Application of

Microwaves in Textile
Finishing Processes

By:
Prof. Drago Katovic,
Sandra Bischof Vukusic
&
Sandra Flincec Grgac
Application of microwaves in textile finishing processes
By: Prof. Drago Katovic, Sandra Bischof Vukusic and Sandra Flincec Grgac

Planar microwave (MW) device for thermal treatment of textile material was constructed and tested at
Faculty of Textile Technology. The treated material, which is in a wide state, is horizontally passed through
the slots of the applicator. The feasibility of use of developed device for textile treatment was tested on
cellulose materials impregnated with different finishes: durable press, water and oil-repellent and flame
retardant. Obtained effects of microwave treatments were compared with conventional drying and curing
method and significant improvements of physical and mechanical properties were found. This might pave a
way toward use of proposed technology in textile finishing field.

Introduction

According to well known physical definition electromagnetic waves are oscillating electric and magnetic
fields traveling together through space. In the electromagnetic radiation spectrum, shown at figure 1,
microwaves (300 MHz – 300 GHz) lie between radiowave (Rf) and infrared (IR) frequencies, with relatively
large wavelength (1m-1mm) [1].

The energy of microwave photons is very low (0,125 kJ/mol)

relative to the typical energies for chemical bonds (335-84
kJ/mol); thus MW will not directly affect the molecular
structure. They cannot change the electronic structure
around atoms or among them, but they can interact with the
electronic differences between atoms.

Different materials can be divided according to their

response on microwave radiation:

The materials that reflect MW radiation (stayed cold)

The materials that is transparent to MW radiation (non-

heated)

The materials that absorb MW energy (being heated).

However, chemical reactions can be accelerated due to selective absorption of MW energy by polar
molecules, while non-polar molecules are inert to the MW radiation.

For a microwave electromagnetic field oscillating at 2, 5 GHz, which is preferred frequency for heating
applications, the charge changes polarity nearly 5 billion times per second. Microwave radiation is specially
tuned to the natural frequency of water molecules to maximise the interactions.

Some important applications of microwaves come from their interaction with various types of material. The
interaction of microwaves with dielectric materials causes a net polarization of the substance. There are
several different mechanisms of polarization: electronic polarization, ionic, molecular (dipole) polarization
and interfacial (space-charge) polarization. The overall net polarization creates a dipole moment. Dipole
rotation is an interaction, in which polar molecules or species try to align themselves with the rapidly
changing electric field of applied radiation. The motion of the molecule as it tries to orient to the field results
in a transfer of energy. The second way to transfer energy is ionic conduction that occurs if there are free
ions or ionic species present in the substance being heated.
The main difference between conventional heating with hot air and microwave heating is the heating
mechanism. While conventional techniques heat a surface, the microwaves heat the whole volume of the
treated object. During the conventional heating, the heat is generated outside the treated product and
conveyed by conduction or convection. Hence, the surface is heated at first and afterwards the heat flows
toward the inside, which always remains colder than the surface. The required internal temperature can be
reached only by sufficient increase of the surface temperature of the material above the temperature needed
for particular treatment.

On the contrary, in MW treatment, the heat is generated in a distributed manner inside of the material,
allowing more uniform and faster heating. According to the literature [2], the energy consumption is 60-70 %
lower in a case of microwave treatment.

Term "microwaves" was used for the first time in 1932nd, and its first usage was during the Second World
War in radiocommunication and radar technology. The activity of electromagnetic field of high frequency was
discovered accidentally during a radar-related research project, while testing a new vacuum tube, called a
magnetron. Until now, MW have been used for food preparation, chemical sludge, medical waste, organic
synthesis, analytics and curing of hi-tech polymers [3, 4]. Today they are widely accepted and spread to
mobile phones, television, wireless computer networks and some special applications such as rocket
engines.

Electromagnetic waves have been used in the textile finishing for the purpose of drying of thick materials,
performed at radio frequency (RF) dryers which are operating at different frequencies. This kind of dryers
are operating at frequencies of 27,12 MHz with power from 10 till 100 kW.

