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CHAPTER 4

MATERIALS AND METHODS

4.1 MATERIALS

The materials, dyes, dyeing recipes used in different technologies

are given below.

4.1.1 Cloth Materials Used

 Cotton
 Polyester
 Blend (67% cotton and 33% polyester)

4.1.2 Dyes Used

Reactive Dyes (Cotton)

 C.I. Reactive Blue 3 (Procion Brilliant Blue)
 C.I. Reactive Red 29 (Procion Brilliant Red)
 C.I. Reactive Yellow 5 (Procion Supra Yellow)

Disperse Dyes (Polyester)

 C.I. Disperse Blue 2 (Acetoquinone Dark Blue)

 C.I. Disperse Red 15 (Resoform Red)
 C.I. Disperse Yellow 16 (Suden Yellow)
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4.1.3 Dyeing Recipe

4.1.3.1 Cotton

Material: Liquor ratio - 1: 40

Dye concentration - 1%, 3%, 5%, 7% on weight of cloth
NaCl - 30 g/l
Na2CO3 - 20 g/l
Weight of the sample cloth - 4g

4.1.3.2 Polyester

Material: Liquor ratio 1:30

Dye concentration 1%, 3%, 5%, 7% of weight of cloth
Depth of shade: upto 0.5% = 6% carrier on weight of cloth
0.5 - 2% = 8% carrier on weight of cloth
2 - 4% = 10% carrier on weight of cloth
4 - 8% = 12% carrier on weight of cloth
Weight of the sample cloth = 3g

4.1.3.3 Blend

Material: Liquor ratio - 1: 30

Dye - 1%, 3%, 5%, 7% of weight of fabric
Weight of the sample cloth - 4g
Blend material - 33% Polyester and 67% Cotton

4.2 METHODS

Dyeing experiments were conducted with three different colours

such as blue, red and yellow on different fabric materials by varying process
parameters like time, temperature and concentration. Liquor ratio could not be
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varied due to restriction in the size and space constraints of the individual
experimental setup. Cotton, polyester and blend material with cotton (67%)
and polyester (33%) were used for evaluation. In case of cotton, reactive dyes
were used. In case of polyester, disperse dyes were used. In case of polyester,
carrier dyeing method was adopted. In case of blend, 2-bath dying procedure
was adopted. The power consumption in each experiment was measured using
watt-hour meter. The dyed sample and remaining dye solution was analysed
using spectrophotometer for absorbance measurements. The
spectrophotometer figure is shown in Appendix . F.2. In order to assess the
final quality in each technology, dyed samples are tested for parameters like,
colour matching, K/S values and fastness values. Conventional electric heater,
ultrasonic equipment, microwave oven, infrared dyeing machine and
magnetic stirred hot plate are the equipments used for different technologies
respectively. The different process parameters for different technologies have
been chosen in such a way that the maximum values do not exceed the
conventional operating values. The dye concentrations were kept at 1%, 3%,
5% and 7% respectively.

Experiments on dyeing were conducted for three different colours

such as blue, red and yellow for different fabric materials by varying process
parameters like time, temperature and concentration of dye. Different
processes are adopted and energy consumption figures were noted.

4.2.1 Procedure for Dyeing Cotton

The sample cotton cloth to be dyed is taken and weighed. The

required amount of reactive dye, dye liquor and salts like (NaCl, Na2CO3) are
taken according to the sample weight. The required amount of liquor is put in
a beaker and kept in the heater and is slowly heated. After that, the sample
cotton cloth and the dye, into the beaker and kept for 5 minutes. One third of
the salt is to be added for fixation of the dye. After 10 minutes, half of the
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remaining salt is added. Again after 10 minutes, the remaining salt is added.
Now Na2CO3 is added and allowed for thirty minutes to react. The
temperature is maintained at desired value till the process is completed. Then
the sample is taken out rinsed and soaped for about 15 minutes and washed
with cold water thoroughly and dried.

The dried sample is weighed. The liquor solution left in the beaker
is put in spectrophotometer and absorbance is measured. The initial dye
solutions absorbance value was also measured using the spectrophotometer.
The reference absorbance graphs for cotton dyes are given in Appendix -A.
The dyeing cycle graphs for cotton are given in Appendix – B.1.

4.2.2 Carrier Dyeing of Polyester

Four methods are normally used for dyeing polyester fabrics:

a. Conventional aqueous dyeing (batch dyeing)

b. Aqueous dyeing with a carrier (batch dyeing)
c. High-temperature (above 100°C usually 130°C) aqueous dyeing
(batch dyeing)
d. “Thermo sol” dyeing (continuous dyeing)

When dyeing polyester with disperse dyes below 100°C without

special auxiliaries known as carriers, only light shades can be obtained. This
is because of the low dye absorption rate by this method; other techniques are
required to obtain medium or heavy shades.

