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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

Table of contents
1. 2. 2.1 2.2 2.3 2.3.1 2.3.1.1 2.3.2 2.3.2.1 2.3.2.2 2.3.3 2.3.3.1 2.3.3.2 2.3.4 2.3.5 2.3.6 2.3.7 2.4 2.4.1 2.4.2 2.4.3 2.5 2.6 3. 3.1 3.2 3.3 3.3.1 3.3.1.1 3.3.2 3.3.2.1 3.3.2.2 3.3.3 3.3.4 3.3.4.1 3.3.5 Introduction Pad Batch process Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparation of the pad liquor Dissolving the dyes The alkali liquor Alkali systems Fixation with sodium silicate and caustic soda Fixation with soda ash and caustic soda Pad liquor stability Padding Fixation by batching Washing off Rapid fixation (lab technique) Rapid fixation in a microwave oven Rapid fixation in a drying cabinet Examples Clariant tailing test Shade change during drying Pad Dry Chemical Pad Steam process Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparation of the dye pad liquor Dissolving the dyes Pad liquor stability Padding Intermediate drying Explanation of migration Preparation of the chemical pad liquor 3 3 3 3 3 3 4 4 4 4 4 4 5 5 6 6 7 7 7 8 8 8 9 9 9 9 10 10 10 10 10 10 10 10 11 11 11 3.3.6 3.3.7 3.3.8 3.4 4. 4.1 4.2 4.3 4.3.1 4.3.1.1 4.3.2 4.3.2.1 4.3.2.2 4.3.3 4.3.3.1 4.3.3.2 4.3.4 4.3.5 4.3.6 4.4 5. 5.1 5.2 5.3 5.3.1 5.3.1.1 5.3.2 5.3.2.1 5.3.3 5.3.4 5.3.4.1 5.3.5 5.3.5.1 5.3.5.2 5.3.6 5.3.7 Padding Fixation by steaming Washing off Shade change during drying Pad Wet Steam process Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparation of the pad liquor Dissolving the dyes The alkali liquor Pad liquor stability Pad liquor stability with a metering pump Pad liquor stability without a metering pump Padding Fixation by steaming Washing off Shade change during drying Pad Thermofix process Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparation of the pad liquor Influence of the urea Dissolving the dyes The alkali liquor Working without a metering pump Pad liquor stability Pad liquor stability with a metering pump Pad liquor stability without a metering pump Padding Intermediate drying 11 12 12 12 12 12 12 13 13 13 13 13 13 13 14 14 14 14 14 14 14 15 15 15 15 15 15 15 16 16 16 16 16 16 16 16 16

4.3.2.2.1 Working without a metering pump

3.3.4.1.1 Clariant migration test

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

5.3.8 5.3.9 5.4 6. 6.1. 6.2 6.3 6.3.1 6.3.2 6.3.3 6.3.4 6.3.5 6.3.6 6.3.7 6.3.8 6.3.9 6.4 7. 7.1 7.2 7.3 7.3.1 7.3.1.1 7.3.2 7.3.2.1 7.3.2.2 7.3.3 7.3.4 7.3.5 7.3.6 7.3.7 7.3.8 7.3.9 7.4 8.

Fixation in hot air Washing off Shade change during drying Pad Moist process Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparing the dyestuff pad liquor Dissolving the dyestuffs The alkali liquor Pad liquor stability Padding Drying/Fixation Washing off Shade change during drying SWIFT process for dyeing PES/CEL blends Introduction Process principle Operating procedure Fabric requirements Sewing together the pieces Preparation of dye pad liquor Dissolving the dyes Pad liquor stability Padding Intermediate drying Thermosoling Preparation of the chemical pad liquor Padding Fixation by steaming Washing off Shade change during drying Dye selection

16 17 17 17 17 17 17 18 18 18 18 18 18 18 18 19 19 19 19 19 20 20 20 20 20 20 20 20 21 21 21 21 21 21 21

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

1. Introduction
In continuous dyeing processes, the substrate is treated far more gently than in exhaust processes, i.e. on jets or in package dyeing machines. For large batches continuous processes are often far more economical. Most of the Drimaren HF and CL dyes are

2.2 Process principle


The principle of the pad batch process is to pad the goods at room temperature with a dye solution which also contains the necessary alkali for fixation and any other chemicals. The fabric is rolled up on a beam and wrapped in plastic film ready for the fixation step. Dye fixation takes place during batching at room temperature. Slow rotation of the fabric batch is necessary during batching to avoid unlevelness and drainage of the dye liquor.

suitable for the continuous processes described in this shade card.

2. Pad Batch process


2.1 Introduction

The fabric is batched for the required fixation time before the unfixed dye is removed from the fibers by rinsing then soaping at the boil. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade.
Dye pad liquor Batching

2.3 Operating procedure


The pad batch process is a semi-continuous dyeing method which is extremely interesting from the point of view of both the machinery and the application technique. The only machines required are a padder, batching device and washing off equipment.

Various factors, which are important for a reliable process flow, are described in the following sections: The prepared state of the material to be dyed Preparation of the pad liquor Padding Fixation by batching The washing off process

In view of the steadily increasing cost consciousness in the textile processing industry, this economical, time and energy-saving process is of considerable importance. This shade card contains detailed information in the text section about the technique of this process which will ensure its reliable application in the dyehouse.

2.3.1 Fabric requirements The pad batch process offers the following decisive advantages:

Optimum, uniform pre-treatment of the substrate is one of the most important fundamentals for obtaining perfect dyeing results with regard to levelness and appearance of the fabric, etc.

Simple working method Short setting up and machine down time Low machine and energy cost High color build-up Good penetration even with tightly structured goods Economic process

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The pre-treated fabric should fulfill the following criteria for perfect results:

Before adding dissolved dyes to the feed tank the dye liquor should be passed through a filter to ensure that any non-dissolved dye or contamination is held back. Unlevelness and/or spots and possible damage to the pumps can be avoided in this way. Cold water should then be used to adjust the dye liquor to the required volume.