First idea of MW application for textile finishing processes originated in 1970-es when cellulose fabrics were
treated with Durable Press (DP) finishing agents and cured in MW oven [5]. Although these first results were
promising, the idea was abandoned till 1955, when Miller [6] patented his Pre-set process without
awareness of the earlier patent. Both cases involved garment microwave treatment, but they were
abandoned because of efforts to control the process failed. Until now, MW irradiation for textile finishing has
been used for the combined desizing, scouring and bleaching processes [7], dyeing [8] and drying
processes, as well as for eradication of insects from wool textiles [9]. Additional usage was for continuous
measuring of low humidity [10]. All this experiments were performed in a resonant cavity. Completely
different system was used in microwave device constructed by american firm Industrial Microwave System
(IMS). Treated material is passed through the waveguides in a rope state [11].

Experimental

Main idea of microwave device construction was to treat textile material on continous flow basis. It has been
achieved by passing the textile material through a slots of waveguide-based applicator. Experiments were
performed at textile material treated with different finishing processes. Cellulose material was impregnated
with baths 1-7, and passed through a waveguides.

Microwave device

Laboratory microwave device, shown in figure 2, was constructed at

the Department for Textile Chemistry and Material Testing of
Faculty of Textile Technology, University of Zagreb. This novel
system offers passage of textile material in a wide state through a
waveguides. The system consists of 6 centrally sloted rectangular
waveguides (dimensions 4 x 8 cm) and 2 magnetrons fed by 500 W.
Waveguide is terminated with water-based dummy load that
prevents leakage of residual microwave energy.
With proper design of the waveguides and supporting equipment, a specific environment (at the particular
wavelength) can be created in order to provide controlled distribution of the microwave energy, making it
possible to achieve uniform exposure to material passed through a channel. The leakage of microwave
energy is inherently small due to the fact that waveguide slots are oriented along the wave guideline of
symmetry, and therefore they cannot act as efficient slot antennas. Furthermore, in this way the material lies
in the maximum of the electric field that assures effective coupling to the flowing microwave energy. In a
case that request for slots symmetry is fulfilled, only the load (textile material) which passes through the
waveguides has an influence on energy loss. The amount of microwave energy absorbed by the textile in
each waveguide pass depends on the material thickness and moisture content.

In a case of single pass applicator, exponential decay of electric field might cause non-uniform heat
distribution. To prevent this negative tendency, the material is passed through a number of waveguide
passes. Additionally, the level of applied microwave energy is increased by the use of second magnetron,
that feeds the applicator at the other end. Meander type of traveling wave applicators provides uniform
energy distribution across the treated material.

Before this novel device comes into commercial use, the unintentional leakage of microwave energy must be
checked in order to comply with existing safety regulations of Ministry [12]. The upper limit of tolerable
microwave irradiation for professional exposure is 10 W/m2, or 1 W/m2 in higher sensibility range.
Preliminary determination of irradiation level has been performed at Department of Radio communications
and Microwave Engineering at Faculty of Electrical Engineering and Computing.

Applied material and chemicals

Pre-treated cellulose fabrics, 100% cotton (desized, scoured, bleached and mercerised) of different surface
mass: 105 and 250 g/m2 were used in the study. The fabric samples were passed through squezze rolls on
laboratory foulard, Benz, Zürih Switzerland to give wet pick up of 100% owf. Impregnation was performed
with baths containing reagents for durable press finishing (baths 1-4), water and oil repellent finishing (bath
5) and flame retardant finishing (baths 6-7), shown in Table 1. After the impregnations part of the samples
was dryed by conventional method in a tenter at 110 ºC for 2 minutes and cured in a second pasage under
the producer instructions. Second part of the samples was treated by microwaves in planar microwave
device with the speed of 0,5 m/min.

2.2.1. Durable Press (DP) Finishing

N-methylole based reagents, such as dimethyloldihydroxyethylene urea (DMDHEU), as well as newly

developed polycarboxylic acids (PCA) represented with 1,2,3,4-butanetetracarboxylic acid (BTCA) were
used in the study [13-15].

Applayed baths were containing:

DMDHEU as conventional agent with high formaldehyde (HF) content

etherified DMDHEU with low (LF) formaldehyde content
dymethylglyoxalurea (DMGU) as non-formaldehyde or free formaldehyde (FF) agent
BTCA as FF agent applied with sodium hypophosphite (SHP) catalyst.