A carrier is an organic chemical that has an affinity for and will

swell polyester fibers. Chemicals such as biphenyl, orthophenylphenol,
benzyl benzoate, butyl benzoate, 1, 2, 4-trichlorbenzene and butyl
phthalamide have been used. The use of a carrier at 100°C increases the
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amount of dye absorbed and decreases staining of other fibers by disperse

dyes.

It is important that as much carrier as possible be removed from the

yarn or fabric after dyeing because fastness properties, particularly light
fastness, can be reduced by traces of some carriers. Another reason for
complete removal of carrier from dyed fabrics is to prevent skin irritations in
wearers who might be sensitive to these chemicals. To effect complete
removal of residual carrier and loose surface dye, carrier-dyed fabrics are
normally given a reduction clear using sodium hydrosulphite and caustic soda
at 60°C for 10 – 15 minutes. Sodium hydrosulphite is a reducing agent that
destroys the surface deposited dyestuff that if not removed would result in
dyeing of poor fastness to wet treatments as well as rubbing.

In this experiment, carrier dyeing is adopted due to low temperature

use and low pressure requirements.

4.2.3 Procedure for Dyeing Polyester

The sample polyester cloth is weighed. The required amount of

disperse dye and carrier as per the weight of the sample cloth are also taken.
A beaker with a required amount of liquor is kept in a heater and the liquor is
slowly heated to attain the desired temperature of 85°C. After the temperature
is reached, the cloth is put and the temperature range is maintained at 85-95°C
for 80 minutes. Throughout the process, the specified temperature range is
maintained. Then the sample is taken out, reduction clearing on polyester is
done before washing with cold water and squeezed.

The liquor solution left in the beaker is put in spectrophotometer

and absorbance is measured. The initial dye solutions absorbance value was
also measured using the spectrophotometer. The reference absorbance graphs
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for polyester are given Appendix C. The dyeing cycle curve for carrier dyeing
of polyester is given in Appendix B.2.

4.2.4 Dyeing of Blend Material

The blend material consists of 67% cotton and 33% polyester. Here
the dyeing of the blend material is carried out under 2 bath procedure. First,
the cotton is dyed as per the procedure given the earlier (paragraph 4.2.1) and
then polyester is dyed with carrier as given in (paragraph 42.3).

4.2.5 Procedure for Dyeing Blend

The cloth which is to be dyed is weighed. The required amount of

dye liquor, dye and salts like (NaCl, Na2CO3) are taken according to the
sample weight. The required amount of liquor is taken in a beaker and kept in
the heater until it slowly reaches a temperature of 40°C. Then the cloth and
the reactive dye are added in the beaker. The same procedure used to dye
cotton at the temperature of 80°C and kept for 1 hour is followed. After
1 hour, the disperse dye and the carrier solution should be added according to
the recipe. The temperature is raised until it reaches 95°C. Then the sample is
taken out and reduction cleared hot and cold water and squeezed and it is
completely dried.

The liquor solution left in the beaker is put in spectrophotometer

and absorbance of the spent solution is measured. The initial dye solutions’
absorbance value was also measured using the spectrophotometer. The
standard values of absorbance are calculated based on the earlier graphs.
Dyeing cycle for the blends is obtained by the addition of both individual
cycles of cotton and polyester.
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4.3 EQUIPMENTS

For different technologies, the following different equipments

are used

 Conventional heater
 Ultrasonic cleaner
 Microwave oven
 Infra red dyeing machine
 Magnetic hot plate stirrer

4.3.1 Conventional Heater

The following are the specifications of conventional heater. The

setup figure is shown in Appendix – D.1. The specifications of conventional
heater are given below.

Dimensions water bath - 41cm x 30 cm

Supply voltage and frequency - 230V, 50 Hz
Heater capacity - 1000 W

4.3.2 Ultrasonic Dyeing Equipment

Dyeing experiments were carried out with flat bottom vessel,

clamped inside the ultrasonic vessel containing water. The photograph of
experimental setup is shown in Appendix – D.2. A piezoelectric ultrasonic
transducer fixed at the centre of the bottom wall of the ultrasonic cleaner
generates ultrasound of 120W power at a frequency of 50 kHz. The diffuse
sound field will be operative in the heterogeneous system comprising of dye
solution and cloth. Experiments were carried out using a dyeing drum having
120 mm x 175 mm width and having temperature and speed control.
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Experiments were carried out at 45 rpm with temperature control. Different

temperatures, processing time, concentration of liquors are maintained in the
ultrasonic vessel for studying the energy utilization. The following are the
specifications of ultrasound dyeing vessel.

Tank size - 250 x 175 x 90 mm

Power - 120 W
Tank Capacity - 3 Litres (Approx)
Tank Material - SS 304, 18G
Frequency - 34 ± 3 kHz
Generator - Built in
Timer - Digital
Power Supply - 230 V Single Phase, 50 Hz
Heater capacity - SS Strip type heater, 200 W

4.3.3 Microwave Dyeing

Microwave dyeing is carried out in a microwave oven consisting of

the following.

 a magnetron
 a magnetron control circuit (usually with a microcontroller)
 a waveguide and
 a chamber

The photograph of microwave oven is shown in Appendix – E.1.

