Asia Pacific – Continuous dyeing of indigo

DyStar Continuous Dyeing of Indigo

Regional Business Development Denim

Page 1 June 2003

Asia Pacific – Continuous dyeing of indigo

Co te t Content
1. 2. 3. 4. 5. 6. 7. 8 8. 9. General overview DyStar Product Offer Dyeing machinery and principle Pretreatment Dyeing Metering system Guideline recipes Aft t Aftertreatment t t Conversion factors for caustic soda
Page 2 June 2003

Regional Business Development Denim

Asia Pacific – Continuous dyeing of indigo

1. Ge General ea O Overview e e Indigo d go
¾ ¾ ¾ ¾ ¾ Main application is the continuous dyeing of warp yarn for denim fabric. The indigo pigment is a water-insoluble vat dye (no affinity to cotton). Indigo is converted to its water-soluble leuco form by reduction (affinity to cotton). cotton) With DyStar Indigo Granules the reduction process (vatting) takes place in the stock vat. DyStar Indigo Vat 40% Solution and DyStar Indigo Vat 60% Grains have been reduced by hydrogenation process during their manufacture. Preparation of a stock vat is therefore unnecessary with both these products.

Regional Business Development Denim

Page 3 June 2003

Asia Pacific – Continuous dyeing of indigo 2. cottage g industry y applications pp z Wool. Regional Business Development Denim Page 4 June 2003 . DyStar ySta Product oduct O Offer e Product D t Indigo Dystar I di G Granules l DyStar Indigo Vat 40 % Solution Characteristics/main application area z Low L d dusting ti z Denim z Prereduced product z No stock vat preparation z Up to 70 % saving in hydrosulfite z Contains 9 % NaOH z Denim DyStar Indigo Vat 60 % Grains z Prereduced product z Contains 15 % NaOH .

Dyeing 3 ye g machinery ac e y and a d principle p cpe ¾ Rope dyeing: The yarn is assembled into ropes of about thumb thickness. which is dyed in the open-width open width form. 4000) from several section-warp beams are assembled to form a warp warp.Asia Pacific – Continuous dyeing of indigo 3. Before sizing sizing. the ropes are opened and the warp ends wound onto section-warp beams. ¾ Slasher dyeing: The ends (approx. form sized and then wound onto beams for the loom. 12 – 36 ropes (1 – 3 warps) are run through the dyeing range side-by-side side by side. Regional Business Development Denim Page 5 June 2003 . each containing round 350 ends.

provided that leader is used Disadvantages z The Th ropes must t be b “opened” “ d” after ft dyeing z Lack of flexibility y owing g to the large g dyebath volume (up to 40000 l) z Additional costs for softener to facilitate opening of the ropes Regional Business Development Denim Page 6 June 2003 .1 Dyeing 3 ye g machinery ac e y – Rope ope Dyeing ye g Advantages z High Hi h rate t of f production d ti z No stoppage with lot changes z No p possibility y of side-to-center shade variations in the finished fabric z Little yarn wastage.Asia Pacific – Continuous dyeing of indigo 3.

2 Dyeing 3 ye g machinery ac e y – S Slasher as e Dyeing ye g Advantages z Compact C t range z Fine yarns (shirting materials) can be processed ( p (up p to Ne 40/1) ) z Continuous production from sectionwarp beam (undyed) to sized warp beam (dyed) z Small dyebath volume (1500 – 8000 l) z Allows flexible change in process z Produces maximum ring dyeing changes Regional Business Development Denim Disadvantages z Possibility P ibilit of f side-to-center id t t shade h d variations in the finished fabric z Yarn wastage g from lot changes g z Short immersion times and/or a small number of dips – which are particularly likely with older dyeing ranges – result in a lower standard of fastness with dark shades z Relatively long stoppages during lot changes Page 7 June 2003 .Asia Pacific – Continuous dyeing of indigo 3.

¾ The dyebath can consist of one box only or be made up of several boxes. e. Regional Business Development Denim Page 8 June 2003 . i.3 3 3 Dyeing ye g p principle cpeI ¾ The dyeing process on indigo-dyeing ranges is carried out in a number of dips. the warp yarn is passed through a dyebath several times.Asia Pacific – Continuous dyeing of indigo 3. usually from 4 – 8.

Asia Pacific – Continuous dyeing of indigo 3.3 3 3 Dyeing ye g p principle c p e II ¾ Dipping ƒ ƒ ¾ ƒ ƒ ƒ ¾ ƒ immersion time 4 – 20 s reduced indigo exhausts onto the cellulosic fibre Squeezing 70 – 80% liquor pick-up contributes to rapid oxidation improves the fastness Air passage the hydrosulfite and the indigo is oxidized Page 9 June 2003 Regional Business Development Denim .

