off of fabric: too little reducing agent. Prepare the stock solution. Wait 15 minutes and check vat again before dyeing. Carefully add the lye and set mixture aside to cool.* If white specks appear or the vat appears "milky" add small amount (1 tsp for full size vat) of Lye. 7. Stir gently. 6. * Always dissolve Thiox and Lye in water BEFORE adding to the dye vat. dissolved in ½ cup water. If necessary set the jar of stock solution in a pan of HOT . * Occasionally. In a third container add the Thiox to ¼ cup (60 ml) water. more than one addition is required to revive a vat. Measure 1½ cups (375 ml) of COLD water into a separate container. and wait 15 to 20 minutes between additions. Mix Indigo with enough luke warm water to make a lump free paste. * Cover with a tight fitting lid when not in use. 3. * Crocking off (Dye rubs off): too little alkali Procedure for dyeing wool 1. DO NOT add dry flakes. Mini Vat PRO Indigo 3 Tbl (15 gm) Lye 5 tsp (23 gm) Thiox 1 tsp (4 gm) 2. Use small amounts. 4. Stir gently until it’s dissolved. Add the Thiox solution slowly to avoid making air bubbles. testing each time. making it impossible to build up deep shades.
After 30 to 60 minutes the vat should be clear greenish-yellow with a shiny. Wool that is not thoroughly wet carries large quantities of air which quickly oxidize the reduced Indigo and destroy the vat. Add reduced stock solution by carefully lowering the container into the dye vat and sliding the liquid out at an angle. 11. Let the wool oxidize (turn blue) for approximately 15 minutes. Raise the temperature no higher than 135oF (57o) for 15 to 30 minutes or until reduction takes place. 16. remove the wool. 12. Stir gently. Use non-reactive metal such as stainless steel or un-chipped enamel as your dye pot. Soak the wool in the dye vat for 30 minutes with gentle. 10. intermittent stirring. 13. Mix the remaining ingredients in the order listed above making certain each item is thoroughly mixed before adding the next. making sure all the wool remains below the surface of the vat. Measure warm water into dye pot. Squeeze out excess water evenly from the wool. 14.Water. 15. 17. The wool should sink in the Synthrapol soak. Maintain a 120oF(49oC) temperature throughout the dye process. not float. 8. The vat is now ready to use. After 30 minutes. Gently push the dark blue scum aside before putting your wool into the vat. Soak your wool for at least 15 minutes in 1 gallon (4 liters) of 120oF (49oC) water with 1 tsp (5 ml) of Synthrapol. Repeat dipping and oxidizing until the desired depth of blue is obtained. Mini Vat Warm Water 120oF (49oC) 3 gallons (12 liters) Unflavored Gelatin powder 1 tsp (2 gm) Synthrapol 1 tsp (5 ml) Clear Household Ammonia 2 Tbl (30 ml) Thiox 1 tsp 4 gm) 9. Make the dye vat. . squeeze excess liquid back into the vat while holding the wool close to the surface to avoid introducing air into the vat. dark blue metallic surface.
dyeing(1-20). Indigo Dyeing Methods Indigo dyeing follows the same basic steps regardless of machine design. . Scour or dye bottoming in a heated tank. With a knife. © Copyright 2002 http://www. Make the acid soak by mixing 2 Tbl (30 ml) of White Distilled Vinegar in 1 gallon (4 liters) of room temperature water. After the final dip and the fiber is fully oxidized.8.denimsandjeans. washing tanks. Only Indigo dyeing requires multiple dye applications for a dark shade.the same color is produced using 1.com/denim/manufacturing-process/indigo-dyeing-methods-engineeringcolor-wash-fastness-and-fashion-effects/ Indigo Dyeing Methods – Engineering Color. gently wash the wool in a warm 120oF (49oC) water bath for 10 minutes in a generous bath of Ivory bar soap or Ivory Flakes. Commonly. In different areas of the world. 2. a single dye lot will have between 8 and 15 visually different shades from beginning to end and also have shade differences from one side to the other. Color consistency of Indigo in recent decades has been unsatisfactory as a result of machine designs that do not apply basic principles of fluid mechanics properly and unstable dye mixes. Gently stir the wash bath occasionally and rinse the fiber until the water runs clear.18.a heated tank for topping (optional) and wash tanks. Then rinse the wool thoroughly in plain water and hang to dry.0 or 4% Indigo depending on dyeing method. Then soak the wool for 10 minutes in a bucket of acid soak. Wash Fastness And Fashion Effects Indigo Dyeing Indigo dyeing is unique and because of the complex chemical reactions should be correctly viewed a a form of chemical engineering. it’s easy to flake off a 1/8 inch thick peel of soap.
4%) For dark Indigo that does not lose color 2% applied normally. with an Indigo bottom. 15% caustic cold 2. which loses color faster. in Latin America 2.Wash 50°C /Softener Chemical Feed 120 g/l 50% caustic 60g/l Hydro powder Feed 1.. In order to produce the same depth of color as 1. Wash 50°C 15. Wash cold Drying cylinders hot Steamer cold Boxes 5-12 Indigo Steamer cold 13.Wash 60°C 3.S.Wash 60°C 4. 2% Indigo will produce the same depth if low levels of caustic are used(0-0. Many companies use 4% or more Indigo on weight of yarn.2% in the U.Wash 50°C 14. Darkest Indigo Shades Very dark shades of Indigo are in demand currently around the world. method results in more surface (ring dyeing). The U. for a very dark shade.4 to 2. which is expensive. Dark Indigo Color This was an example of a typical method used in the U.S.8%) 1.S.8%. .0% is used and in Asia from 2. Wash 50°C 16. Dark Indigo(1.4 liters per minute Stock Mix 80 g/l Indigo Pure 100 g/l 50% Caustic 70 g/l Hydro powder.
Sulfur bottoms are an exception to the normal pH for sulfurs(11). which require 85 C. Wash 50°C 16. If dextrin reducing agents are used.Wash 60°C 4. 4% caustic 90°C 2.Wash 50°C/softener Control Of Sulphur Bottoming The typical methods used for dyeing sulfur bottoms result in denim shade differences. This is useful for shirting fabrics that are not strong enough for stonewashing. there will be variation. Special procedures are necessary in order to avoid colorfastness problems. When applied as light colors. bleaching or cellulase treaments. Light Indigo 0.Wash 60°C 3.4% 1. Wash 50°C 15. Wash 60°C Bypass drying cylinders Bypass steamer Close off boxes 5-8 Boxes 9-12 Indigo 13. Wash 50°C 14. .Light Indigo Shades Dyeing Indigo in light shades results in a sky-blue impossible with any other dye. requiring 12. sulfur dyes should be dyed at temperatures <60 C.
Sulfur topping colors include black. Pad sulfur(cold) Steamer hot 2. Sulfur Top 1. Indigo or wash 50°C 12.Wash 60°C 4.Wash 50°C 4. yellow brown and green.Sulfur Bottom 1. Wash 50°C 14. Wash 50°C 15. Sulfur topping permits much darker color than a sulfur bottom.Wash 50°C or softener Sulphur Topping In topping the sulfur dye is applied after the Indigo dyeing.Wash 60°C 3.Wash 50°C Boxes 5-10 Indigo 11. Indigo or wash 50°C Bypass steamer 13. but is duller.Wash cold 3. Wash cold By pass drying cylinders . blue-black. Pre-wet 2% caustic 90°C 2. Sulfur toppings are used to produce slub appearances in normal yarn. Wash 50°C 16.
Steam Reactives 1. drying units near the front of the machine and high-quality dye padders are required for quality dyeing. Wash cold 16. Pad monochlortriazine dye cold. Wash 60°C 14. Wash 60°C 15. Steamers. Small 150 liter boxes are inserted inside the larger dye tanks for Indigo and sulfur. Pad sulfur topping Steamer hot 13. Wash 50°C 15. Pad-Dry Chempad. Soap 90°C 12.Wash 50°C/Softener Reactive Dyes in Indigo Dyeing Reactive dyes can be applied on specially-Designed Indigo machines. Wash cold 14. Soap 90°C Steamer hot 13.Wash 50°C 3.Wash cold/softener . Wash 60°C 12. neutral pH Drying cylinders hot Pad caustic in salt brine Steamer hot Bypass boxes 5-10 11. Pre-scour wetter plus chelate 90°C 2.Bypass steamer Boxes 5-10 Indigo 11. Wash 50°C 16.
