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
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Asia Pacific Continuous dyeing of indigo

1. Ge General ea O Overview e e Indigo d go

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.

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Asia Pacific Continuous dyeing of indigo

2. 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 , cottage g industry y applications pp z Wool,
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Asia Pacific Continuous dyeing of indigo

3. Dyeing 3 ye g machinery ac e y and a d principle p cpe

Rope dyeing: The yarn is assembled into ropes of about thumb thickness, each containing round 350 ends; 12 36 ropes (1 3 warps) are run through the dyeing range side-by-side side by side. Before sizing sizing, the ropes are opened and the warp ends wound onto section-warp beams.

Slasher dyeing: The ends (approx. 4000) from several section-warp beams are assembled to form a warp warp, which is dyed in the open-width open width form, form sized and then wound onto beams for the loom.

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Asia Pacific Continuous dyeing of indigo

3.1 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, 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

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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
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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
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Asia Pacific Continuous dyeing of indigo

3.3 3 3 Dyeing ye g p principle cpeI

The dyeing process on indigo-dyeing ranges is carried out in a number of dips, usually from 4 8, i. e. the warp yarn is passed through a dyebath several times.

The dyebath can consist of one box only or be made up of several boxes.

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Asia Pacific Continuous dyeing of indigo

3.3 3 3 Dyeing ye g p principle c p e II

Dipping 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

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Asia Pacific Continuous dyeing of indigo

3.4 Dyeing 3 ye g machinery ac e y a and dp principle cpe

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Asia Pacific Continuous dyeing of indigo

4. Pretreatment et eat e t - 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. g. 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
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Asia Pacific Continuous dyeing of indigo

4.1 Prewetting e ett g

3 g/L wetting agent e.g. Primasol NF (BASF) Temperature: room temperature Immersion time: at least 6 s Replenishment: by level control

Rinse cold

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Asia Pacific Continuous dyeing of indigo

4.2 Boiling o g off o

10 15 mL/L NaOH 50% 1-3 2-4 g/L sequesting agent e.g. Kieralon MFB (BASF) g/L complexing agent e.g. Trilon TA (BASF) Temperature: 90 C Immersion time: at least 10 s Replenishment: by level control 2 x rinse hot (approx. 60 C) Rinse cold

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Asia Pacific Continuous dyeing of indigo

4.3 3 Caust Causticizing c g

NaOH 12 - 22 B 4 g/L wetting agent e.g. Leophen MC (BASF)

2 - 4 g/L complexing agent e.g. Trilon TA (BASF) Temperature: room temperature Immersion time: 10 15 s Replenishment: by level control

To maintain a NaOH concentration of 20 B in the causticizing box, the liquor must be replenished with NaOH of 22 B.
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Asia Pacific Continuous dyeing of indigo

4.3.1 3 Caust Causticizing c g with/without t / t out neutralization eut a at o

Causticizing without subsequent neutralization Causticize 2 3 x rinse hot (approx. 60 C) Rinse cold several times

g with subsequent neutralization Causticizing Causticize 1 2 x rinse hot ( (approx. pp 60 C) ) Neutralize/acidify 1 2 x rinse cold
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5. Dyeing 5 ye g
Irregular dyeing results particularly variations within dyeing lots are a problem in denim production. As a rule, the finished denim material is classed into groups according to the dyeing results and the appearance after washdown. Maintaining the dyebath parameters constant reduces the number of these groups and also the proportion of off shades.