Asia Pacific – Continuous dyeing of indigo 3.4 Dyeing 3 ye g machinery ac e y a and dp principle cpe Regional Business Development Denim Page 10 June 2003 .

“salt and pepper”) z Can be carried out on all dyeing ranges Without pretreatment z Only for slasher dyeing ranges z Gives good ring dyeing z Higher risk of streakiness zAddition of wetting agent to the dyebath necessary Regional Business Development Denim Page 11 June 2003 . g.Su Survey ey Process P Prewetting tti Boiling off Causticizing Process Application z Standard St d d process f for slasher l h d dyeing i ranges z Standard process for rope dyeing ranges z Process to obtain extreme ring dyeing and/or special effects (e. Pretreatment et eat e t .Asia Pacific – Continuous dyeing of indigo 4.

1 Prewetting e ett g ™ 3 g/L wetting agent e. Primasol NF (BASF) Temperature: room temperature Immersion time: at least 6 s Replenishment: by level control ™ Rinse cold Regional Business Development Denim Page 12 June 2003 .Asia Pacific – Continuous dyeing of indigo 4.g.

2 Boiling o g off o ™ 10 –15 mL/L NaOH 50% 1-3 2-4 g/L sequesting agent e.g.g.Asia Pacific – Continuous dyeing of indigo 4. Trilon TA (BASF) Temperature: 90º C Immersion time: at least 10 s Replenishment: by level control ™ ™ 2 x rinse hot (approx. Kieralon MFB (BASF) g/L complexing agent e. 60º C) Rinse cold Regional Business Development Denim Page 13 June 2003 .

Regional Business Development Denim Page 14 June 2003 .Asia Pacific – Continuous dyeing of indigo 4.g.4 g/L complexing agent e.22º Bé 4 g/L wetting agent e.3 3 Caust Causticizing c g ™ NaOH 12 .g. the liquor must be replenished with NaOH of 22 °Bé. Leophen MC (BASF) 2 . Trilon TA (BASF) Temperature: room temperature Immersion time: 10 – 15 s Replenishment: by level control To maintain a NaOH concentration of 20 °Bé in the causticizing box.

60 °C) Rinse cold several times g with subsequent neutralization Causticizing ƒ ƒ ƒ ƒ Causticize 1– 2 x rinse hot ( (approx.Asia Pacific – Continuous dyeing of indigo 4.3. pp 60 °C) ) Neutralize/acidify 1– 2 x rinse cold Page 15 June 2003 Regional Business Development Denim .1 3 Caust Causticizing c g with/without t / t out neutralization eut a at o ¾ Causticizing without subsequent neutralization ƒ ƒ ƒ ¾ Causticize 2 – 3 x rinse hot (approx.

Asia Pacific – Continuous dyeing of indigo 5. Maintaining the dyebath parameters constant reduces the number of these groups and also the proportion of “off shades”. the finished denim material is classed into groups according to the dyeing results and the appearance after washdown. As a rule. Regional Business Development Denim Page 16 June 2003 . Dyeing 5 ye g Irregular dyeing results – particularly variations within dyeing lots – are a problem in denim production.

Asia Pacific – Continuous dyeing of indigo 5.1 Process 5 ocess Parameters a a ete s I Parameter R d Reduced di indigo di Nature of the change Ri i Rise in concentration t ti Fall in concentration Indigo pigment content Increase Effect z Increase I in i depth d th of f shade h d z Decrease in depth of shade z Lowers the fastness z Less contrast in wash-down Decrease Immersion time Extending z Improves the fastness z Greater dye penetration z Increase in depth of shade Shortening z More pronounced ring dyeing z Decrease in depth of shade Regional Business Development Denim Page 17 June 2003 .

. clearer Lowering z Lowers the pH z More p pronounced ring g dyeing y g z Shade becomes greener.5 Regional Business Development Denim Page 18 June 2003 .Asia Pacific – Continuous dyeing of indigo 5.2 Process 5 ocess Parameters a a ete s II Parameter Caustic C ti concentration Nature of the change R i i Raising Effect z Raises R i th the pH H z Greater dye penetration z Shade becomes redder. duller z Risk of formation of the vat acid at pH <11.

