Indigo Dyeing Methods – Engineering

Color, Wash Fastness And Fashion Effects

Harry MercerMarch 5, 20118

This is a guest post by Harry Mercer. This is a very technical description – read on if you are
technically oriented..

Here are given some important dyeing processes related to indigo dyeing – specially on Rope
Dyeing .

Pre Treatment
Pre-treatment is conducted in the 1st tank. The most common pre-treatments are :

1.  Sulfur bottoming

2.  Scouring with sodium hydroxide

3.  Causticizing or Mercerizing

Pre- Treatment : Sulphur Bottoming

•The purpose of sulfur bottoming was to:

 Originally to produce a dark shade on denim using less Indigo for lower costs
 In the U.S. sulfur bottoms were dyed using a combination of blue and black dyes
 In denim operations outside the U.S. the bottom is normally dyed with sulfur black

Pre – Treatment : Cotton Scouring

Cotton fibers contain impurities like waxes, pectins and minerals that will interfere with
Indigo dyeing and result in streaks.-Sodium hydroxide at low concentrations (<5%) are
applied at high temperatures (>85 C) in order to remove impurities and melt natural cotton
waxes.

Pre – Treatment : Causticizing

 Causticizing generally refers to using sodium hydroxide at below Mercerizing
concentrations (<18%).
 Cold causticizing of cotton yarn results infaster Indigo dye fading from
laundryabrasion, darker Indigo color with the same % of Indigo and unique
washdowns.
 Hot causticizing improves colorfastness
Pre – Treatment : Mercerizing
Mercerizing is the use of strong sodium hydroxide (18-30%) to swell surface fibers.

Caution:

 When using strong sodium hydroxide it is important to remove all of it.

 If sodium hydroxide is on the yarn as it enters the Indigo tanks, the yarn color will
change.
 Concentrations of sodium hydroxide more than 18% are not a solution, but a gel
and are difficult to remove.
 Mercerized yarns are more ring-dyed and dye more darkly than non-Mercerized.
 Mercerizing is normally conducted at low temperatures, but hot Mercerizing can be
employed for a more abraded appearance after garment laundering.

Indigo Dyeing
 Indigo dyeing is unique and because of the complex chemical reactions should be
correctly viewed a a form of chemical engineering.
 Only Indigo dyeing requires multiple dye applications for a dark shade.
 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.
 Commonly, 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.

Indigo Dyeing Methods

 Indigo dyeing follows the same basic steps regardless of machine design.
 Scour or dye bottoming in a heated tank,
 washing tanks, dyeing(1-20),a heated tank for topping (optional) and wash tanks.
 In different areas of the world,the same color is produced using 1.8, 2.0 or 4% Indigo
depending on dyeing method.


 
 

Dark Indigo(1.8%) 1. 15% caustic cold

2.Wash 60°C
3.Wash 60°C
4. Wash cold
Drying cylinders hot
Steamer cold
Boxes 5-12 Indigo
Steamer cold
13.Wash 50°C
14. Wash 50°C
15. Wash 50°C
16.Wash 50°C /Softener
Stock Mix 80 g/l Indigo Chemical Feed 120 g/l 50%
Pure 100 g/l 50% Caustic 70 caustic 60g/l Hydro powder
g/l Hydro powder. Feed 1.4 liters per minute

Dark Indigo Color

 This was an example of a typical method used in the U.S. for a very dark shade.
 In order to produce the same depth of color as 1.2% in the U.S., in Latin America
2.0% is used and in Asia from 2.4 to 2.8%.
 The U.S. method results in more surface (ring dyeing), which loses color faster.

Darkest Indigo Shades

 Very dark shades of Indigo are in demand currently around the world.
 Many companies use 4% or more Indigo on weight of yarn, which is expensive.
 2% Indigo will produce the same depth if low levels of caustic are used(0-0.4%)
 For dark Indigo that does not lose color 2% applied normally, with an Indigo bottom.

Light Indigo Shades

 Dyeing Indigo in light shades results in a sky-blue impossible with any other dye.
 This is useful for shirting fabrics that are  not strong enough for stonewashing, 
bleaching or cellulase treaments.
  Special procedures are necessary in order to avoid colorfastness problems.

Light Indigo 0.4% 1. 4% caustic 90°C

2.Wash 60°C
3.Wash 60°C
4. Wash 60°C
Bypass drying cylinders
Bypass steamer
Close off boxes 5-8
Boxes 9-12 Indigo
13. Wash 50°C
14. Wash 50°C
15. Wash 50°C
16.Wash 50°C/softener

Control Of Sulphur Bottoming

 The typical methods used for dyeing sulfur bottoms result in denim shade differences.
 When applied as light colors, sulfur dyes should be dyed at temperatures <60 C,
 If dextrin reducing agents are used, which require 85 C, there will be variation.
 Sulfur bottoms are an exception to the normal pH for sulfurs(11), requiring 12.

Sulfur Bottom 1. Pad sulfur(cold)

Steamer hot
2.Wash cold
3.Wash 50°C
 4.Wash 50°C
Boxes 5-10 Indigo
11. Indigo or wash 50°C
12. Indigo or wash 50°C
Bypass steamer
13. Wash 50°C
14. Wash 50°C
15. Wash 50°C
16.Wash 50°C or softener

Sulphur Topping
 In topping the sulfur dye is applied after the Indigo dyeing.
 Sulfur topping permits much darker color than a sulfur bottom, but is duller.
 Sulfur topping colors include black, blue-black, yellow brown and green.
 Sulfur toppings are used to produce slub appearances in normal yarn.