The specifications are given below.

Power supply - 230V, 50 Hz

Power - 1400 W
Output power - 900 W
Heater output power - 1200 W
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4.3.4 Infrared Dyeing Machine

This dyeing machine comprises multiple dyeing beakers, a rotating

support assembly mounting the beakers and a frame mounting the support
assembly for moving the beakers about an axis of rotation, wherein at least
one beaker is provided with a dosing hose for supplying the beaker with a dye
or other chemical during movement of the rotating support assembly. The
figure of Infrared dyeing machine is given in Appendix F.1. The beaker
carriage present in the machine will rotate in the infrared heated zone with the
variable speed of 24 rpm to 45 rpm through A.C. frequency drive and geared
motor. The temperature obtained in the heating chamber can be up to 145˚C.
Injection dosing system is provided for making time to time additions to the
beakers without opening the beakers. A micro processor based programmer
model DC4 F/R is provided for temperature control, rate of cooling control,
rate of heating, alarm for indication of completion of process cycle and for the
setting of hold times at different temperature as required. Because of its
proper control of temperature, efficient heating occurs which minimizes
energy losses. The specifications are given below.

12 x Beakers of 250 ml - 4.5 kW

16 x Beakers of 100 ml - 4.5 kW

8 x Beakers of 500 ml - 4.5 kW

4 x Beakers of 1000 ml - 4.5 kW

18 x Beakers of 250 ml - 6 kW
12 x Beakers of 500 ml - 6 kW

8 x Beakers of 1000 ml - 6 kW
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Microprocessor based programmer model: MC 10 F/R/ DC4-F/R

Gasket for Beaker - 48 Nos

Sensor with lid - 2 No
5 CC and 10 CC dosing syringe - 1 No. each
Needle set - 1 No
Lamps - 3 Nos
Beaker Locking Spring - 6 Nos
8 Pin Relay - 1 No
Fuses - 1 set
Heater 750 W - 2 Nos

4.3.5 Magnetic Stirrer Dyeing

It consists of a hotplate and a temperature controller and a stirrer

which is shown in Appendix – E.2. The speed of the stirrer is controlled by a
knob. The specifications are given below.

Features - MR 3000 D
Speed, Max. - 1250 rpm
Load max. - 25 kg
Power consumption - 30 W
Hot plate dia. - 145 mm
Dimension l x w x h - 240m x 155m x 120m
Weight - 2.6 kg
Supply Voltage - 230 V / 50 Hz

4.4 PROCESS PARAMETERS

The process parameters varied in the different methods of

dyeing are temperature, time and concentration.
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Three different temperatures and times are chosen to dye cotton and
polyester with three colours based on the equipment capacity for experiments.
The temperature and time values for different equipments and different
materials are tabulated in Table 4.1, 4.2 and 4.3 respectively. The
concentrations (1% indicates 1 g per 100 g of fabric) are varied as 1%, 3%,
5% and 7%. The different temperatures are represented as T1, T2 and T3 and
the times are represented as t1, t2 and t3.

Table 4.1 Experiment parameters used in cotton dyeing

Temperature (˚C) Time (min)

Parameters
T1 T2 T3 t1 t2 t3
Conventional 60 80 90 100 120 140
Ultrasonicator 40 60 80 75 90 105
Microwave oven 60 80 90 75 90 105
Magnetic stirrer 60 80 90 100 120 140
Infrared dyeing 60 80 90 80 90 100

Table 4.2 Experiment parameters used in polyester dyeing

Temperature (˚C) Time (min)

Parameters
T1 T2 T3 t1 t2 t3
Conventional 80 85 95 90 110 130
Ultrasonicator 60 80 90 60 75 95
Microwave oven 75 85 95 60 75 95
Magnetic stirrer 80 85 95 90 110 130
Infrared dyeing 80 85 95 60 75 95
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Table 4.3 Experiment parameters used in blend (67% cotton and 33%
polyester) dyeing

Temperature (˚C)* Time (min)

Parameters
T1 T2 T3 t1 t2 t3
Conventional 60-80 80-85 90-95 160 200 220
Ultrasonicator 40-60 60-80 80-90 100 130 150
Microwave oven 60-75 80-85 90-95 90 110 120
Magnetic stirrer 60-80 80-85 90-95 160 200 220
Infrared dyeing 60-80 80-85 90-95 100 130 150

Note: *The first value represents temperature for cotton and second value represents
for polyester.

Different parameter values are kept for different processes due to

process constraint. The values are so chosen that they represent minimum,
maximum and likely optimum condition. For both temperature variation
experiments and time variation experiments, the concentration is kept at 4%.
When one of the parameter is changed, the other two parameters are kept
constant. The temperature is kept below 100°C to avoid evaporation of the
dye solution. Most of the non-conventional technologies are based on open
systems.