Uniform moisture content, very good absorbency (prevent over drying) and crease free Neutral pH (6-7) and uniform degree of whiteness (important for pale shades) Free from size, bleaching chemicals, earth metals and salts Cooled to ambient temperature

2.3.2.2 The alkali liquor


The alkali required for fixation is pre-dissolved then added, cold, to the feed tank. The liquor volume is then adjusted as required with cold water.

Regenerated cellulose fibers can be pre-causticized to improve color yield and significantly reduce their tendency to fibrillate under mechanical stress.

2.3.1.1 Sewing together the pieces


In order to avoid seam impressions during batching the pieces should be sewn with a butted seam. The sewing yarn should be of the same substrate, i.e. cotton or viscose and have received the same pre-treatment.

2.3.3 Alkali systems


Drimaren HF and Drimaren CL dyes can be applied using different alkali systems:

Fixation with sodium silicate/caustic soda Fixation with soda ash/caustic soda

2.3.2 Preparation of the pad liquor

2.3.3.1 Fixation with sodium silicate and caustic soda Standard recipe:

2.3.2.1 Dissolving the dyes


When dissolving the dyes it should be considered that there are different commercial forms. Some products are specially designated as Cold Dissolving Granules (CDG). There is a fundamental difference between granules (which include the CDG formulation) and powder. Some products are specially designated as Cold Dissolving Granules. Granules should never be pasted but sprinkled into water. For the CDG form the water can be cold (2030 C). For other forms it is better to use water at 6080 C. This is also true for the powder products. Mixtures of different commercial forms should always be dissolved at higher temperature (> 60 C) by sprinkling them into water.

x 0.53 0.53 y 50

g/l g/l g/l g/l ml/l

Drimaren HF/CL dye Leonil EHC liq c Ladiquest 2005 liq c Caustic soda 36 B Sodium silicate 38 B
g/l m/l ml/l g/l m /l ml/l 05 50 8.0 4050 50 19.0 510 50 10.0 5060 50 21.0 1020 50 12.0 6070 50 23.0 2030 50 15.0 7080 50 25.0 3040 50 17.0 80100 50 29.0

Drimaren HF/CL dye Sodium silicate 38 B Caustic soda 36 B Drimaren HF/CL dye Sodium silicate 38 B Caustic soda 36 B

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

Characteristics:

Characteristics:

Rapid fixation High operational reliability High pad liquor stability Stable pH value The influence of CO2 (carbonation) and other acid components in the air are excluded

Rapid fixation Easy washing off No influence on fabric handle

2.3.4 Pad liquor stability


The separately prepared dye and alkali solutions are cooled to the required pad liquor temperature and sent to the padder via a mixing device. A mixture ratio of 4 parts dye solution and auxiliaries to 1 part alkali solution has provided good results in practice. Other mixture ratios are also possible. After mixing with alkali the dye becomes reactive. To ensure

The caustic soda is added to the bath first, before the sodium silicate. Sodium silicate can form precipitations with hardness forming salts which are later deposited on the material and machine parts. The alkali liquor should be prepared using soft water or hard water should be corrected by adding a sequestering agent such as 0.5-3 g/l Ladiquest 2005 liq c.

When the operating temperature is >30 C, or high concentrations of dyestuff are used, the bath stability can be improved by increasing the amount of sodium silicate to between 70 and 100 ml/l.

optimum pad liquor stability, i.e. to avoid premature dye hydrolysis, it is essential to use a mixing device. Where possible the padding temperature should be 25 C +/ 3 C. All reactive dyes are subject to hydrolysis in the presence of alkali in the pad liquor. It depends on the time, amount of dye and

2.3.3.2 Fixation with soda ash and caustic soda


A combination of caustic soda and soda ash can be used when the padding and fixation temperatures are between 2025 C.

temperature. Hydrolyzed dye cannot react with the cellulose. If dye hydrolysis already takes place in the pad liquor or in the padding trough there is a danger of tailing. Exact knowledge of the pad liquor stability of the Drimaren HF/CL dyes is therefore important. Details of individual dyes can be found in the shade card inserts or calculated exactly using the HYDREC program.

Standard recipe:
x 0.53 0.53 y

g/l g/l g/l ml/l

Drimaren HF/CL dye

Leonil EHC liq c Ladiquest 2005 liq c

The highest pad liquor stability is achieved with the caustic soda/ sodium silicate formula. It decreases with increasing dye concentration i.e. the rate of hydrolysis increases. This can be explained by the buffer capacity of this system whose optimum efficiency is in the low dye concentration region and decreases
510 10 4.0 5060 20 14.0 1020 20 6.0 6070 20 16.0 2030 20 8.0 7080 20 16.0 3040 20 10.0 80100 20 16.0

1020 g/l

Soda ash Caustic soda 36 B


g/l g/l ml/l g/l g/l ml/l 05 10 2.0 4050 20 12.0

Drimaren HF/CL dye Soda ash Caustic soda 36 B Drimaren HF/CL dye Soda ash Caustic soda 36 B

with increasing dye and alkali concentration. The bath stability can be improved, when the padding and fixation temperature is > 30 C or high concentrations of dye are used, by increasing the amount of sodium silicate to between 70 and 100 ml/l. This may impair the washing off properties depending on the fabric construction and washing off equipment adopted.

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The HYDREC calculation program gives information on the bath stability and fixation times, taking into consideration the existing conditions (temperature, bath volume, running speed, weight of the goods and liquor pick-up). The HYDREC program can calculate the required amounts of caustic soda and sodium silicate necessary by taking into consideration the different grades (B) used in the industry.