Wash 50°C 15.Wash 60°C 3. Wash 50°C 16. Wash 60°C 12. This concentrated mixture (70-90 g/L Indigo) is delivered by pipes to the Indigo dye tanks where the dye concentration is reduced to 1-4 g/L for dyeing the cotton.Pad Steam Reactive Topping 1. Wash cold 14. The primary source of color differences is the instability and inconsistency of Indigo mixtures. the color changes. Dye Mixing Procedures Many denim companies find it difficult to control original and washed Indigo shades. Wash 50°C / softener Control Of Indigo Dyeing The Indigo dyeing process begins with a concentrated mixture of Indigo. Pre-wet 10% caustic 90°C 2.Wash 60°C 4. Wash cold By pass drying cylinders Bypass steamer Boxes 5-10 Indigo 11. As the concentration of reducing agent going to the dye machine changes. Pad Dichorotriazinyl cold with bicarbonate Steamer hot 13. sodium hydroxide and reducing agent. Uniform Indigo Mixtures .
precipitation occurs. The Indigo color is the principal source of the almost magical appeal of denim. The dyeing process is unique among all methods of commercial dyeing. greenercolor and as the dye from the top of the tank enters the machine. there is a higher concentration than in the top of the tank. Indigo Dyeing – Problems And Potential -Part 1 October 24th. At higher levels. there is about 50 g/L of reducer. As the dye enters the machine. Consistency of Concentration There is a limit to the amount of any chemical that can be dissolved in water. principally on wool and silk . Reductive buffers can eliminate color differences in Indigo-dyed denims and can reduce hydrosulfite use by 30-50%. When the limit of solubility of any chemical •In water is exceeded. This is a highly technical article on Indigo dyeing by Harry Mercer. more ring-dyed.. the color is darker and redder. This is the first of a series of 4 articles addressing the problems and potential of Indigo dyeing. Dye Control In Feeding Tank Stirring the tank for 2 minutes will improve dye uniformity between top and bottom. faster fading. Instability of Indigo mixtures results from the decomposition of sodium hydrosulfite. Improving Dyeing Consistency When reducing agent sinks to the bottom of the tank. If dye requires 50 seconds to oxidize. Read on if you are technically oriented. 2011 by Harry Mercer | Filed under Manufacturing Process. the higher concentration results in a lighter. chemicals and dye sink to the bottom of the tank. To avoid settling of dye and chemicals the total solids should not exceed 20%. The “glass plate” test can be used to test concentrations of hydrosulfite in the top and bottom. the mixture must have consistent concentrations of Indigo. sodium hydroxide and reducer from the top of the mixture to the bottom. Indigo mixes should not have more than 20% solids. Buffers In Indigo Dyeing Alkaline buffers have been used to make very dark shades of Indigo with as little as 1% dye. The main cause of inconsistent Indigo mixtures relates to concentration levels. Indigo has been used for thousands of years. For consistent Indigo dyeing. with the unusual design that is necessary for cotton dyeing with Indigo.
Machine factors that affect Indigo dyeing results 1) Circulation system design: Indigo dye in its reduced form consists of dye particles that have been partially solubilized and exists in the form of charged colloidial particles. Colloidial dispersions will sink due to the influence of gravity and require some agitation to keep them uniformly dispersed in the dye box. BASF. No other method of cotton textile dyeing requires the multiple application of dye to achieve a dark color. Part 1 of 4 MACHINERY Indigo dyeing is a unique process that makes denim special and distinguishes denim operations from all other types of cotton fabrics. the concentrations are usually different. Many Indigo machines have the dye entry line on one side and the exit line at the yarn entry. In terms of Reynold‟s number . the flow should be slightly beyond laminar. both of which are more complex to conduct at a high level of quality. recommended that the volume of the dye box be “turned over” 2 or 3 times an hour. If sample are collected from different parts of an Indigo dye box(top. which is a . then the finishing. and the machine itself. The 2 most significant sources of Indigo dyeing are the control of chemical concentrations.fibers for which Indigo is more suitable The difficulties in dyeing cotton with Indigo are apparent with the numerous different shades that result. the entry line should be positioned in the yarn exit side of the box near the top. up to 15 per dye lot and also with side-center side variation. front and back). which will be addressed in future articles. Also. slow production speeds and extremes of color variation and color-fastness. The uneven distribution of dye in the box as the machine operates contributes to color variation. For many years. for uniform dispersion of Indigo. but it requires a deep understanding of the unusual variables of Indigo dyeing. thousands of liters of dye bath. This means that if the box volume is 2000 liters that 4-6000 liters of flow into and out of the dye box is needed to prevent low concentrations in part of the box and high in others. Elimination of this variation has been accomplished. while the exit line should be at the yarn entry side near the bottom. in the low transitional range to ensure uniform disper-sion while avoiding turbulence that would destabilize the dye. bottom. The 2 keys to success in manufacturing denim is firstly the dyeing. Indigo machines produced in recent decades have been furnished with pipes that are too small to deliver the right kind of flow. The failure of most denim companies to overcome the challenges in denim wet-processing is the reason why they are held hostage to low profit margins. a leader in indigo dye for most of the 20th century. Indigo dyeing has been conducted without these problems.
The dye penetration was complete which resulted in the darkest possible color with 3% Indigo and that would never fade. the more easily the dye penetrates into fibers and yarn. in a 2000 liter box with 2 square meters of surface area . so the immersion time was 2-3 times longer than on modern sheet ranges. which means that it is already wet. The loss in yarn strength results in higher warp breaks in weaving. Until the 1970‟s. So.the yarn loses strength and the ability of the dye to penetrate the cotton fibers is reduced. The yarn is normally scoured and washed before entering the dyeing section. In most indigo machines the box design is responsible for massive losses of hydrosulfite at the surface of the dye boxes during operation which results in economic losses as well as variations in hydrosulfite concentrations in the machine which leads to color variation. the hydrosulfite will decompose at twice the rate of a 2000 liter box with 1 square meter of surface area. the faster the hydrosulfite is lost. resulting in better colorfastness and darker color. The reduced penetration of Indigo into the fibers results in rubbing fastness problems and a higher per cent Indigo on weight of yarn for a specific depth of shade. while in the smaller boxes of a typical sheet range the losses will be from 4570%. 3) Tension Control: High yarn tensions on continuous Indigo dyeing machines has 2 significant effects. Indigo machines operated at speeds of 12 meters per minute through the much larger boxes of rope ranges.cause of cross-shade variation. . 2) Dye box design: In a previous article I discussed the effect of dye box design on the color consistency of Indigo. The principle is known as Specific Surface Area which means that the larger the surface area of the Indigo box to the volume. 4) Immersion time: Indigo dyeing is a form of wet-on wet processing. The total hydrosulfite losses in a typically larger box of a rope range will average around 15%. This is a slow process and the longer the immersion time . meaning lower efficiency and higher weaving off-quality. In order for the Indigo dye to enter the wet yarn efficiently‟ a process known as “liquor exchange” is necessary in which the Indigo dye/water displaces the water already in the yarn.
2011 by Harry Mercer | Filed under Manufacturing Process. Sodium dithionite can be extremely unstable. both of which attach to the dye molecule in the reduction process. The concentrated Indigo mix is then ready to pump into the dye machine for dyeing. but ultimately the most important factors involve the preparation of Indigo and chemical feeds to the machine. 4) Most of the variation in Indigo dyeing is a result of instability in this concentrated mix. Approximately 80% of Indigo dyeing control depends on the stability and consistency of the dye and chemicals being sent to the machine. the basic machine factors in Indigo dyeing were discussed. sodium hydroxide and the hydrosulfite (sodium dithionite).com/denim/manufacturing-process/indigo-dyeing-problems-andpotential/ Indigo Dyeing : Problems And Potential–Part 2 November 11th.http://www. The first part can be seen by clicking here Preparation For Dyeing In the previous article. The solution then is referred to as “leuco” Indigo. 3) The reduction of Indigo with sodium hydroxide and sodium dithionite is known as vatting and has been used for thousands of years. There are many other details required to achieve the highest quality Indigo dyeings . 1) Raw materials: The basic ingredients for Indigo dyeing are the Indigo dye. Vatting refers to mixing the dye and chemicals into a tank or “vat” with some stirring and then waiting from 1-4 hours usually for the complete reduction of the dye to occur which is noted when the solution color is a clear. It is second part of the article in series. with the concentrations in this feeding mixture becoming smaller with the . but this nomenclature is incorrect because the molecule does not contain hydrogen. yellow-brown. The “hydrosulfite acts on the sodium hydroxide to split it into NaO and hydrogen. This is a guest post by Harry Mercer on Indigo dyeing..Reduction is basically a process where hydrogen is produced which opens up the Indigo dye molecule allowing it to attach to a water molecule which carries the vat dye into the fiber.denimsandjeans. Indigo is an insoluble vat dye which means that it cannot enter the cotton fiber until it is made soluble by the process of reduction . The most commonly-used 2) The reducing chemical is known as “sodium hydrosulfite”. a Greek word meaning “without color”.