Sulfur Top 1. Pre-wet 2% caustic 90°C

2.Wash 60°C
3.Wash 60°C
4. Wash cold
By pass drying cylinders
Bypass steamer
Boxes 5-10 Indigo
11. Wash 60°C
12. Pad sulfur topping
Steamer hot
13. Wash cold
14. Wash 50°C
15. Wash 50°C
16.Wash 50°C/Softener

Reactive Dyes in Indigo Dyeing

 Reactive dyes can be applied on specially-Designed Indigo machines.
 Small 150 liter boxes are inserted inside the larger dye tanks for Indigo and
sulfur.
  Steamers, drying units near the front of the machine and high-quality dye padders are
required for quality dyeing.

Pad-Dry Chempad- Steam 1. Pre-scour wetter plus

Reactives chelate 90°C
2.Wash 50°C
3. Pad monochlortriazine dye
cold, neutral pH
Drying cylinders hot
Pad caustic in salt brine
Steamer hot
Bypass boxes 5-10
11. Soap 90°C
12. Soap 90°C
Steamer hot
13. Wash 60°C
14. Wash 60°C
15. Wash cold
16.Wash cold/softener

Pad Steam Reactive 1. Pre-wet 10% caustic 90°C

Topping 2.Wash 60°C
3.Wash 60°C
4. Wash cold
By pass drying cylinders
Bypass steamer
Boxes 5-10 Indigo
11. Wash 60°C
12. Pad Dichorotriazinyl cold
with bicarbonate
Steamer hot
13. Wash cold
14. Wash 50°C
15. Wash 50°C
16. Wash 50°C / softener
Vat Dyeing
 Indigo and sulfurs are types of vat dyes.
 In non-denim cotton dyeing, another class of vats, anthaquinoids are used to
produce a full range of colors that are colorfast.
 Some of these vat dyes can be blended with Indigo or applied using standard
procedures on specially designed machines.

Pad-Dry Chempad Vats 1. Pre-wet 4% caustic 90°C

2.Wash 60°C
3. Pad vat dye cold
Drying cylinders hot
4. Chempad caustic/hydro
cold
Steamer hot
Bypass boxes 5-10
11. Wash 60°C
12. Oxidize
13. Soap with anti-oxidant
Steamer hot
14. Wash 50°C
15. Wash 50°C
16. Wash 50°C / softener

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Pad-Dry Chempad Steam 1. Pre-wet 4% caustic 90°C
Vat Bottom 2. Wash 60°
3. Pad vat dye cold
Drying cylinders hot
4. Chem-pad caustic/hydro
cold
Steamer hot
Boxes 5-10 Indigo
11. Wash 60°C
12. Soap 90°C
Steamer hot
 13. Wash cold
14. Wash 50°C
15. Wash 50°C
16. Wash 50°C

Control Of Indigo Dyeing

The Indigo dyeing process begins with a concentrated mixture of Indigo, sodium hydroxide
and reducing agent.  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.

Dye Mixing Procedures

 Many denim companies find it difficult to control original and washed Indigo shades.
 The primary source of color differences is the instability and inconsistency of Indigo
mixtures.
 As the concentration of reducing agent going to the dye machine changes, the color
changes.

Uniform Indigo Mixtures

 For consistent Indigo dyeing, the mixture must have consistent concentrations of
Indigo, sodium hydroxide and reducer from the top of the mixture to the bottom.
 The main cause of inconsistent Indigo mixtures relates to concentration levels.
 Instability of Indigo mixtures results from the decomposition of sodium hydrosulfite.

Consistency of Concentration
 There is a limit to the amount of any chemical that can be dissolved in water.
  When the limit of solubility of any chemical •In water is exceeded, precipitation
occurs.
 Indigo mixes should not have more than 20% solids. At higher levels, chemicals and
dye sink to the bottom of the tank.

Improving Dyeing Consistency

 When reducing agent sinks to the bottom of the tank, there is a higher concentration 
than in the top of the tank. As the dye enters the machine, the higher concentration
results in a lighter, greenercolor and as the dye from the top of the tank enters the
machine, the color is darker and redder.

Dye Control In Feeding  Tank

 Stirring the tank for 2 minutes will improve dye uniformity between top and bottom.
 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. If dye requires 50 seconds to oxidize, there is about 50 g/L of reducer.

Buffers In Indigo Dyeing

 Alkaline buffers have been used to make very dark shades of Indigo with as little
as 1% dye, more ring-dyed, faster fading.
 Reductive buffers can eliminate color differences in Indigo-dyed denims and can
reduce hydrosulfite use by 30-50%.

Cold Dyeing Methods

 Sulfur colors can be dyed at low temperatures with specific buffers which produce
more colorfast dyeings with no color variation.
 Cold dyeing methods have been used to blend Indigo and sulfurs, eliminating the need
for separate bottoming and topping, while eliminating shade changes in both.

Special Dyeing Techniques

 On rope ranges, space dyeing techniques can be simple and produce a wide range of
special effects in denim.
 By dyeing part of the yarns with a sulfur top and leaving the rest un-dyed, many
companies produce a slub appearance with regular yarns.
 Blending ring yarns of different sizes also produces a slub appearance.

This is a guest post by Harry Mercer. Mr. Mercer has 30 years

experience in the denim business including 3 prominent U.S.
denim companies. He is an expert colorist for measurement and
color matching as well as textile testing.
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