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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
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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, , clearer Lowering z Lowers the pH z More p pronounced ring g dyeing y g z Shade becomes greener, duller z Risk of formation of the vat acid at pH <11.5

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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
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Lowering

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Asia Pacific Continuous dyeing of indigo

5.3 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. 200 threads (magnification 7 : 1)

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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 11.5

Surface view of a yarn bundle

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Asia Pacific Continuous dyeing of indigo

5.4 Examples 5 a p es o of hydrosulfite yd osu te variation a at o c change a ge in s shade ade

0.5 g/L excess hydrosulfite

2.0 g/L excess hydrosulfite

Surface view of a yarn bundle

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Asia Pacific Continuous dyeing of indigo

6.1 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

Little flexibility when there is a change in the style to be dyed Little flexibility when it is necessary to change the processing parameters instable because of d decomposition iti of f hydrosulfite h d lfit not recommended

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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

Most frequently used method More flexible than the stock vat method without chemical replenishments Does not allow automatic pH control limited stability of dissolved h d hydrosulfite lfit

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Asia Pacific Continuous dyeing of indigo

6.3 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

Particularly flexible Processing parameters can be readily changed by altering the setting of the metering pumps Allows automatic pH control Allows several dyeing ranges to be supplied from one mixing station t ti The recipes for the stock vat and chemical replenishment need not be changed limited stability of dissolved hydrosulfite

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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

No stock vat preparation Dye metered direct from the storage tank Particularly flexible Allows automatic pH control

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Asia Pacific Continuous dyeing of indigo

6.5 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

No stock vat preparation Dye metered direct from the storage tank Does not allows automatic pH control

NaOH

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Asia Pacific Continuous dyeing of indigo

7.1 Stoc Stock Vat at Preparation epa at o I

80 1 g/L g/L DyStar Indigo Granules wetting agent e.g. Primasol NF (BASF) complexing agent e.g. Trilon TA (BASF) dispersing agent e.g. Setamol WS (BASF)

4 8 g/L 1 70 65 g/L

mL/L NaOH 50% g/L hydrosulfite

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Asia Pacific Continuous dyeing of indigo

7.1 Stoc Stock Vat at Preparation epa at o II

Fill cold water into the mixing vessel to approx. 75% of the final volume Add auxiliaries Strew in and disperse indigo. Add caustic soda Slowly strew in hydrosulfite. Stirring for 3 5 min dissolves the hydrosulfite. Fill up with water to the final volume. The mix is finally stirred again for 3060 s. Depending on the temperature, vatting of the indigo is completed in 2 3 hours
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7.2 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. 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 .

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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. 7.1) = 2.0 g/L DyStar Indigo Granules

1.5 g/L 5 mL/L

The dyebath is set cold with salt, caustic soda and hydrosulfite, followed by addition of the stock vat. 12.5 mL/L of the stock vats described in 7.1 corresponds to 1 g/L DyStar Indigo Granules.
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7.4 Example a p e ca calculation cu at o I

7 Ne yarn 4000 number of ends 25 m/min running speed 7.4 kg/min yarn throughput 1.8 % indigo concentration based on weight of yarn 0.5 g/L hydrosulfite concentration 11.7 pH 6 dips 75 % liquor pick-up
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Asia Pacific Continuous dyeing of indigo

7.4 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 1.6 6 L/min replenishment 80 65 70 g/L Dystar Indigo Granule g/L hydrosulfite mL/L NaOH 50%

Chemical liquor : 0.7 L/min replenishment 135 g/L hydrosulfite 70 mL/L NaOH 50%

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Asia Pacific Continuous dyeing of indigo

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

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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 B 1 L NaOH N OH 38 B 1 L NaOH 38 B 1 L NaOH 38 B = = = = = = = = 1.74 L NaOH 38 B 1.09 L NaOH 48 B 766 g NaOH 100% 1525 g 0.57 L NaOH 50% 0 63 L NaOH 0.63 N OH 48 B 441 g NaOH 100% 1358 g

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Asia Pacific Continuous dyeing of indigo

9. Co 9 Conversion e s o factors acto s Caust Caustic c soda II

1 L NaOH 48 B 1 L NaOH 48 B 1 L NaOH 48 B 1 L NaOH 48 B = = = = 0.91 L NaOH 50% 1.59 L NaOH 38 B 700 g NaOH 100% 1500 g 1.30 L NaOH 50% 2 27 L NaOH 2.27 N OH 38 B 1.43 L NaOH 48 B

1 kg NaOH 100% = 1k kg N NaOH OH 100% = 1 kg NaOH 100% =

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