These stirrers should turn at only 10-15 RPM in order to avoid turbulence that would lower the strength of the mix. There are 2 simple . but special test methods to measure the concentration of alkali and sodium dithionite in the feeding mix: a 2-endpoint titration for alkali and the glass plate test which have been in use by the best denim companies for over a century and will be covered in a future article. This is evidenced in many denim operations that suffer 10-15 colors after fabric washing per dye lot. Stirring beyond that will result in more reducing agent being oxidized. Conclusion: The problem of Indigo color variations is principally a result of inconsistent dye and chemical concentrations going to the machine. the initial recipe may specify 100 grams per liter of sodium dithionite. Sponsored Link: http://www. Management of the feeding mix requires an understanding of the chemistry of reduced dye solutions. but by the time the last liter goes into the machine. 5) There are several causes for the decomposition and strength losses of the reducing agent in the feeding mix: Oxidation at the surface of the tank. With regard to concentrations. No more than 80 grams per liter of indigo should be added to a feeding mix as this is the maximum amount that has long been proven that can be completely reduced. the concentration often drops to 20 to 30 grams per liter and each 5 gram per liter loss in dithionite concentration produces a small Indigo color variation. making a redder Indigo tone later in the dyeing. and lower concentrations of reducer at the top of the tank. Concentrations above 23% solid have a tendency to settle. unnecessary stirring and high concentrations of ingredients. The Indigo feeding mix is of very high viscosity and in order to stir the entire mix out to the edge of the tank.passage of time. large propellers that cover the tank diameter are needed. if the viscosity of the dye mix is too high. measurement of concentrations and skill in correcting strength losses of ingredients in the feeding mix especially of reducing agent and alkali. The amount of reducing agent should also be limited to 80 grams per liter since greater amounts will cause more rapid decomposition due to aerobic and anerobic decay. Also. A glance at the design of flow of dye and chemicals into Indigo dye machines should make this obvious. the reduced Indigo will not disperse uniformly resulting in areas of varying concentration in the tank that will cause color change as the mix is fed to the machine. The stirring should be only enough to maintain consistent concentrations of dye and chemicals from the top of the feeding tank to the bottom. so that there are very high concentrations of reducer in the bottom of the tank.otherwise the color will change. The multiple dye box arrangement and circulation in the dyeing section of indigo machines allow the blending of indigo and reducing agents. 6) The concentrations of indigo and reducing agent must be actively managed so that the same concentrations of dye and reducer are feeding to the machine every minute.denimsandjeans. in many Indigo operations the stirring units are badly designed with small propellers that turn at high speeds.com/denim/manufacturing-process/indigo-dyeing-problems-andpotentialpart-2/ . For example. making a greener Indigo tone when pumped to the dye boxes. so the problem of variation obviously starts at the mixing tank.
Textil Kafi. a series of parallel cylinders begin to move apart allowing the yarn from the dye unit to continue through dyeing and allows the size machine approximately 2 minutes of time to install an empty weaving beam and re-start the sizing machine. Tear. in order to prevent the dyeing unit from stopping as well. Advantages and Disadvantages . there is only a single Indigo box through which the yarn passes 4-5 times. this oxidation takes place above each dye box. passes into the air and so forth until the required depth of shade is developed. Currently. Canatiba. the yarn passes directly to sizing where the yarn is prepared for weaving. 2010 by Harry Mercer | Filed under Manufacturing Process. There are other claimed advantages such as higher speeds and darker Indigo color. After drying the Indigo-dyed yarn. the yarn is conducted through the air after each box. the dyed yarn is passed through from 6-8 Indigo boxes on rope machines or 6-20 Indigo boxes on slasher (sheet) Indigo machines. Loopdye Machines in the Denim Industry In the early 1990‟s. The biggest concentration of these machines is in Brazil. This continuous passage of yarn between the yarn creel and the dye box is in the form of a “loop” which is almost circular. The name “Loopdye” results from the method of skying or air passage for oxidizing the Indigo-dyed yarn and the method of passing through the Indigo dye. lowering costs and pollution. then the yarn enters the next dye box. Santana and Cedro have 2 units each. followed by washing. there is a yarn accumulator between the drying cylinders at dyeing and the wet-size boxes. The white cotton is pulled into the front of the machine and passes first through the pre-treatment boxes. The Loopdye machine is a simplified version of a “sheet” or “slasher” Indigo machine. Vicunha employs 11 of these machines. On the other 2 important Indigo machine types. When the yarn stops moving on the sizing unit. then moves through a reactor which can be used for steaming or additional reaction time for sulfurbottoming or Mercerization. After immersion in each Indigo dye box. The wet yarn then enters the Indigo dye box. the yarn is carried to the rear of the machine. Because the sizing part of the machine must stop in order to remove a completed weaving beam. In the Loopdye process. In the case of rope and sheet ranges. When the yarn exits the dye box.Indigo Dyeing With Loop Dyeing Machinery November 4th. while Tavex. passes under the yarn creel where it is returned to the Indigo box for another dye passage. instead of moving forward. After making multiple loops through the Indigo dye box the yarn is conducted through wash boxes and on to drying cylinders. thee were approximately 30 Loopdye machines in use. the number is reported to be 60 or so. There are 9 of these machines that have been equipped with nitrogen units which use nitrogen gas as protective blanket over the surface of the Indigo dye. around the top and rear of the yarn creel from where it started. where the reduced Indigo (yellow-green) is oxidized or “fixed” by oxygen in the air returning to the original blue. The nitrogen gas prevents oxygen in the air from attacking sodium hydrosulfite resulting in more consistent dyeing and reducing consumption of hydrosulfite. Santista have 1 each. multiple dye boxes being necessary for dark shades because only a small amount of Indigo can be applied in each immersion.
The Loop machine is not provided with enough boxes after Indigo dyeing for sulfur topping as the slasher dyeing is. 6. Sulfur dyeing – The Loopdye machine can be equipped with a steamer for cold-pad sulfur bottoming which will provide greater consistency than a hot application in the 1st box. Versatility – In the higher denim fashion market. but this may be overcome by employing improved chemical blending. Rope machines still have the greatest flexibility with regard to producing a full range of denim colors. Rope machines still have an overall advantage in terms of Indigo dyeing quality. Operating Costs – Maintenance and energy costs are reported to be approximately 20% lower with Loopdye when compared with slasher dyeing and even lower than with rope dyeing. start-up times and speeds are similar. largely because yarn breaks in dyeing can be repaired at long-chain re-beaming. Overall. 8. . Weaving Efficiency – The methods of dyeing. the Loop machine is ideal for sulfur colors since it the dye can be applied in only one box. Productivity – When compared to a multi-box slasher machine. Rope dyeing machines can produce up to 4 times as much dyed yarn.1. Rope dyeing results in the lowest-level of weaving stops. has a direct effect on warp yarn breakage in weaving. 4. while rope dyeing provides the greatest flexibility for denim product development. which allows for faster color changes and less dye discarded after the dye lot is finished. Space requirements – The Loop machine with a single dye box requires less floor space than either sheet dyeing or rope dyeing. Capital Investment – The Loopdye machine has the lowest initial costs of continuous Indigo dyeing machinery. productivity is essentially equivalent since the yarn loading. Indigo consistency from the start-to-finish of dyeing can be expected to be better with the inclusion of nitrogen units. 2. currently reported to be approximately 25% less than 8 dyebox slasher machine. 5. Experience with the older design of Loopdye machines demonstrated higher levels of warp breaks in weaving than other Indigo machines. 7. 3. Rope machines also require higher ceilings because of the design of the airing arrangement. which lowers operating efficiency as well as fabric and garment quality. Indigo Dyeing Quality – The newer designs of Loopdye are reported to have little of the problems with Cross-Shade (side-to-side) shading than with slasher dyeing equipment. especially of sulfurs. With the newer methods for cold-sulfur dyeing. some companies like Vicunha have had success using a combination of Loopdye and slasher dyeing. the slasher dyeing with its greater number of application boxes offers more flexibility in product development.
Based on my 30 years of experience in this area.denimsandjeans. including as a consultant in about 40 denim operations worldwide. 2011 by Harry Mercer | Filed under Manufacturing Process. the first rope dyeing machine appeared and only in the 1970‟s was sheet dyeing introduced.http://www. This is a guest post by Harry Mercer Until 1915. The relative advantages of rope as opposed to sheet Indigo machines is a common subject of debate. most Indigo dyeing was conducted in skein machines for cotton or loose fiber dyeing for wool.com/denim/manufacturing-process/indigo-dyeing-with-loop-dyeingmachinery/ Rope Dyeing Vs Slasher (Sheet) Dyeing May 19th. In 1915. here are some basic observations that I have . Skein dyeing of Indigo is still the best method for dyeing Indigo on very fine yarns for the delicate high-fashion fabrics.