2.3.6 Fixation by batching


The padded goods are rolled onto a beam, finishing with the padded end cloth and wrapped in plastic film to avoid premature drying. The beam is then batched for 624 hours while rotating slowly. Dye-fiber reaction takes place during batching. For this process the following points should be considered:

The goods must be rolled up with straight edges under constant tension The padding and batching temperatures should be identical (+/-3 C) During batching, the fabric heats up due to the exothermic reaction. If the batching (surrounding) temperature is higher than the padding temperature, condensation may form under the plastic film causing water spotting. Water spotting can be prevented by covering the fabric batch in a layer of leader cloth, before it is wrapped in plastic film.

2.3.5 Padding

Padding is carried out on a two or three roller padder, preferably with an economizing trough (low liquor volume).

Pick-up:
6080 % For cotton woven goods 8020 % For cotton knit goods 7090 % For regenerated cellulose

If the batching (surrounding) temperature is lower than the padding temperature, the rate of fixation will slow down, especially at the edges of the beam. This can be the reason for poor shade reproducibility, listing and tailing problems. It is particularly problematic at temperatures < 20 C.

The immersion time, i.e. the time the fabric remains in the pad liquor before squeezing, is 12 seconds. The pad liquor turnover time should be as fast as possible, i.e. < 5 min to maintain stability and reduce the risk of tailing. Pad liquor turnover time is calculated with the following formula:

The fixation times depend on the reaction speed of the individual dyes, which depends on:

The amount of dye The padding temperature The batching temperature The alkali system

V 10

gfv

= Pad liquor turnover time in minutes

V = trough volume in liters g = weight of the goods in grams per running meter f = dry pick-up in % v = speed of the goods in m/min.

Drimaren Yellow CL-2R, Drimaren Green HF-5BL, Drimaren Turquoise CL-B and Drimaren Turquoise K-2B require a minimum fixation time of 24 hours, depending on the depth of shade, to achieve full fixation. The alkali amounts given for Drimaren HF and Drimaren CL dyes can be used for Drimaren Turquoise K-2B.

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

2.3.7 Washing off


Optimum fastness properties can only be achieved on perfectly washed off material. If sodium silicate has been applied, soft water should be used for the first few rinsing baths, beginning with cold water. This prevents deposits of insoluble salts on the machines and the goods. Depending on the machinery available, washing off can be carried out on

6. 7. 8.

Wash at 95 C Wash at 70 C Neutralize at 4060 C to pH 67 with Sirrix NE liq

Due to the high alkaline stability of Drimaren HF dyes, it isnt necessary to neutralize the fabric before washing off at high temperature (8095 C) in a continuous washing range. The material should have a neutral pH ready for drying. The dye-fiber bond of certain elements from the Drimaren CL range can be sensitive to washing off at high temperature under high alkaline conditions. It is therefore necessary to neutralized (pH 67) the fabric before the high temperature washing off step.

Open width washers Rope washers Beam washers Any other suitable machine

Soaping is carried out with an addition of Ladiquest 2005 liq c or Ladipur RSK/R3C liq as follows:

2.4 Rapid fixation (lab technique)


Shade matching can be carried out in the lab quickly and with a

Discontinuous method
After warm rinsing adjust the fabric pH to 67. Care should be taken to ensure that the fabric has a neutral pH before soaping at the boil. 0.53 g/l Ladiquest 2005 liq c or Ladipur RSK/R3C liq is added to the soaping bath and the fabric treated at the boil for 1020 min. This is followed by warm then cold rinsing.

high degree of precision. There are two possible methods:

2.4.1 Rapid fixation in a microwave oven


A microwave oven can be used for rapid checking of pad liquors in the dyehouse. It requires a nonmetallic container with a lid, which is partially filled with water to imitate ideal fixation conditions and avoid drying out of the fabric.

Continuous method (example)

Working method

Commercial microwave oven, at least 600W capacity Prepare dye and alkali solutions separately Fill a plastic container with 23 cm water and place in the microwave. Set the time to 15 min, 80% capacity (500W). Switch on the oven without a sample, but with the container to condition the surroundings

Continous washing range with 8 compartments:


1. 2. 3. 4. 5. Overflow rinse at room temperature Overflow rinse at room temperature Wash at 70 C Wash at 95 C with 13 g/l Ladipur RSK liq Wash at 95 C with 13 g/l Ladipur RSK liq

Prepare the fabric sample, 9x13 cm Pad at 3 m/min The pick-up should correspond to that in practice (2 immersions have proved advantageous)

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

Place the padded sample in a polyethylene bag or wrap in plastic film (to prevent drying) and dwell for at least 15 min at room temperature

2.4.3 Examples Shade 1


2.2 1.2 1.2 1.0 8.0 g/l g/l g/l g/l ml/l Drimaren Yellow HF-CD Drimaren Red HF-CD Drimaren Aquamarine HF-CD Leonil EHC liq c Sodium silicate 38 B NaOH 36 B
Reference 9 h, at 25 C

Microwave CMC 0.9, 105% 15 min RT + 4 min at 500 W Drying cabinet CMC 0.7, 97% 15 min RT + 60 min at 50 C Microwave CMC 0.6, 101% 15 min RT

Hang the sample in the preheated fixation box (without bag) and switch the oven on

After fixation the samples are rinsed and soaped in the usual manner. The values given are guide values. Depending on the oven and weight of the material different fixation times may be necessary (usually between 35 min).