Asia Pacific – Continuous dyeing of indigo 5.2 Process 5 ocess Parameters a a ete s III Parameter Hydrosulfite H d lfit concentration Nature of the change R i i Raising Effect z Greater dye penetration z Shade becomes greener. clearer z Lowers the pH z More pronounced ring dyeing z Promotes oxidation of the indigo in p g the air passage z Risk of increased formation of indigo pigment in the dyebath z Risk of bronzy dyeings z Shade becomes redder. duller z Raises the pH Page 19 June 2003 Lowering Regional Business Development Denim .

200 threads (magnification 7 : 1) Regional Business Development Denim Page 20 June 2003 .3 5 3 Examples a p es o of p pH variation a at o – deg degree ee o of ring g dyeing dye g pH 13.2 pH 11.5 Cross-section of a yarn bundle with approx.Asia Pacific – Continuous dyeing of indigo 5.

5 Surface view of a yarn bundle Regional Business Development Denim Page 21 June 2003 .Asia Pacific – Continuous dyeing of indigo 5.4 Examples 5 a p es o of p pH variation a at o – c change a ge in s shade ade pH 13.2 pH 11.

0 g/L excess hydrosulfite Surface view of a yarn bundle Regional Business Development Denim Page 22 June 2003 .4 Examples 5 a p es o of hydrosulfite yd osu te variation a at o – c change a ge in s shade ade 0.Asia Pacific – Continuous dyeing of indigo 5.5 g/L excess hydrosulfite 2.

1 Stoc 6 Stock vat at without t out c chemical e ca replenishing ep e s g add additions to s DyStar Indigo Granules NaOH Hydrosulfite Auxilliaries ¾Little flexibility when there is a change in the style to be dyed ¾Little flexibility when it is necessary to change the processing parameters ¾instable because of d decomposition iti of f hydrosulfite h d lfit ¾not recommended Regional Business Development Denim Page 23 June 2003 .Asia Pacific – Continuous dyeing of indigo 6.

Asia Pacific – Continuous dyeing of indigo 6.2 Stoc 6 Stock vat at with t sepa separate ate c chemical e ca replenishing ep e s g add additions to s DyStar Indigo Granules NaOH Hydrosulfite Auxilliaries NaOH Hd Hydrosulfite lfit ¾Most frequently used method ¾More flexible than the stock vat method without chemical replenishments ¾Does not allow automatic pH control ¾limited stability of dissolved h d hydrosulfite lfit Regional Business Development Denim Page 24 June 2003 .

3 6 3 Stoc Stock vat at with t sepa separate ate c chemical e ca add additions to sa and d metering ete g of the caustic soda DyStar Indigo Granules NaOH Hydrosulfite Auxilliaries NaOH Hd Hydrosulfite lfit NaOH ¾Particularly flexible ¾Processing parameters can be readily changed by altering the setting of the metering pumps ¾Allows automatic pH control ¾Allows several dyeing ranges to be supplied from one mixing station t ti ¾The recipes for the stock vat and chemical replenishment need not be changed ¾limited stability of dissolved hydrosulfite Regional Business Development Denim Page 25 June 2003 .Asia Pacific – Continuous dyeing of indigo 6.

Asia Pacific – Continuous dyeing of indigo 6.4 DyStar 6 ySta Indigo d go Vat at 40% 0% So Solution ut o with t separate sepa ate c chemical e ca replenishment additions DyStar Indigo Vat 40 % Solution Storage tank NaOH Hydrosulfite ¾No stock vat preparation ¾Dye metered direct from the storage tank ¾Particularly flexible ¾Allows automatic pH control Regional Business Development Denim Page 26 June 2003 .

5 6 5 DyStar ySta Indigo d go Vat at 40% 0% So Solution ut o with t separate sepa ate c chemical e ca additions and metering of the caustic soda DyStar Indigo Vat 40 % Solution Storage tank NaOH Hydrosulfite ¾No stock vat preparation ¾Dye metered direct from the storage tank ¾Does not allows automatic pH control NaOH Regional Business Development Denim Page 27 June 2003 .Asia Pacific – Continuous dyeing of indigo 6.

g. Setamol WS (BASF) 4 – 8 g/L 1 70 65 g/L mL/L NaOH 50% g/L hydrosulfite Regional Business Development Denim Page 28 June 2003 .1 Stoc Stock Vat at Preparation epa at o I ™ 80 1 g/L g/L DyStar Indigo Granules wetting agent e.g.Asia Pacific – Continuous dyeing of indigo 7. Primasol NF (BASF) complexing agent e.g. Trilon TA (BASF) dispersing agent e.