VERSATILITY IN DENIM PRODUCT DEVELOPMENT Rope ranges have been designed to apply the widest range of dyeing techniques. B. only about 66 kilograms of 100% hydrosulfite are required for the basic reaction. The surface losses of hydrosulfite are related to the volume and surface area of the dye boxes. but also in many denim companies that employed both. but also consistent application of all other cotton dyes such as vats. weaving efficiency and overall fabric quality. benchmarking. There is often hydrosulfite wasted incurred in the initial mixing of the stock mix. In explanation. The time for half-oxidation (50% loss) is inversely proportional to the SSA. However the most significant source of loss is through surface contact and air brought into the dye tank by yarn. the yarn ropes can be blended to remove the side to side effects. The greater the SSA (the quotient of the surface area and volume). which refers to differences in color from side-to-side in the fabric. the more rapidly the sodium hydrosulfite is oxidized. the Spectrum Dye Machine available from Morrison contains features like additional steamers and drying sections that allow not only the standard dyeing techniques of sulfur bottoming and topping. in order to reduce 100 kilograms of pure Indigo so that dyeing can proceed. These evaluations included mass-balance studies. Lower consumption of reducing agent per kilogram of yarn.made in companies that had only sheet or rope dyeing. In rope ranges that are designed with that style of circulation there is also some difference in the yarn color from to side-to-side. It should also be noted that rope ranges have the advantage in regards to Cross Shade Variation(CSV). but unlike sheet ranges where the yarns are fixed in their final fabric position. For example. The scientific explanation for this phenomenon is related to what is known as Specific Surface Area (SSA). reactives and directs in combination with Indigo or dyeing yarns with these dye classes only. The instability of hydrosulfite in smaller Indigo boxes is also the primary cause of color variation in Indigo dyeing. which means that decomposition is slowest in a large dye tank with a relatively small surface area. CSV is basically a result of dye circulation system design where the Indigo enters the dye box from the side instead of the front. The primary reducing agent utilized in Indigo dyeing is sodium dithionite. due to excessive stirring or concentrations of hydrosulfite greater than 80 grams per liter which promotes anerobic decomposition. A great deal of hydrosulfite is lost because of contact with atmospheric oxygen at the surface of Indigo dye boxes as a result of aerobic decomposition. A. which on rope ranges is much better controlled. commercially known as sodium hydrosulfite. The amount of hydrosulfite actually consumed in Indigo dyeing is often3 or 4 times this amount. The amounts of this reducer that are consumed in Indigo dyeing are greatly in excess of what is necessary for the Indigo dyeing itself. with approximately 15% loss in larger Indigo boxes found on rope ranges and 50% or more in the smaller dye boxes found on sheet ranges. There are other factors involved such as the initial concentration of hydrosulfite in the dye boxes – a higher initial concentration decomposes more slowly. . There have been some newer designs of Loop indigo machines which have greatly improved CSV.
Another important cause of high weaving breaks in denim is dirty yarn – the cleaner the yarn the higher the weaving efficiency. This is because chemicals not washed from the yarn after Indigo dyeing result in bad sizing and lower protection of warp yarns. yarns from different dyeings such as Indigo only and sulfur only. lowering efficiency and increasing off quality. have very high levels of yarn tension and therefore higher weaving breaks than yarn dyed on rope ranges. Wash boxes on rope ranges are typically more efficient than the smaller wash boxes on sheet ranges that use overflow washing methods. HIGHER PRODUCTION AND FABRIC QUALITY Common methods of operating Indigo machines have a damaging effect on yarn quality which results in very high warp breaks in weaving. Yarn on the machines is made weaker as yarn tension increases. Rope ranges are also easily adaptable for random effects such as space dyeing of yarn. A yarn quality that would result in 10 warp breaks per million weft insertions without Indigo dyeing often will have around a break level of 200 with sheet dyeing. Sheet Indigo machines. The importance of washing the yarn dictates that it is better not to apply softeners in the final box for rebeaming efficiency which is optimal though improved washing and moisture control after drying. or with only a sulfur color. can be blended for producing stripe patterns. but as low as 15 if processed on rope machines. The need for a separate rebeaming step in rope dyeing is often considered objectionable in rope dyeing. since yarn breaks can be repaired at rebeaming .Also available are specially designed dye boxes that allow the simultaneous dyeing of 2 different sulfur applications. because they are attached to size machines. but this is actually an important advantage. With the rope design. C. such as one set of yarn with a sulfur topping and the other set without topping. which allows flexibility in production. This is because tension on rope machines is much lower and can be easily controlled at very low levels.
higher priority fabric orders can be processed without delays resulting from the need to complete a dye set as with sheet dyeing. from 1 to 50 ropes can be dyed at one time. http://www. Also. D. This is a very critical operation carried out in the Dye houses in a series of steps. There are today available latest and state-ofthe-art dyeing methods that effectively colour the various substrates.denimsandjeans. which avoids the waste of yarn which occurs when sheet ranges must stop in order to change yarn lots. Yarn breaks from warping and dyeing cannot be repaired in sheet machines because they are passed directly from dyeing to sizing. Any combination of yarns can be processed for completely different fabric constructions at the same time and dyed with the same Indigo color.com/denim/manufacturing-process/rope-dyeing-vs-slasher-sheet-dyeing/ dyes & pigments B2B MARKETPLACE Manufacturers Directory | B2B Trade Offers | Trade Fairs & Events | Global Dyestuff Industry Colour Index Dyes Pigments Applications Machinery Glossary FAQ's Buyers Guide What is Dye | Types of Dyes | Dye House | Dyeing Process | Dyeing Machinery | FAQs on Dyes | Buyer's Guide to Dyes Dyeing Process basically discusses what you do with the dyes. In a rope range. rope ranges can be operated continuously without stopping. FLEXIBILITY IN PRODUCTION Sheet ranges are usually limited to producing yarn for only 1 weaving set at a time. Because the yarn is sized separately.resulting in higher weaving efficiencies. The pages here gives precious information regarding the various dyeing processes in different industries. normally 12 ropes will produce enough yarn for a weaving set and because rope ranges do not pass the yarn directly to the size machine. Buyer's Guide to Dyes • Buyers Guide to Dyes • Buyers Guide to Pigment • Related Articles .
Dyeing Process » Continuous Dyeing Process Batch Dyeing Process Continuous Dyeing Process Semi-continuous Dyeing Process Pigment Dyeing Process The working of a continuous dyeing process is described here. space dyeing. A Continuous dyeing process typically consists the following. Optimizing the Continuous dyeing Process . Some of the popular methods in continuous dyeing process are Pad-steam. Dye application. thermosol dyeing. but the design ranges for them is unlike that for flat fabrics. dye fixation with heat or chemicals and finally washing. Continuous dyeing has been found to be most suitable for woven fabrics. Wet-steam. Sometimes Nylon carpets are also dyed in continuous processes. That is more for continuous dyeing as compared to batch dyeing. One important factor that separates continuous dyeing from batch dyeing is the tolerance factor for color variation. Mostly continuous dye ranges are designed for dyeing blends of polyester and cotton. TAK dyeing. The step of padding plays a key role in the operation of continuous dyeing. The speeds can vary between 50 to 250 meters per minute. Very good examples of such warp dyeing are long chain warp dyeing and slasher dyeing using indigo. b) presence of a large number of process variables which affects dye application. This is so because of two reasons a) the speed of the process. The textile substrates are feeded continuously into a dye range. According to Industry estimates Continuous dyeing is a popular dyeing method and accounts for around 60% of total yardage of the products that are dyed. and pad-steam dyeing long chain warp dyeing etc. A continuous dye range has been found useful and economically sustainable for dyeing long runs of a given shade. Warps are also dyed in continuous process. The process that is illustrated below is designed for dyeing of blended fabric of polyester and cotton.
Important to know that it should be strictly according to the measurement of the pick up: o A proper measurement of the dyeing liquor quantity consumption in comparison to the processed fabric. Using any of the following systems for dosing of the padding liquor. Typically. Streams of variety color dyes are applied in different patterns to create those special effects. As a result of this. They gets mixed only at the moment just before the delivery to the applicator. Generally acid dyes are used. A continuous dye range for carpet typically consist of a steamer and a dye applicator. with steps that are based on on-line measurement of the pick up. Applying low add-on liquor application systems along with minimising of volume capacity of the dip through when pad dyeing techniques are in operation. application method is used to meter the dye solution into the carpet. o Application of the technique of rapid batch dyeing.Continuous and to some extent semi-continuous dyeing processes both are less prone to water consumption than batch dyeing. Patterned effects are produced when the stream of dye that is metered onto the carpet are momentarily interrupted. The following steps may prove useful. Adoption of latest dispensing systems. but results in high concentration of residues. many variations of dye applicators exist.html Continuous Processing of Cotton woven fabric: A general process sequence may be as below: .dyespigments. This proves better than those dyestuff that is kept prepared already for the whole batch before the commencement of the dyeing batch.com/continuous-dyeing-process. Here the dyestuff solution is prepared just in time. To increase washing efficiency based on the proven principles like reduction of carry-over and countercurrent washing. The resulting values thus obtained are processed automatically and applied in preparing the next comparable batch. a very high liquor ratio is must to produce good quality dyeing of carpet. If some strict control measures are taken up it is possible to reduce this losses of concentrated liquor. where the chemicals get dispensed on-line as separate streams. Under normal circumstances. Carpet manufacturers are very adept in application of dye for producing special color effects on their product. What gives Carpet its vibrant colour? The carpets that you see in different colour and hues is dyed by a continuous dyeing. Site Designed and Maintained by Dyes and Pigments http://www.