50.0 ml/l

Shade 2
It is advisable to compare the shade found using a microwave against that obtained by standard batching conditions. 4.0 6.5 1.0 g/l g/l g/l Drimaren Yellow HF-CD Drimaren Red HF-CD Drimaren Aquamarine HF-CD

+ 4 min at Reference 15 h, at 25 C 500 W Drying cabinet CMC 0.7, 97% 15 min RT + 60 min at 50 C

11.0 g/l

Leonil EHC liq c Sodium silicate 38 B NaOH 36 B

2.4.2 Rapid fixation in a drying cabinet Working method:


50.0 ml/l 15.0 ml/l

Prepare dye and alkali solutions separately Prepare the fabric sample Pad at 3 m/min The pick-up should correspond to that in practice (2 immersions have proved advantageous) Tailing is responsible for shade differences between the beginning and end of a batch in a continuous process. Clariant has developed a very severe test which imitates this phenomenon: Prepare 500 ml dye liquor.
liquor collected from Step 2

2.5 Clariant tailing test

Place the padded sample in a polyethylene bag and dwell for at least 15 min at room temperature Store the padded sample, in the polyethylene bag, for 1h at 50 C in drying cabinet (constant temperature must be maintained)

After fixation the samples are rinsed and soaped in the usual manner. It is advisable to compare the shade found using a drying cabinet against that obtained by standard batching conditions.

Step 1

Step 2

Step 3

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

Step 1 (beginning) Pad 20 cm CO-merc. through 100 ml dye liquor from the 500 ml prepared. A fixation step follows to fix the dyestuff.

3. Pad Dry Chemical Pad Steam process


3.1 Introduction

Step 2 5 m CO merc. is passed through the remaining 400 ml dye liquor then squeezed on the lab padder. The squeezed liquor is collected. Step 3 (end) Pad 20 cm CO-merc. through the collected liquor. A fixation step follows to fix the dyestuff. Assessment is carried out at the beginning (Step 1) and at the end (Step 3) by comparison with each other. The differences in concentration and shade are determined colorimetrically. Reference or 100% is always the beginning. The less tailing there is, the smaller the difference between the beginning and the end (shade and strength). The test can be used to assess tailing in pad batch and all continuous dyeing processes.
Dye pad liquor Drying Chemical pad liquor Steaming

This is a continuous process for dyeing cellulosic fabrics with Drimaren HF/CL dyes. The process is particularly suitable for dyeing large production batches, where the process becomes economically attractive.

The pad dry chemical pad steam process offers the following advantages:

Simple working method Short preparation time High color yield Excellent surface appearance even with heavy, tightly woven fabrics Excellent reproducibility No risk of dye hydrolysis Tailing with pale shades should not be an issue Especially recommended for very large batches

2.6 Shade change during drying

Depending on the dyestuff, but regardless of the substrate, changes of shade can occur after the drying operation. This shade change is dependent on the fabric temperature, pH and moisture content. A stable final shade is only achieved when the fabric pH is neutral and the temperature and moisture content have reached equilibrium. It is therefore important that the shade is assessed against the standard once this equilibrium has been reached. A conditioning cabinet (e.g. 20 C, 65% RH) can be used to condition samples before assessing the shade.

3.2 Process principle


The principle of the Pad Dry Chemical Pad Steam process consists of padding the goods with dye solution at room temperature and then drying. The dried goods are then padded with chemical pad liquor and the dye fixed in a steamer. The unfixed dye is removed by rinsing then soaping at the boil. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade.

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

3.3 Operating procedure


Various factors, which are important for a reliable process flow, are described in the following sections:

3.3.2.1 Dissolving the dyes


See section 2.3.2.1 Dissolving the dyes

The prepared state of the material to be dyed Preparation of the dye pad liquor The intermediate drying step Preparation of the chemical pad liquor Padding Fixation by steaming The washing off process

3.3.2.2 Pad liquor stability


The stability of the dye solution is very good because the dye pad liquor doesnt contain alkali.

3.3.3 Padding
See Section 2.3.5 Padding.

3.3.1 Fabric requirements


See section 2.3.1 Fabric requirements.

See Section 2.5 Clariant tailing test

3.3.4 Intermediate drying 3.3.1.1 Sewing together the pieces


See section 2.3.1.1 Sewing together the pieces. The fabric is first passed through an infra-red pre-drier to reduce the fabric moisture content to below ~35% in the absence of strong air flow and fabric to metal contact, which accelerate dye migration.

3.3.2 Preparation of the dye pad liquor


Standard recipe: x 520 0.53 0.53 g/l Drimaren HF/CL dye

The drier used should ensure that the fabric is dried uniformly, over its entire width and length (uniform air flow and temperature). Residual humidity should not exceed 1015% and should be constant. The dried fabric should be allowed to cool before steaming (uniform temperature and moisture content).

g/l Solidokoll NX liq g/l Leonil EHC liq c

g/l Ladiquest 2005 liq c

Intermediate drying has the following advantages:


The appearance of the goods is excellent The dye stability is very good Very deep shades are attainable

10

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

Intermediate drying has the following disadvantages:

High affinity dyes migrate slower than low affinity dyes as the probability of dye adsorption on the fiber surface is higher. If the dye affinity is too high then the tailing and washing off properties become an issue. Migration can also be drastically reduced by

It makes the process slightly more expensive

3.3.4.1 Explanation of migration


During pre-drying the dye liquor may migrate, by means of capillary forces, from the wetter (cooler) to drier (hotter) areas of the fabric resulting in face to back or side to center shade variation. Dye molecules continue to migrate as long as free water molecules diffuse from the surface of the fabric. Migration stops when only bonded water molecules remain and the moisture content of the fabric has dropped below 30%. Infra-red pre-driers are used to reduce the fabric moisture content to below ~35% in the absence of strong air flow and fabric to metal contact, which accelerate dye migration. Clariant has developed a very severe test which imitates this phenomenon.

adding electrolyte, however this may result in tailing. As a guide it can be said that if a value of > 60% is determined in the Clariant migration test, the dye exhibits minimum migration and is suitable for this process. The dye selection guide provided has been optimized so that migration and tailing are as minimal as possible.