The mix is finally stirred again for 30–60 s. vatting of the indigo is completed in 2 – 3 hours Page 29 June 2003 Regional Business Development Denim . Add caustic soda Slowly strew in hydrosulfite.Asia Pacific – Continuous dyeing of indigo 7. Depending on the temperature. 75% of the final volume Add auxiliaries Strew in and disperse indigo.1 Stoc Stock Vat at Preparation epa at o II ™ ™ ™ ™ ™ ™ ™ Fill cold water into the mixing vessel to approx. Stirring for 3 – 5 min dissolves the hydrosulfite. Fill up with water to the final volume.

i The Th amounts t prepared d should h ld be b such h that th t they th are consumed within 60 – 90 min . Regional Business Development Denim Page 30 June 2003 .2 C Chemical e ca replenishment ep e s e t ™ 135 g/L 70 mL/L hydrosulfite NaOH 50% Temperature: room temperature ™ Chemical liquors should be stored under cool conditions and protected from exposure to t air.Asia Pacific – Continuous dyeing of indigo 7.

3 3 Dyebath yebat p preparation epa at o ™ 40 g/L 2 mL/L salt (common salt or Glauber salt) NaOH 50% hydrosulfite stock vat (cf.1 corresponds to 1 g/L DyStar Indigo Granules. followed by addition of the stock vat. Page 31 June 2003 Regional Business Development Denim .5 mL/L of the stock vats described in 7. caustic soda and hydrosulfite.1) = 2.Asia Pacific – Continuous dyeing of indigo 7. 12.0 g/L DyStar Indigo Granules 1. 7.5 g/L 5 ™ ™ mL/L The dyebath is set cold with salt.

7 pH 6 dips 75 % liquor pick-up Regional Business Development Denim Page 32 June 2003 .4 kg/min yarn throughput 1.8 % indigo concentration based on weight of yarn 0.5 g/L hydrosulfite concentration 11.4 Example a p e ca calculation cu at o I ™ 7 Ne yarn 4000 number of ends 25 m/min running speed 7.Asia Pacific – Continuous dyeing of indigo 7.

6 6 L/min replenishment 80 65 70 g/L Dystar Indigo Granule g/L hydrosulfite mL/L NaOH 50% ™ Chemical liquor : 0.4 Example a p e ca calculation cu at o II ™ 130 g/min 250 g/min 190 mL/min replenishment of DyStar Indigo Granules replenishment of hydrosulfite replenishment of NaOH 50% ™ Stock vat at : 1 1.Asia Pacific – Continuous dyeing of indigo 7.7 L/min replenishment 135 g/L hydrosulfite 70 mL/L NaOH 50% Regional Business Development Denim Page 33 June 2003 .

¾ With rope-dyeing ranges. 30% and are then sized.Asia Pacific – Continuous dyeing of indigo 8. a softener should be used. The last rinsing bath to facilitate rebeaming rebeaming. Regional Business Development Denim Page 34 June 2003 . better. ¾ Warp yarns dyed on slasher machines are given an intermediate drying to a residual moisture content of approx. warm water of up p to 50 °C to wash out any y unfixed dye y and chemicals. Aftertreatment 8 te t eat e t ™ ¾ 2 – 3 x rinse hot (up to 50 °C) The dyed warp yarns are rinsed at least twice with cold or.

63 N OH 48 °Bé 441 g NaOH 100% 1358 g ™ Regional Business Development Denim Page 35 June 2003 .74 L NaOH 38 °Bé 1.09 L NaOH 48 °Bé 766 g NaOH 100% 1525 g 0.Asia Pacific – Continuous dyeing of indigo 9. Co 9 Conversion e s o factors acto s Caust Caustic c soda I ™ 1 L NaOH 50% 1 L NaOH 50% 1 L NaOH 50% 1 L NaOH 50% % 1 L NaOH 38 °Bé 1 L NaOH N OH 38 °Bé 1 L NaOH 38 °Bé 1 L NaOH 38 °Bé = = = = = = = = 1.57 L NaOH 50% 0 63 L NaOH 0.

Asia Pacific – Continuous dyeing of indigo 9.30 L NaOH 50% 2 27 L NaOH 2.59 L NaOH 38 °Bé 700 g NaOH 100% 1500 g 1. Co 9 Conversion e s o factors acto s Caust Caustic c soda II ™ 1 L NaOH 48 °Bé 1 L NaOH 48 °Bé 1 L NaOH 48 °Bé 1 L NaOH 48 °Bé = = = = 0.43 L NaOH 48 °Bé ™ 1 kg NaOH 100% = 1k kg N NaOH OH 100% = 1 kg NaOH 100% = Regional Business Development Denim Page 36 June 2003 .91 L NaOH 50% 1.27 N OH 38 °Bé 1.