Singeing & Desizing: Recipe: Bactosol HC = 5 g/l Common Salt = 5 g/l Wetting Agent (100%)= 3 g/l i. Recipe: 1. 4 dips – 1 nip @ 90 mtrs/minute speed. 2. a. ii. Neutralization 5. c. Recipe: 1. Desize washing in 4 compartments @ 90mts/minute speed. b. Cold Wash in 2 compartments (4 dips – 1 nip) x 2 b. . Sodium Hypochlorite = 2 g/l Avl Cl2 2. Scouring or Boiling 3.PRETREATMENT PART: 1. Singe & Desize (Semi Continuous process) 2. Ready For Dyeing (RFD stage). Neutralizing 8. Peroxide Impregnation: i. Steaming @ 105°C for 45 minutes in the steaming chamber. Lissopal D paste = 10 gram/liter a. Bleaching (Continuous Process)a. Recipe: 1. Peroxide Bleaching 4. No washing c. Hydrogen Peroxide(50%) = 3 ml/liter 1. Dwell time in J box – 30 to 45 minutes at room temp. Drying 6. Caustic Impregnation: i. J-BOX Bleaching optional i. c. Mercerising and washing off to a pH of 6 7. Drying 9. Caustic Soda = 70gram/liter 2. batch. 3. b. and keep rotating the batch for 8 hours. Do cold padding with the above chemicals.
Mercerisation: (Chainless Merceriser) i. 3. 4 Dips – 1 Nip at cold. Steam in Peroxide Steamer for 45 minutes. compartment – strength = 1.5. 4.0 g. Recipe: 1. nd compartment – temp = 65 to 95°C e. Washing in 5 compartments with each 4 dip and 1 nip. Mangle Pressure: 3. Recuperation: i. 3. Tank 3 – 60 to 70°C iv. Bleached Fabric = 25 mtrs/minute ii. 1 st compartment – temp = 90 to 95°C 2 2 iii. Final fabric pH – 5. Scoured Fabric = 20 mtrs/minute b. Drying: nd T T . b.4 gpl iv. Wash Tanks: i.6 to 6.2 to 4 kg/cm2 c. Dry and batch on A frame roller. Cold Padding Speed: i. Grey Fabric = 15 mtrs/minute iii. 1 st compartment – strength = 8 to 27 gpl ii.2. Caustic Soda = 280 to 300 gpl 2. Stabilizer = 0.5 gram/liter a. Liquor Pickup : 110% d. Permenol N = 10 g/l a. ank 1 – 50 to 55°C ii. ank 2 – Acetic Acid Neutralizing iii. Wetting Agent room temp f.to 6.
PAD LIQUOR PREPARATION for VS dyes: G/L 10 20 30 40 50 >50 G/L 0~50 0~50 0~50 50~70 50~75 50~75 G/L 5 10 15 15-18 20 20-25 10 10 10 10 10 10 Dyestuff Urea Sodium Bicarbonate Resist Salt G/L . Dye Liquor Preparation & recipe: a. Chemical Pad Recipe: Dyestuff G/L Caustic Soda Salt (g/l) Soda Ash (g/l) < 20 Nil 200 20 30 – 40 Nil 250 20 > 40 Nil 250 20 5. Pad-Dry-Steam: 1. Liquor Pickup 70 to 80% 7. Steaming 45-90 seconds with Saturated steam (101 to 105°) the steam should be free from acid. Mild Oxidizing Agent = 5-10 gram/liter 2. There are 3 methods: i. F abric is dried in cylinder or stenter and batched as RFD. 2.i. Continuous Dyeing Method for 100% Cellulose: a. Cotfix Dyestuff = x grams/liter b. Liquor Pick up% = 60 to 80 4. 4. ii. Pad – Dry – Chemical Pad – Steam 1. Antimigartion agent = 8-10 gram/liter d. To fix the dyestuff. Chemical Padding Temperature < 35°C 6. the dried material is steamed in the normal continuous steamer for 4 to 7 minutes at 100 to 103°C. This is carried out on a padding mangle attached with either Hot Flue or Flow Dried. Wetting Agent = 2-3 gram/liter c. Padding Temperature should be < 35°C 3.
Soaping with 2 g/l of soaping agent (Sandopur RSK) at 90°C e. Hot wash in one compartment (soaper) @ 80° . 2nd soaping with 1 g/l soaping agent (Sandopur RSK) at 90°C f. After treatment: a. Soda Ash Method b.3. Here again there are 2 processes: a. Squeezed on the last mangle and either plaited or wound on a batcher and taken for drying. Overflow Cold wash in soapers 4 dip 1 nip in 2 compartments b. . Sodium Bicarbonate Method PAD LIQUOR PREPARATION for VS dyes Dye G/L 2 10 20 40 60 Urea G/L 15 30 45 60 80 Soda G/L 8 12 17 25 33 Ash(OR) Sodium G/L 12 18 27 36 45 Bicarbonate The material is padded in the above liquor at room temperature. Hot Wash g. Neutralization with Acetic Acid in the soaped at cold with 2 ~3 g/l Acetic acid. 4 dip 1 nip in d. iii. c. Hot Wash h. Pad-Dry-Thermo fix Process: 1. Cold Wash i. Take all the precautions and conditions mentioned for Pad –DryChemical Pad-Steam.Bicarnonate process 5-7 minutes 3-5 minutes 60-90 seconds 5. dried & thermo fixed as follows: Temperature 100°C 120°C 140°C Soda Ash Process 4-6 minutes 2-4 minutes 40-60 seconds Sod.5 g/l j. Acetic Acid Treatment 1 g/l or Formic Acid treatment 0.
Expression of the squeezing mangle is to be checked at frequent intervals. c. Final Alkalinity of the mercerized fabric should be less than 0. Tailing: The Alkalinity in the mercerized fabric would be un-uniform ranging from 0. C/S Variation – may arise due to 1. Desizing – Expression of the squeezing mangle is to be checked at frequent intervals. 4. S team Pressure ii. 3. Mercerising – Impregnation Mangle expression has to be checked. Any variation in the alkalinity of the mercerized fabric can show up through the length by the dye affinity difference and that is tailing. Check Point: i. That means more and more alkalinity would be carried over on the mercerized cloth and that can be checked in lab by titration. 2.25 to 1 and above gram/liter due to inefficient recuperation. a. Caustic Impregnation .Possible Faults that may occur during the above process and check points/rectification: 1. Alkalinity of the mercerized cloth has to be quantitatively checked in the lab at intervals of 500 meters. Peroxide Bleaching: i. Soaper washing – Acid for neutralization should be prepared in volume and should be fed in to the neutralization tank continuously. . It must be uniform. ii. 2. To counter check. b. a.25 g/l of caustic. Time duration of the steaming are to be controlled. the fabric absorbency may be checked in the center and the two selvedges at regular intervals. Recuperator Efficiency has to be checked at every 1000 meters. S team Temperature iii.
out of the two bottom rollers. c. b. About 40 liters of hot water at 85°C is added to the slurry which is kept under a high speed stirrer. The quantity of the dyestuff is to be pasted. 5 liters of soft water should be used for pasting. dyeing. d.com/faq/continuous-dyeing. Specky Dyeing: a. Thermosol temperature difference between faces may result in migration of dyestuff. The hot water should be added slowly to the rotating vertex of the dye slurry.a uniform circle shows proper dissolution. V.thesmarttime.3.htm Dyeing of Reactives by Exhaust Method . ii. finishing etc. ME. one is not rotating properly then back to face variation is possible. HE = 80°C. Then 1 kg of urea is dissolved in 5 liters of water and this solution is added in the paste and stirred well to make a uniform lump less slurry. In jigger dyeing machine. e. iii. The dissolved dyestuff may be spotted on a filter paper . Face to back variation a. M-Brand = 50°C 2.S = 80°C 3. XL. In a 2 dip 2 nip mangles. 4. In stenters. http://www. there may be face to back variation. say for 1 kg of dyestuff. then back to face variation is possible at any stage. if the expression of both the mangle are not identical. if the hot air blowers are not functioning. The filter this dissolved dyestuff through a fine gauze. Mangle Expression in the dye padding should be 70% and chemical padding should be 80%. Temperature of dissolution: 1. Improper dissolution of dyestuff: i.