3.3.5 Preparation of the chemical pad liquor


Standard recipe: 250 20 g/l Na2SO4 or NaCl g/l Soda ash g/l Revatol NS liq c

3.3.4.1.1 Clariant migration test


The fabric is padded with dye solution, at room temperature then dried at 110 C for 90 seconds. Before drying, a watch glass is placed on the wet fabric. A damp atmosphere develops in the watch glass and the dye solution migrates to the hotter areas. See following illustration:

1020 ml/l Caustic soda 36 B 10

The alkali required for fixation, electrolyte and Revatol NS liq c are
Inside Outside

pre-dissolved then added together, cold, to the feed tank. The liquor volume is then adjusted as required with cold water. The electrolyte in the chemical pad liquor reduces bleeding of the dye into the chemical pad trough as it has only been dried and not fixed. The electrolyte also improves dye diffusion inside the fiber during

Fig: Example of dye migration after drying Assessment is made colorimetrically by measuring the difference in color strength between the inside and outside. Reference of 100% is always outside. The less migration there is, the smaller the difference between inside and outside.

steaming.

3.3.6 Padding
See Section 2.3.5 Padding.

11

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

3.3.7 Fixation by steaming

4. Pad Wet Steam process


4.1 Introduction
This is a steaming process without intermediate drying for the

Padding temperature: Fixation:

2030 C 60 seconds with saturated steam at 102104 C

continuous dyeing of cellulosic fabrics with Drimaren HF/CL dyes. This process is especially suitable for heavy fabrics such as corduroy, velvet or toweling where it is impossible to control dye migration if an intermediate drying step is used.

In a fully continuous operation, the machine running speed is governed by the time required to pre-dry the fabric. This is determined by the fabric weight, the moisture content of the wet fabric, the drying temperature, the airflow speed and machine capacity. When processing heavy weight fabrics a slower running speed may be necessary resulting in longer steaming times. Extended fixation times do not affect the yield of Drimaren HF dyes due to the high alkaline stability of the dye-fiber bond. The dye-fiber bond of certain elements from the Drimaren CL range can be sensitive to prolonged steaming times. Care should be taken to adhere to the recommended fixation time.

Dye pad liquor

Steaming

The pad wet steam process offers the following advantages:


Omission of an intermediate drying stage saves energy No dye migration Simple process Short preparation time

3.3.8 Washing off


Optimum fastness properties can only be achieved on perfectly washed off material. Washing off is usually carried out on an openwidth washing machine. The soaping step is carried out with an addition of Ladipur RSK/R3C liq See Section 2.3.7 Washing off.

The pad wet steam process has the following disadvantages:

Shade build-up is inferior to other continuous dyeing processes, therefore it is only economical for dyeing large batches This process is not recommended for tightly constructed or mercerized fabrics

3.4 Shade change during drying


See Section 2.6 Shade change during drying

4.2 Process principle


The principle of the pad wet steam process consists of padding the

12

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

fabric with dye solution at room temperature, followed directly by fixation in a steamer. Unfixed dye is removed from the fiber by rinsing then soaping at the boil. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade. Glaubers salt is recommended for the highest solubility. The amount of Glaubers salt can be increased when dyeing very deep shades

4.3 Operating procedure


Various factors, which are important for a reliable process flow, are described in the following sections:

to improve the yield, however, this could have a negative influence on the solubility and tailing behavior of certain dyes. An addition of 100 g/l urea is therefore recommended to prevent dyestuff precipitation, with certain dyes, at high concentrations. Depending on the article and dyestuff concentration, preliminary lab trials are recommended. For reasons of solubility an addition of 100 g/l urea is recommended for Drimaren Scarlet HF-3G, Drimaren Yellow HF-CD, Drimaren Turquoise CL-B, Drimaren Green HF-5BL and Drimaren Turquoise K-2B at all concentrations.

The prepared state of the material to be dyed Preparation of the pad liquor Padding Fixation by steaming The washing off process

4.3.1 Fabric requirements 4.3.2.1 Dissolving the dyes


See Section 2.3.1 Fabric requirements. See Section 2.3.2.1 Dissolving the dyes.

4.3.1.1 Sewing together the pieces 4.3.2.2 The alkali liquor


See Section 2.3.1.1 Sewing together the pieces. The alkali necessary for fixation is pre-dissolved then added, cold, to the feed tank. The liquor volume is then adjusted as required

4.3.2 Preparation of the pad liquor Standard recipe:


x g/l Drimaren HF/CL dye

with cold water.

4.3.2.2.1 Working without a metering pump


If a metering pump isnt available then special attention must be paid to the pad liquor stability. If the dyestuff is dissolved warm or hot then care should be taken to add the soda ash to the cooled pad liquor. Some dyes may precipitate if the pad liquor is allowed to stand too long before use.

1020 g/l Soda ash 2040 g/l Glaubers salt 0.53 10 0.53 g/l Leonil EHC liq c g/l Revatol NS liq c

g/l Ladiquest 2005 liq c

13

Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The alkali required for fixation is pre-dissolved then added, cold, to the feed tank. The alkali is added last, immediately before the production run.

4.3.5 Fixation by steaming

4.3.3 Pad liquor stability


Padding temperature: 2030 C 90 seconds with saturated steam at 102104 C

4.3.3.1 Pad liquor stability with a metering pump


The separately prepared dye and alkali solutions are cooled to pad liquor temperature and sent to the padder via a mixing device. A mixture ratio of 4 parts dye solution and auxiliaries to 1 part alkali solution has provided good results in practice. Other mixture ratios are also possible. If a metering pump is used the pad liquor stability isnt normally an issue.

Fixation:

Drimaren Yellow CL-2R, Drimaren Green HF-5BL, Drimaren Turquoise CL-B and Drimaren Turquoise K-2B require 90180 seconds steaming time, depending on the depth of shade, to achieve full fixation. The fabric is padded with the dye solution then passed directly into the steamer.