Effects of Durable Press finishing were determined as wrinkle recovery angle (WRA) according to ISO 2313
method and tensile strength according to DIN EN ISO 1394-1. Free formaldehyde was determined by
AATCC 112 method. Whiteness degree was measured at reflective spectrophotometer Datacolor -
Spectraflash SF 300 at D 65/10 conditions with Data Match 300 program according to AATCC 110-2000
method.
2.2.2 Water and oil repellent finishing

Fluorocarbon polymers have been chosen to satisfy both water- and oil-repellency demands. Their main
characteristic is a low surface tension (aprox. 15 mNm-1) which causes excellent water and oil repellency
effects. For good oil-repellency effects the orientation of hydrophobic atoms is of primary concern.
Perfluorinated groups should be lined parallel which makes thick water and oil repellent layer [16, 17].
Because of the influence of alternating electric field it is assumed that hydrophobic fluoroalkyl groups could
rotate into the polymer substrate what will decrease the repellency. For the purpose of thermal activation of
hydrophobic FC groups microwave device have been modified with additional heated cylinder incorporated
in the system [18]. In this study FC polymer with extender included in a formulation was applied with
following concentration:

Durability of water- and oil-repellency to laundering and dry cleaning was tested after washing and cleaning
cycles. Washing was performed in apparatus: Linitest, with 5 g/l of detergent and ratio 1 : 20, at 50 ºC, for 30
min. Dry cleaning was performed according to HRN.F.S3.027; AATCC 132-1998; ISO 105-DO1. Water
repellency was tested by unstandardized Du Pont method. Tests were performed with drops of
isopropanol/water mixure in ratios: from 0/100 (W as minimal degree) till 100/0 (10 as maximal degree). Oil
repellency was tested according to AATCC 118-2002 (ISO 14419).

2.2.3. Flame retardant (FR) finishing

FR finishing was performed with high concentrations of organophosphorus reactant on cellulose material
used for working clothes, whose surface mass was 250 g/m2.

First bath (6) contains organophosphorus reactant (OFR) with conventional type of cross-linking agent
based on melamine formaldehyde (MF). This type of binding agent between celullose and
organophosphorus reactant was tried to be replaced with BTCA, which does not contain formaldehyde [19].

Effects of flame retardancy have been tested according to the method: ASTM D 626-68T. Durability to
laundering was performed according to the Soaking test method: BS 5651:1978.

3. Results and discussion

Possibility of microwave treatment application for different finishing processes was determined in the present
study.

3.1. Durable press finishing

From the results of WRA shown in tables 2 and 3 noticeable improvements can be seen in a case of
treatment with microwaves. At the same time tensile strength retention has been improved, meaning that
there is no usual negative interference with mechanical strength. Reasons of such an improvement have
been presented earlier [20], giving an explanation with more uniform crosslinking obtained with microwaves.

According to Yang mechanical strength loss can be attributed to the choice of catalyst and its concentration
rather than to the differences in the molecular structure and reagent reactivity.

Further improvement can be seen from the results of free formaldehyde release. Under the influence of
microwaves formaldehyde release has been reduced by 50% compared to conventional thermal treatment
what certainly gives an advantage to this method of treatment. Obtained reduction of formaldehyde content
has been explained with the influence of microwaves to polar formaldehyde molecules. Because of the rapid
charge changes molecules are heated resulting with expansion of the heat from the inside of the material to
the surface. Liberated formaldehyde has the same flow what causes its reduction on the textile material.
Obtained results are suggesting that because of the reduction of formaldehyde release noticed on
conventional N-methylole based products, which are cheaper and more reactive, but abandoned because of
the formaldehyde problem, can be used. Further interesting investigation to be performed would include
improvement of molecules polarity degree. In this way further formaldehyde release can be enhanced while
its quantity is further reduced or completely eliminated from the treated material.

3.2. Water and -oil repellent finishing

Comparing the results of water and oil repellent finishing, shown in tables 4 and 5, improvements of water
repellency are noticeable in a case of microwave treatment. With both thermal treatments effects of the oil
repellency are similar.