No other class of colours can boast of the versatile range of shades with unmatched brilliance. The . Even as Reactive dyes are most popular for dyeing solid shades it is equally sought after for various resist and discharge printing styles. yet economically viable and cost effective that this class of dyes can offer. Influence of Substantivity Migration phase Secondary Exhaustion Hydrolysis of Reactive dyes Typical Examples REACTIVE DYES Choice of Reactive class of Dyes has become indispensable for application of colours on the cellulosics to provide bright range of shades with reasonably good fastness features.DYEING OF REACTIVE DYES BY EXHAUST METHOD REACTIVE DYES EXHAUSTION PHASE Primary Exhaustion Phase Adsorption Diffusion Substantivity REACTIVE DYES AND DIRECT COTTON DYES Direct Cotton Dye Reactive Dyes Role of Electrolyte Partition /Distribution Coefficient and Degree of Exhaustion Liquor Ratio Temperature Influence of pH. it reacts with Water also to get hydrolyzed in which state the dye behaves no better than a direct cotton dye. formation of covalent bonds between the reactive group of the dye and the OH of cellulose proceeds. thanks to its suitability to be resisted or discharged readily and effectively The reaction mechanism is apparently simple in that on just altering the pH after exhaustion. For the same reason of ready reactivity with Cell OH groups.
4 Beta Glucoside link (OH of #2 to #6 of the succeeding glucose unit and #3 OH with the ring O of the preceding Glucose Unit) that stabilize the cellulose chain. fastness etc multifold. The exhaust method of dyeing would include the following phases 1. 3. reproducibility. Secondary exhaustion phase. 4.management of the various factors/variables that govern the transport of dye uniformly from an aqueous bath to the cellulose substrate and its preferential reactivity to the fibre than to water is far more complex and critical to perform to obtain a satisfactory dyeing. Tubular knit-ware. advanced machineries obtainable in recent years claim satisfactory open width dyeing by Pad Batch technique. the behaviour of individual dyes with different exhaustion and reactivity characteristics. Fixation (Reaction) phase -Secondary exhaustion and Fixation can run concurrently/over lapping. Primary exhaustion phase /Migration 2.1Alpha and 1 Beta of Cellulose molecular chains that are packed compactly and there are intra molecular Hydrogen bonding parallel to the 1. Absorption/ Exhaustion/Migration Adsorption It would be relevant to briefly look at cellulose structure with respect to its Hydrogen bonding behaviour at the surface layers and in the interiors of the cellulose micro fibrils The interior layers contain both forms . by its very physical form is more amenable to exhaust dyeing in „rope„s form. Washing off phase. all the more compounds the complexity of the problems of differential shade build up. uneven dyeings. . pad – dry-cure or pad-dry-steam etc exhaust dyeing is practiced widely because of its flexibility to process fabrics in rope form and in the case of yarn and other packages. Top EXHAUSTION PHASE Primary Exhaustion Phase Exhaustion of dye from the dye bath to the cellulose during Primary Exhaustion phase is governed by the following three physical processes and the phenomenon of substantivity Adsorption Diffusion. exhaust dyeing is the only alternative as on date. however. Though there are other methods of dyeing „Reactives‟ like pad batch. variations. As the shades invariably are tertiary matchings.
The zeta potential is partially overcome due to the presence of large amount of dye anions. That is the starting phase for the rest of the diffusion and absorption phenomenon. with abundance of „free‟ OH groups available at the surface (six numbers in each of the repeat Cellobiose unit). some of which are forced across the electron cloud through increase in energy (raise in temperature) or through mechanical agitation to come within the effective distance for the inter molecular forces like Wander Vaal‟s forces/secondary valence forces to facilitate the dye anion to get adsorbed on the surface of cellulose. In the case of Cellulose exposed to a dye solution in water at slightly acidic pH there is no ionization of cellulose. (Discussed under „Role of Electrolyte‟) . Presence of electrolyte also helps in providing the positive charge that can effectively neutralize the zeta potential and improve the adsorption. water molecules are drawn in clusters around the cellulose molecules to form hydrogen bonds causing an overall charge separation. However.The other four hydroxyl groups are fully free for Hydrogen bonding. Adsorption in an exhaust dyeing process is fundamentally the inter-phase phenomenon of a dye (solute) in its solution in water coming in to surface contact with the substrate and forming a surface layer/ coating. Resultant surface thus carries a negative charge known as the zeta potential This surface negative charge would repel the advances of the negatively charged ionized dyestuff anions. At the surface layers of cellulose even the O-3 (OH) and 2-6 Hydrogen bondings are reported to be absent and therefore all the six Hydroxyl groups in the Cellobiose repeat units at the surface are free to attract Hydrogen bonding with the water molecules.
F is the dyestuff sorbed across Unit area of the fiber surface in unit time (Rate) (C1-C2) concentration gradient during the process of diffusion. the surface area of the cotton substrate in contact with the dye bath. Higher the Diffusion coefficient.) F= -D (C1-C2) / L And D = Do e -E/RT Where F = Mass flow of dye gms/cm2 sec D = Diffusion coefficient of the dye m2/sec D0 = Diffusion Coefficient at Infinite Temperature C1 = Concentration of dye in the dye bath g/cm3 C2 = Concentration of dye on surface of the fiber g/cm3 L = Thickness of the layer cm e. temperature and time and the physical characteristics of the substrate. Time taken for dyeing 50% of the equilibrium depth of shade is an index of the speed Increase in Temperature increases Diffusion coefficient. Diffusion is influenced by the concentration gradient across the interface of cellulose surface and dye bath. Top Diffusion Diffusion process is explained by the relationship (Ficks Law of Diffusion in its simplest form. absorption diffusion and migration in that order. R Universal Gas Constant) T = Temperature Kelvin Applying the above relationship the following dynamics may be inferred during the diffusion / exhaustion stages of the dye to the cotton substrate. The concentration gradient at the initial stages would be higher and therefore the rate of dyestuff transport to the fibre phase will be correspondingly higher tending towards zero at equilibrium. E. This is termed as the primary exhaustion phase. R = Constants (E activation Energy. lesser the time taken to reach the equilibrium. The term exhaustion would include the collective phenomenon of adsorption. D Diffusion coefficient Temperature .Diffusion phenomenon takes over followed by the absorption and migration of dyestuff across the cellulose membrane. Greater the surface area of the fiber in contact with the dye bath greater is the dyestuff sorbed. e exponential.
. at the present status of Colouration technology. substantvity by primary exhaustion of Reactive dye to cellulose cannot be improved or maximized. The corollary is that thinner the fibre/count and lower the density factor greater is the surface area available and better would be the diffusion. cross section.Since surface area is a factor. micronaire. the temperature and the fibre surface area characteristics. Substantivity ratio is the unit concentration of dye on the fibre to the unit concentration of dye in the bath at the equilibrium state (both expressed in the same units) The process of primary exhaustion proceeds to its limiting values dictated by the substantivity beyond which it ceases. etc and different packing densities of the cellulose molecular chains thus altering the surface area characteristics. This is influenced by the salt concentration in the dye bath. without salt additions. In the absence of salt. Nature of cotton from different sources would have different shape. the liquor ratio. as a general rule. impurities. the characteristics of the fiber and construction would influence the diffusion. Therefore. the dye uptake by substantivity phenomenon as stated above is around 20 to 40% of the starting bath concentration or lower. besides the chemistry of the dye chromophore. Top Substantivity The term substantivity is primarily a measure of the amount of the molecular dye chromophore that can penetrate/diffuse into the interstices of cellulose micro fibrils assisted by physical forces from an aqueous dye bath. a figure far too low to have any significant economically feasible colour yield. fineness.
to provide the heat energy to facilitate diffusion and migration. Molecules of sufficiently large enough size and shape that on aggregation could get trapped in the interstices of the Cellulose molecular chains thus difficult to be removed/washed off.[Efforts are on for reduced salt /salt-less systems based on changes in the chemistry of the dyes to exhibit reduced anionic behaviour. More number of hydrogen bonding groups. there is less propensity to desorb and higher . groups that would facilitate inter molecular attraction / diminish repelling forces and groups that can chelate with hydroxyl groups of the Cellulose 2. Optimized number of solubilizing groups (invariably „-SO3Na‟). metal chelation etc. Higher temperatures can also cause de-aggregation and consequent de-sorption Since the dyes have good substantivity due to affinity caused by physical forces like Hydrogen bonding. The Reactive dyes are smaller sized more akin to Acid class of dyes (not necessarily as a general rule) with Reactive groups. while retaining the reactive system for the ultimate fixation. just enough for the dye to go in to aqueous solution. 3. fibre substrate modification/sensitization to display cationic behavior to induce exhaustion with less/no salt. Dyeing is invariably carried out at boil. Such developments are still in the R&D Labs and not presently available for bulk] Top REACTIVE DYES AND DIRECT COTTON DYES Reactive and Direct Cotton dyes sport similar dye chromophoric structures but for the Reactive groups present in the Reactive dyes as opposed to Direct cotton dyes.. Direct Cotton Dye Direct Cotton Dyes molecules are engineered to include some or all of the important features listed below 1.