4.3.3.2 Pad liquor stability without a metering pump


After mixing with alkali the dye becomes reactive. To ensure optimum pad liquor stability, i.e. to avoid premature dye hydrolysis, the temperature should be kept at 25 C +/ 3 C where possible. All reactive dyes are subject to hydrolysis in the presence of alkali in the pad liquor. It depends on the time, amount of dye and temperature. Hydrolyzed dye cannot react with the cellulose. If dye hydrolysis already takes place in the pad liquor or in the padding trough there is a danger of tailing. Exact knowledge of the pad liquor stability of the Drimaren HF/CL dyes is therefore important. Details of individual dyes can be found in the shade card inserts.

In a fully continuous operation, the machine running speed is governed by the time required to dry the fabric, usually on a cylinder drier, after passing through a continuous washing range. This can result in longer steaming times. Extended fixation times do not affect the yield of Drimaren HF dyes due to the high alkaline stability of the dye-fiber bond. The dye-fiber bond of certain elements from the Drimaren CL range can be sensitive to prolonged steaming times. Care should be taken to adhere to the recommended fixation time.

4.3.6 Washing off


See Section 2.3.7 Washing off.

4.3.4 Padding
See Section 2.3.5 Padding. See Section 2.5 Clariant tailing test

4.4 Shade change during drying


See Section 2.6 Shade change during drying

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Textile Chemicals

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Pad Batch and Continuous Dyeing procedures

5. Pad Thermofix process


5.1 Introduction
After padding and intermediate drying the dyestuff is fixed by hot air in a hotflue. This process is used for the continuous dyeing of cotton fabrics with Drimaren HF/CL dyes.

5.3 Operating procedure


Various factors, which are important for a reliable process flow, are described in the following sections:

The prepared state of the material to be dyed Preparation of the pad liquor Padding Intermediate drying Fixation by hot air The washing off process

Dye pad liquor

Drying

Fixation

5.3.1 Fabric requirements


See Section 2.3.1 Fabric requirements.

The pad thermofix process offers the following advantages:


Simple process Short preparation time Good lab to bulk shade reproducibility See Section 2.3.1.1 Sewing together the pieces.

5.3.1.1 Sewing together the pieces

The pad thermofix process has the following disadvantages:


Build-up Reduced light and chlorine fastness The process requires urea

5.3.2 Preparation of the pad liquor Standard recipe:


x y g/l g/l g/l g/l g/l g/l Drimaren HF/CL dye Alkali Solidokoll NX liq Leonil EHC liq c Ladiquest 2005 liq c Urea

5.2 Process principle


The principle of the pad thermofix process consists of padding the goods with dye solution at room temperature and then drying. The dried goods are then fixed at 150180 C. Unfixed dye is removed from the fiber by rinsing then soaping at the boil. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade.

520 0.53 0.53 50150

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

5.3.5.1 Pad liquor stability with a metering pump


Drimaren HF/CL dye

g/l g/l g/l g/l

05 50 15

510 75 15

1020 100 15

2040 150 10

> 40 150 20

Urea Sodium bicarbonate Soda ash

See Section 4.3.3.1 Pad liquor stability with a metering pump.

5.3.5.2 Pad liquor stability without a metering pump 5.3.2.1 Influence of urea
The recommended amount of urea can be reduced for very pale shades. Reducing the amount of urea may lead to a loss in color strength depending on the dyes used and depth of shade. 510 g/l Borax can be added to the pad liquor to prevent yellowing of the cotton fiber at temperatures >160 C. See Section 2.3.5 Padding. See Section 2.5 Clariant tailing test. See Section 4.3.3.2 Pad liquor stability without a metering pump.

5.3.6 Padding

5.3.3 Dissolving the dyes


See Section 2.3.2.1 Dissolving the dyes

5.3.7 Intermediate drying


See section 3.3.4 Intermediate drying. See section 3.3.4.1 Explanation of migration. See section 3.3.4.1.1 Clariant migration test.

5.3.4 The alkali liquor


The alkali necessary for fixation is pre-dissolved then added, cold, to the feed tank. The alkali is added last, immediately before the production run.

5.3.8 Fixation in hot air 5.3.4.1 Working without a metering pump


See Section 4.3.2.2.1 Working without a metering pump.

5.3.5 Pad liquor stability


See Section 4.3.3 Pad liquor stability.

Padding temperature: Fixation:

2030 C 60 seconds with hot air at 160 C

The fabric is padded with the dye solution, dried and then fixed at 150180 C.

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The fixation time and temperature may vary depending on the machine configuration, dye and depth of shade. In general, however, it is very short (60 s). Longer fixation times dont have a negative effect on the yield but may impair the light fastness. Drimaren Yellow CL-2R, Drimaren Green HF-5BL, Drimaren Turquoise CL-B and Drimaren Turquoise K-2B require 90120 seconds thermofixation time, depending on the depth of shade, to achieve full fixation.
Dye pad liquor Drying/ Fixation

The Pad Moist process offers the following advantages:


Fully continuous dyeing process Ideal for short or long production batches Low chemical load in the waste water (no urea, salt or sodium silicate) High fixation yield Simple working method Short setting up and machine down time

5.3.9 Washing off


See Section 2.3.7 Washing off.

5.4 Shade change during drying The Pad Moist process has the following disadvantages:
See Section 2.6 Shade change during drying.

Machine size must be adapted for heavy weight fabrics (longer drying time) Laboratory shade matching requires special equipment

6. Pad Moist process


6.1. Introduction
The Pad Moist process is a continuous dyeing procedure used for dyeing cellulosic fabrics with Drimaren HF/CL dyes. The principle

6.2 Process principle


The reactive dyes are fixed during 24 minutes (depending on fabric weight and machine capacity). under controlled humidity (2530 % steam content) and an air temperature of 110130 C. Infrared pre-drying increases productivity when dyeing heavy weight fabrics. The dry goods are then washed off (preferably continuously) to remove the unfixed dyestuff from the fibers.

of the process consists of padding the fabric with dye solution at room temperature before passing it through a hot flue with an air temperature of 110130 C and a relative humidity of 2530 % inside each chamber. Under these conditions the fabric is dried and at the same time dyestuff fixation takes place at 6871 C (the wet bulb temperature). The unfixed dye is removed by rinsing then soaping at the boil. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade.

6.3 Operating procedure


Various factors, which are important for a reliable process flow, are described in the following sections:

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The prepared state of the material to be dyed Preparation of the pad liquor Padding Drying/fixation The washing off process

with cold water. A metering device is required to guarantee sufficient dye liquor stability.
Drimaren HF/CL dye Soda ash Caustic soda 36 B Drimaren HF/CL dye g/l g/l g/l g/l g/l g/l 010 10 5060 20 5.0 1020 20 1.0 6070 20 6.0 2030 20 2.0 7080 20 7.0 3040 20 3.0 8090 20 8.0 4050 20 4.0 90100 20 10.0

6.3.1 Fabric requirements


See Section 2.3.1 Fabric requirements.

Soda ash Caustic soda 36 B

For Drimaren Black CL-S at concentration greater than 60 g/l the

6.3.2 Sewing together the pieces


See Section 2.3.1.1. Sewing together the pieces.

amount of caustic soda should be increased to 1520 ml/l.

6.3.6 Pad liquor stability 6.3.3 Preparing the dyestuff pad liquor Standard recipe:
x y g/l g/l Drimaren HF/CL dye Alkali Leonil EHC liq c Ladiquest 2005 liq c

The dyestuff and alkali solutions, which have been prepared separately, are cooled to room temperature then fed into the padder via a mixing device. A mixture ratio of 4 parts dye solution and auxiliaries to 1 part alkali solution has provided good results in practice. Other mixture ratios are also possible. The program MOISTFIX in the electronic shade card can be used to calculate the exact alkali requirements as well as the pad liquor stability and required drying/fixation time.

0.53 g/l 0.53 g/l

6.3.7 Padding
See Section 2.3.5 Padding.

6.3.4 Dissolving the dyestuffs


See Section 2.3.2.1. Dissolving the dyestuffs.

See Section 2.5 Clariant tailing test.

6.3.8 Drying/Fixation 6.3.5 The alkali liquor


Here the alkali necessary for fixation is pre-dissolved the added, cold, to the feed tank, before the volume is adjusted as required

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

After applying the pad liquor solution on the padder, the dyestuff is fixed and the material dried in an atmosphere of controlled humidity (2530 % steam content) and an air temperature of 110130 C. Here the fixation time and the running speed must be adapted to the quality of the material (usually between 2 and 4 minutes).

and high diffusion that guarantee excellent washing off properties. High wet fastness can be achieved by soaping at 85 C with only one pass through a continuous washing range. High alkaline stability of the dye-fiber bond (DFP chemistry) is essential as the washing off procedure must be carried out under alkaline conditions.

6.3.9 Washing off


See Section 2.3.7 Washing off.
Dye pad liquor Dry Thermosol Chemical pad liquor Steam

6.4 Shade change during drying


See Section 2.6 Shade change during drying.

The SWIFT process offers the following advantages:

7. SWIFT process for dyeing PES/CEL blends


7.1 Introduction
The SWIFT process is a one bath, 2 stage process for dyeing PES/ CEL fabrics with Foron S-WF and Drimaren HF dyes, where high

Simple working method Suitable for dark shades Increased productivity Reduced water, energy and chemical consumption Excellent surface appearance even with heavy, tightly woven fabrics Excellent reproducibility High level of wet fastness is achieved without a costly reduction clearing process Especially recommended for very large batches

wash fastness is achieved without a reduction clearing step. Disperse and reactive dye can be padded together and the whole process is completed with one pass through a continuous dyeing range. The key to success is the dyestuffs selected: Foron S-WF dyes: A range of alkali clearable disperse dyes with high sublimation fastness. High wash fastness can be achieved in continuous dyeing without an intermediate reduction clearing process. Foron S-WF dyes show minimum sensitivity to temperature fluctuations within their maximum fixation range (205 225 C depending on the fixation time). The danger of center to selvedge and beginning to end shade differences can largely be eliminated guaranteeing excellent reproducibility. Drimaren HF dyes: Reactive dyes with very high fixation values

7.2 Process principle


The principle of the SWIFT (Pad Dry Thermosol Chemical Pad Steam) process consists of padding the goods with dye solution at room temperature and then drying. A thermosol step follows to dye the polyester part of the blend with Foron S-WF dye. The dried goods are then padded with a chemical pad liquor before steaming to fix the Drimaren HF dye on the cellulose part of the blend. During the alkaline steaming process, unfixed Foron S-WF dye, adhering to the fabric surface, is converted to a water soluble anionic form. It can then be removed together with the unfixed reactive dyestuff by the subsequent washing off process.

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

7.3 Operating procedure


Various factors, which are important for a reliable process flow, are described in the following sections:

7.3.2.1 Dissolving the dyes


For preparation of the reactive dye see section 2.3.2.1 Dissolving the dyes. The disperse dye is dispersed by pouring it into warm water (40 C) and stirring. The time required for mixing the dye liquor must be adapted to the total dye concentration and the dyes being used. Before adding dissolved dyes to the feed tank the dye liquor should be passed through a filter to ensure that any non-dissolved dye or contamination is held back. Unlevelness and/or spots and possible damage to the pumps can be avoided in this way. Cold water should then be used to adjust the dye liquor to the required volume.