Migration is facilitated by increase in temperature. Reactive Dyes with features listed under I and 2 of the Direct cotton dyes would exhibit problems of low migration and or difficulty to wash off the hydrolyzed dye. Where . Some of them could be counter productive. All of the features that are desirable for a reasonably „fast to wash‟ Direct Cotton dyes are not essential for Reactive class of dyes (because of the more strong covalent bond). Top Reactive Dyes Reactive Dyes are capable of forming chemical covalent bonds with the Hydroxyl groups of cellulose fibre and therefore. 2.. 3. 6.temperatures facilitates migration within the substrate forming the same physical bonding at new sites (High substantivity always causes an initial „strike‟ – aggregation of colour in most favourable loosely packed sites and migration to other sites to increase uniformity in dyeing is facilitated only by imparting energy. There fore. irrespective of high levels of success achieved in the exhaustion stages. Top Role of Electrolyte Addition of electrolyte induces exhaustion both its rate and extent. The migration of the dye within the substrate during the primary exhaustion phase should be maximized. 4.) Fastness characteristics are just adequate even for the most satisfactory dyes of its class due to bonding only by physical forces that are relatively week to the more powerful covalent bonds. 5. Efficiency of reaction of the exhausted dye to the fibre should be maximized during fixation phase. but higher temperatures induce hydrolysis of Reactive dye during the fixation phase and therefore it would be necessary to bring down the temperature to the most favourble temperature for the reaction between dye stuff and substrate before alkalie addition can be made. Degree of Exhaustion of the dye bath on to the fibre (both primary and secondary) that is directly related to the substantivity should be maximized /optimized (assisted more by salt addition than by the physical forces). better anchored to the substrate and not depend on the relatively weak physical forces to give better levels of fastness.. For example. The corollary here is that the extent of hydrolysis of the dye during exhaustion and fixation stages needs to be minimized. in the case of Reactive dyes the following aspects are most important 1. though exhaustion is an important (primary and or secondary) pre-requisite. The above four aspects need to be performed within a reasonable span of time. The kinetics of reactivity has the final influence on the success of dyeing. Certain quantity of Hydrolyzed dye is inevitable after the fixation stage and non removal of such unfixed dye would entail bleeding/staining of white during washing. though cannot be totally discarded as undesirable.
.e. dyes displaying higher substantivity in the absence of salt would need lesser salt concentrations. say. The Partition/Distribution coefficient of a solute between two phases is calculated as the ratio of the concentration of the solute in one phase to the concentration of the solute in the other phase under equilibrium conditions . Higher the diffusion coefficient faster the exhaustion as discussed earlier under diffusion.The distribution coefficient of dye therefore shifts towards fibre.i. extent of hydrogen bonding groups. The degree of exhaustion increases with increasing concentrations of Salt to a limiting concentration.e. Secondly. where the number of molecules absorbed is equal to the number of molecules desorbed at the cellulose/dye liquor interface. the exhaustion of the dye proceeds from the liquor phase to the solid phase (cellulose) until it reaches an equilibrium.the substantivity is lower the prime driving mechanism for diffusion /exhaustion of dye into the fibre is the concentration gradient across fibre/liquor interface and presence of common ion. ionic character. electrolyte (Salt). This state would be different for different solutes (dyestuffs) and the factors that contribute to this variability are their molecular size. at the end of Exhaustion phase or Partition of the dye from the liquor phase to the solid phase at a notional infinite time It is desirable that the exhaustion proceeds at a satisfactory rate to achieve close to equilibrium exhaustion within a manageable /practicable time span a condition that is influenced by diffusion coefficient. Higher concentrations of Salt result in aggregation of the dye in the dye bath itself and hence „it is salted out‟ much in the same manner as in the manufacture of the dyestuff and less and less monomolecular dyes are available for reaching the fibre phase The optimal quantity of Salt in terms of concentration depends on the chemistry of the dye. Sodium Chloride dissociates in water into Na+ and Cl and Na+ has higher propensity to travel to the fibre /water interface and neutralize the negative charge thus facilitating the free transport of dye anion to be adsorbed onto the surface of the fibre and the subsequent diffusion/ absorption (exhaustion) to take place.. quality of water and the fibre substrate etc. the dissociated NaCl ions are more associated with water than with the large molecular dye Chromophore with a few SO3Na or other solubilizing groups and thus occupy the limited available sites in the water effectively displacing the dye Chromophore. its solubilizing groups. Such equilibrium. Top Partition /Distribution Coefficient and Degree of Exhaustion At a given liquor ratio and bath concentration of dyestuff and salt. i. Secondly. The electrolyte. can safely be assumed to have been reached in a time span of infinity. inter molecular forces. its molecular size. temperature etc. It is not the quantity of the salt but its concentration that influences the degree of exhaustion.
does not do so linearly but progressively diminishes giving relatively lower distribution coefficient values. at the equilibrium state of exhaustion where the concentrations of dye on fibre and in the final bath tend to become steady and constant. In an ionic kind of reactions like Acid dyes on wool the degree of exhaustion would proceed to almost to ..100% subject to the dye present in the dye bath does not exceed the saturation capacity of the reacting sites present in the substrate. the concentration in fiber phase at equilibrium though increases. it is an established fact that as the dye bath concentration is increased. Degree of exhaustion is the ratio of the total amount of dye present in the cellulose at the end of exhaustion to the amount of dye present in the original bath before the start of the exhaustion process.Interestingly. Degree of Exhaustion in terms of distribution coefficient and liquor ratio is given by the relationship Where E Degree of Exhaustion K Partition coefficient L Material Liquor Ratio Top Liquor Ratio Recipe of x% owf (on weight of fabric) in terms of absolute quantity would be present in the starting dye bath but its concentration in the dye bath would vary depending on the liquor ratio The recipe equivalent dye % on the fabric after the completion of dyeing would not be x% but would tend towards x% .the limiting degree of exhaustion in this case.depending on the efficiency of dyeing/the substantivity /reactivity of the dye. In a model scenario where the liquor ratio is changed to a higher one: Amount of dyestuff expressed owf. when present in the higher liquor .
The corollary is that a change in liquor ratio would affect the least in dyes with high substantivity and most in those with poor substantivity Top . In case 1 starting from 1:10 going to 1:5. any increase in L would diminish the E –the degree of exhaustion. There are ready reckoners for recipe correction available for changes in liquor ratios from the dyestuff manufacturers but they are only for guidance. The relationship E= K/ (K+L) as discussed under Distribution coefficient (K).and therefore the rate of diffusion will be lowered and it would take relatively far longer time to reach the equilibrium state.0 Kgs Liquor Ratio 1: 5 1:10 I 2 *Arrow indicates‟ tending towards‟ Only 50% of the dye molecules are available at the interface for adsorption and diffusion in case 2.ratio would register proportionately a lower concentration of the dye in the starting bath and consequently lower concentration gradient at the fibre liquor interface resulting in lesser rate of diffusion of the dye from liquor phase to fiber phase Numerical Example Liquor Volume (Wt) 500L 1000L Dye bath Concn. but also that of salt will be necessary (barring certain marginal cases) quantitative aspects governed by the substatnivity characteristics of the dyestuff. But increased salt addition cannot always fully compensate for the adverse exhaustion behaviour but only to a point (as discussed under Role of Electrolyte) Therefore. As individual dyes would behave differently. Such a situation would entail higher starting concentration of the dye and or increase in concentration of Salt to „occupy the available sites in water‟ (as explained earlier under salt concentration) in a larger volume of water to displace the dye anion to shift the distribution coefficient to the fiber phase.0 Kgs 1. the increased concentration of dye in the bath would increase the rate of diffusion (increased concentration gradient) and take shorter time for exhaustion. Such a situation would be more pronounced in the case of low/poor substantive dyes compared to the dyes with better substantivity. not only increase in concentration of the dye. an intelligent understanding and application of the given information only can give meaningful results. 2 gpl 1 gpl Case Recipe owf 1% 1% Substrate Amount of Weight dye on fibre* 100 Kgs 100 Kgs 1.
also requiring less concentration of salt for exhaustion but for the same reason migration of the dye would be restricted resulting in unlevel dyeing. energy and mechanical efforts . beyond which increase in temperatures results in decreasing degrees of exhaustion explained by the higher degree of de-aggregation of the dye in the fiber phase and lesser physical forces to resist desorption. annulling the influence of salt. Influence of Substantivity High substantivity facilitates exhaustion process.. High substantivity . As long as the pH of the bath is slightly acidic.dyes with low reactivity (Fixation) falling below the exhaustion levels would result in high levels of unfixed and hydrolyzed dye to be washed off and the dye and its hydrolyzed version also being highly substantive. but relatively less in fiber phase and more in the water phase. Top Influence of pH. The pH is relevant to the Reactivity aspect and not considered as a factor in the exhaustion process. Therefore the net effect is that there are more deaggregated monomolecular dye free to move towards the fiber phase than that is desorbed from the fibre and therefore the exhaustion proceeds.5 to 6. Also. There is a maxima in the exhaustion curves of dyes of low substantivity at temperature around 40 to 50 deg C. both in fibre and water phases. the dye bath pH during the exhaustion phase is maintained at 5. Poor substantive dyes that are also not sensitive to electrolyte additions are poor builders and therefore will give poor yields. the washing efforts also will be high requiring more water. unlike in the case of substantive direct cotton dyes. However dyes with medium+ substantivity engineered to provide the balance in the molecular structure to promote migration and good reactivity that matches the exhaustion curve (primary and secondary) would give the best results both in terms of dye yield and washing efficiency. no reaction can take place and therefore primary exhaustion and bringing the temperature close to the reaction temperatures can be carried out conveniently.Temperature Temperature of the bath is another factor influencing exhaustion As explained earlier presence of salt increases the substantivity facilitating aggregation of the dye in the fiber phase Increase in temperature in the case of high substantive dyes as in the case of direct cotton dyes help in the migration of the dye within the substrate but in the case of dyes that are less substantive increase in temperatures could be counterproductive Temperature up to 50 deg C contributes to de-aggregation of the molecules of dye.