The prepared state of the material to be dyed Preparation of the dye pad liquor The intermediate drying step The thermosol step Preparation of the chemical pad liquor Padding Fixation by steaming The washing off process

7.3.1 Fabric requirements


See section 2.3.1 Fabric requirements.

7.3.2.2 Pad liquor stability


The stability of the dye solution is very good because the dye pad

7.3.1.1 Sewing together the pieces


See section 2.3.1.1 Sewing together the pieces.

liquor doesnt contain alkali. The pad liquor mixer should remain running to prevent settling out of the disperse dye.

7.3.3 Padding 7.3.2 Preparation of the dye pad liquor


See Section 2.3.5 Padding. Standard recipe: x y 520 0.53 0.53 530 g/l g/l g/l g/l g/l g/l Drimaren HF dye Foron S-WF dye Solidokoll NX liq Leonil EHC liq c

See Section 2.5 Clariant tailing test.

7.3.4 Intermediate drying


See section 3.3.4 Intermediate drying. See section 3.3.4.1 Explanation of migration. See section 3.3.4.1.1 Clariant migration test.

Ladiquest 2005 liq c Emigen DPR liq

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

7.3.5 Thermosoling

7.3.8 Fixation by steaming

After the intermediate drying process the disperse dye is micro-dispersed on the surface of the polyester fiber, or in the case of PES/CEL blends, to a large extent on the cellulosic fiber. In the thermosol process, the fabric is treated in hot air at 210220 C for 4560 seconds.

Padding temperature: Fixation:

2030 C 60 seconds with saturated steam at 102104 C

In a fully continuous process, the machine running speed is governed by the time required to pre-dry the fabric. This is determined by the fabric weight, the moisture content of the wet fabric, the drying temperature, the air flow speed and machine capacity. When processing heavy weight fabrics a slower running speed may be necessary resulting in longer steaming times. Extended fixation times do not affect the yield of Drimaren HF dyes due to the high alkaline stability of the dye-fiber bond. During the alkaline steaming process, unfixed Foron S-WF dye, adhering to the fabric surface, is converted to a water soluble anionic form. It

The thermosol process can be divided into 3 steps:


Heating of the fabric Adsorption of the disperse dyestuff on the polyester fiber surface Dye diffusion and distribution inside the polyester fiber

7.3.6 Preparation of the chemical pad liquor


See section 3.3.5 Preparation of the chemical pad liquor.

can then be removed together with the unfixed reactive dyestuff by the subsequent washing off process.

7.3.9 Washing off 7.3.7 Padding


See Section 2.3.5 Padding. The liquor pick-up on PES/CEL fabrics is usually ~3545 % using a conventional padder. This isnt high enough to obtain the required amount of chemical liquor on the fabric. Pad-steam machinery therefore incorporates either a booster, kiss roll or flex nip system to ensure that the liquor pick-up is high enough (> 100 %) for fixation of the reactive dye and clearing of the disperse dye (that remains on the fiber surface) during the steaming process. Optimum fastness properties can only be achieved on perfectly washed off material. Washing off is carried out on a continuous open-width washing machine.

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Textile Chemicals

Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

The fabric is washed off under alkaline conditions to ensure that all unfixed disperse dye remaining on the fiber surface is converted to the water soluble anionic form that can be removed together with the unfixed reactive dye. For this reason it is necessary to use Drimaren HF dyes due to the high alkaline stability of the dye-fiber bond. The unfixed dye is removed by rinsing then soaping at 85 C. Higher temperatures are avoided to prevent migration of disperse dye, from within the polyester fiber structure to its surface, thus averting wet fastness issues. Disperse dyes begin to migrate at temperatures above the glass transition temperature (Tg) of the polyester fiber. Drimaren HF dyes, having excellent washing off

8. Dye Selection
State of the art, problem solving range, for difficult pale to medium shades requiring high light fastness

Drimaren Golden Yellow HF-CD (non photochromic element) Drimaren Yellow HF-CD (non photochromic element) Drimaren Red HF-CD Drimaren Aquamarine HF-CD

Top performing elements to meet the highest fastness and reproducibility demands in medium to dark shades

Drimaren Golden Yellow HF-CD Drimaren Dark Red HF-CD Drimaren Red HF-3B Drimaren Aquamarine HF-CD Drimaren Dark Blue HF-CD Drimaren Navy HF-GN Drimaren Navy HF-B

properties, can be washed off at 85 C. This washing off treatment is essential to obtain the optimum wet fastness properties and final shade. Continous washing range with 8 compartments:
1. 2. 3. 4. 5. 6. 7. 8. Overflow rinse at room temperature Wash at 85 C Wash at 85 C with 13 g/l Eganal DFT liq

Cost-effective range recommended for dyeing standard articles in medium to dark shades

Wash at 85 C Wash at 85 C with 13 g/l Ladipur RSK liq Wash at 85 C Wash at 85 C Neutralize at 4060 C to pH 67 with Sirrix NE liq

Drimaren Yellow CL-2R Drimaren Red CL-5B Drimaren Red CL-4B Drimaren Dark Red HF-CD Drimaren Navy CL-R Drimaren Black CL-S

7.4 Shade change during drying


See Section 2.6 Shade change during drying.

Special elements for bright yellow, blue, green and turquoise shades

Drimaren Brilliant Yellow HF-RL Drimaren Turquoise CL-B Drimaren Turquoise K-2B Drimaren Royal Blue HF-CD Drimaren Green HF-5BL

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Drimaren HF/CL reactive dyes


Pad Batch and Continuous Dyeing procedures

www.textiles.clariant.com Clariant International Ltd Rothausstrasse 61 4132 Muttenz Switzerland Business Unit Textile Chemicals The Synergy 1 International Business Park 609917 Singapore Singapore

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