When Alkali is added.it is anchored strongly and cannot be shifted. Migration phase should precede the fixation phase as once the reactive dye forms a covalent bond with Cell O. the hydrolysis of the Reactive dye with water) in competition to the fixation of the dye that is the primary aim. When more and more of dye anions are covalently bond.and H+ (Cell O– Na+) and starts forming covalent bonds with the reactive functional groups of the dye Chromophore. the cellulose ionizes to form Cell-O.Top Migration phase Since fiber surface area is a factor in diffusion process. primary exhaustion alone does not govern the efficiency of dyeing. In a trichromatic mixture the situation could be worse. During the secondary exhaustion when alkalie is added. The other external factors would relate to temperature. Raising the temperature would provide the required thermal energy. The process of Migration of the exhausted dye depends on the molecular size of the dye its spatial profile (Steric) and the solubilizing groups present. the distribution coefficient shifts to fiber phase effecting further exhaustion due to deficiency of dye anions in the cellulose phase and dye bath concentration starts depleting further. Any exhaustion during this stage if it is hydrolyzed dye it would be far more undesirable In a reactive dye system therefore. machinery used and the package profiles and densities (in case of package dyeings). The degree of secondary exhaustion also would influence the efficiency. but cannot be increased arbitrarily due to limitations discussed under „Temperature‟. Both exhaustion and migrations can be maximized /improved by better mechanical agitations that would facilitate intimate surface area contact of the cellulose with dye liquor and by improved flow designs that facilitate better liquor exchange at the fiber liquor inter-phase. Such a situation would result in uneven build up of the dye both in hue and intensity. the exhaustion would proceed to locations where relatively more surface area is presented like in the amorphous areas and less densely packed crystalline areas in that order in the cellulose and therefore the dye concentration within the cellulose substrate would not be uniform/even. The dye anion is equally facilitated to react with OH of water to form the hydrolyzed dye in which state the dye is .e. there is a second reaction that also sets in motion in parallel ( i. Top Secondary Exhaustion The observations and inferences in the above deliberations related to primary exhaustion in a Reactive exhaust dyeing process are incomplete without the final fixation. The degree of alkalinity in terms of pH plays a major role in shifting the fixation of dye to its hydrolysis reacting with water.
) Top Hydrolysis of Reactive dyes The most critical part of the Reactive dyeing is the actual fixation where the covalent bond takes place between the Cellulose O .CH2-OR1 Where [-O-R1] is [-O Cellulose] or [-OH] of water. etc. 1. . Given the right temperatures.5 for High (cold dyeing).as good as a direct dye with all its „undesirable‟ characteristics. 60 º C and 80º. Vinyl Sulphones Dye-SO2 –CH2-CH2-OSO3H CH=CH2 (MINUS) H2SO4 Dye SO2- The electron attracting Sulphone group causes electron deficiency on the terminal carbon atom enabling neucleophylic attack to take place. It is the reactive group in the dye. alkalinity and time the reaction proceeds to completion in all cases. It becomes critical that the hydrolysis is curbed to maximize efficiency. The relationship between temperature and reactivity is that higher temperatures require lower alkalinity. 11.0 for Low (Hot Dyeing) for the reaction to proceed more favorably towards the substrate.levels of pH 12. . Efficiency of Reactive dyeing (Rate of Fixation /Rate of Hydrolysis) for a given exhaust dyeing process has been expressed in mathematical terms .11.CH2-OR1 Dye-SO2-CH 2. to optimize on hydrolysis. pH and temperature that influence the hydrolysis of dye in preference to reacting with cellulose.5 for Medium (Warm) and 10 .C respectively . The term more reactive is used in the sense that it requires lesser levels of alkalinity and lower temperatures (and not the reaction itself. They can be broadly grouped under „High‟ „Medium‟ and „Low‟ categories requiring 40º C. (Addition reaction) Dye-SO2-CH=CH2 + O-R1H (+) Dye-SO2-CH -.and the Reactive group of the Dye Chromophore. The liberated acid in both the two reactions is continuously neutralized by alkalie for the forward reaction to proceed during the fixation process. Cynuryl chloride based dyes 2.
hydrolyzation of the unexhausted dye close to the substrate phase and in the dye bath also starts and it would become critical to control minimize this aspect of the reaction. 1. To whatever extent the variables can be controlled and maintained. On addition of alkalie the reaction starts and the secondary exhaustion proceeds as more and more of the dye takes part in the reaction. That would require precision instruments /plc controls. Secondly since the exhaustion is low and better part of the dye exhaustion takes place in the secondary phase. However. Substantivity and R are high Primary exhaustion would be high and whatever exhausted would be fixed.making use of the competing First order /pseudo first order rate constants of the reaction of the dye with the cellulose and the dye hydrolysis with water .SDC Publication} It has also been emphasized that the expression is too ideal and relates to certain assumptions and conditions that are not practically achievable in the real situation. Low Primary exhaustion (P) and high Reactivity (R) (incidentally higher secondary exhaustion) Where P is low and Fixation is high Initial exhaustion phase will not be critical as less amount of dye is transported. During this phase the competing reaction . the equilibrium concentration of the dye on fabric and concentration of dye in the aqueous phase (For details please refer Chapter 4 of „The Dyeing of Cellulosic Fibres‟ by Maurice R Fox and Harry H Sumner Edited by Clifford Preston 1986 . The direction and rate of reaction towards covalent bonding with substrate have to be controlled by careful manipulation of pH and temperature. the following few examples will highlight the pros and cons of the factors discussed. Where P. In this . the broad principles are applicable and the direction of the reactions proceeds towards the ideal. migration would be affected and the dyeing would be non uniform. Top Typical Examples Reviewing the critical variables that govern the dyeing Efficiency in a Reactive dyeing process. the results achieved could be optimized and also reproduced maintaining the same conditions and controls every time.
case it would be critical during exhaustion phase as the substantivity is high and migration could be a problem. Higher temperatures need to be resorted to for migration and that would not be in favour with Dyes of the low reaction temperatures in view of its high reactivity. The dyestuff manufacturers themselves recommend colours that have similar . a good exhaustion percntage including the seondary exhustion that are achievabe within a paracticable time dimension and reactivity that matches the degree of exhaustion so that all the exhausated dye is fixed. Because of the high reactivity pH control to maintain low and constant alkaline pH through out the reaction/fixation phase would be critical. Such a situation would warrant graduated salt additions to avoid initial strike – linear or step wise in order to facilitate phased migration. It could be possible to standardize on an isothermal dyeing sequence starting with salt bath The desirable features of the dyestuff would be to posess reasonbly good substantivity and migration capability. It would require cooling if higher temperatures were to be adopted. Such a dyeing would require least effort for soaping. migration would be better facilitated. The individual process house labs can conveniently assess substantivity of the dyes and group them for using in their recipe mixtures. This would mean ideally that the curves S and F should super impose at the concluding stages of the dyeing process. Top Evaluation of Substantivity A very useful and simple practical method to assess substantivity of the Reactive dyestuffs in the lab based on chromatographic principles is given in the article “Effects of Dye Substantivity in the Dyeing of Cotton with Reactive Dyes” a prize winning article By Canadian Association of Textile Colourists and Chemists in TCC Nov 91). In the above example where the substantivity before salt addition is relatively lower but enhanced by salt addition. Depending on the hot or cold class of colours the temperature maintenance will be critical. However such an ideal system is not practicable but efforts should be to move towards the ideal system Dyes with similar substantivity that are moderate and having good primary exhaustion (assisted by salt addition) and migration potentials and also a relatively lower secondary exhaustion with reactivity reaching close to equilibrium exhaustion would be the most suitable choice where auto dozing and sophisticated control systems are not available.
P. No. Evaluation of Migration Index Ref. however it would be safe to assess in ones own lab unless supplied by propriety manufacturers.J. Vol.material Practical method to evaluate migration Index “Reactive Dye Selection and Process Development for Exhaust Dyeing of Cellulose” BY M. Collishaw and S. 8 http://www. ZENECA Colours.com/index.substantivity features. Moorhouse. August1995. Bradbury.springsamsolutions. Blackley. S.php?option=com_content&task=view&id=55&Itemid=85 . 27. England.
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