Improvements of the repellency effects are explained with the impact of the heated cylinder, which is
included in the passage of the textile material for additional improvement of FC orientation. Improvements of
the repellency effects obtained with additional thermal treatment (hot-ironing) after the tenter curing have
shown that the reaction was not completely finished, especially when thicker material was treated.

Effectiveness of the repellency after the dry-cleaning is very good with both applied curing methods.

3.3. Flame retardant finishing

Results of flame retardancy, showed in tables 6 and 7, obtained by microwave inducement are equally good
compared to conventional curing method. Application of BTCA for binding purposes gave equaly good FR
effects as conventional MF cross-linking agent which is ecologically unacceptable. Both treating baths gave
good results of flame retardancy, slightly lower after the microwave treatment. Effectivenes of flame
retardancy was tested after the washing, and results have revealed some decrease. Decrease of the results
after the washing is more noticeable at the samples which were treated by microwaves, but they are still
satisfying. Obtained durability to washing of samples treated by microwaves is confirming sufficient
crosslinking of OFR molecules with celullose molecules.

Conclusions

Results of performed investigations are indicating that microwaves are suitable for drying as well as curing
processes of textile finishing. From the results of textile finishing treatment with different finishing agents
further conclusions can be made:

Application of microwaves in Durable Press finishing offers significant improvement in comparison to the
classical curing method performed at tenter.
Microwave treatment reduces formaldehyde release.
In water and oil-repellent finishing with FC polymers MW gives certain improvements.
In flame retardant finishes with organophosphorus reagents MW are showing equally good efficiency.

Application of MW in drying and finishing process gives certain improvements of effects, but its suitability
should be preliminary tested for each reagent.

Favorable effects obtained by MW and treatments cost are indicating good possibility of its implementation
in praxis. After the conclusion of laboratory experiments, construction of an industrial microwave device is to
be expected.
References:

1. Bartolić J.: Inženjerski priručnik: Mikrovalna elektronika, Školska knjiga Zagreb 1999, 627-717
2. Metaxas A.C., R.J. Meredith: Industrial Microwave Heating, Peter Peregrinus 1983, 111-150
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(2001) 1, 193 - 198
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Synthesis, .Org.Chem 59 (1994) 3408 – 3412
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1112
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Cotton Fabrics, J.Text.Institute (1996) 3, 602-607
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dyeing, Colourage 49(2002)12, 83-88
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Conservation 21 (1982) 2, 1-34
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(19) 10, 2-4
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Prosinca 2003.g.
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560
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with Polycarboxylic Acid, AATCC Review 2 (2002) 4, 39-42
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Fabrics, Textile Reaearch Journal 73 (2003) 8, 733-738
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Institute 83rd World Conference, Shangai, May 23-27, 2004, 1165-1169
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List of Tables
Tab.1 Applied agents and treatment conditions

Treatment Agents Conditions

Durable Press (DP) Finishing
1 DMDHEU 120 g/l T = 150 oC
MgCl2 18 g/l t = 4 min
Surfactant 1-2 g/l
o
2 Etherified DMDHEU 120 g/l T = 150 C
MgCl2 18 g/l t = 4 min
Surfactant 1-2 g/l
o
3 Dimethyl glyoxal urea (DMGU) 180 g/l T = 150 C
MgCl2 30 g/l t = 4 min
Surfactant 1-2 g/l
o
4 BTCA 60 g/l T = 180 C
Sodium hypophosphyte monohydrate (SHP) 65 g/l t = 90 s
Surfactant 1-2 g/l
Water Repellent and Oil Repellent Finishing
o
5 Fluorcarbon polymer (FC) 60 g/l T = 180 C
t = 90 s
Flame retardant (FR) Finishing
6 Organophosphorus flame retardant (OFR) 400 g/l T = 150 oC
Melamine formaldehyde (MF) 70 g/l t = 5 min
H3PO4 (80%) 24 g/l
Surfactant 1-2 g/l
7 Organophosphorus flame retardant (OFR) 400 g/l T = 180 oC
BTCA 70 g/l t = 90 s
Sodium hypophosphyte monohydrate (SHP) 65 g/l
Surfactant 1-2 g/l

Tab. 2 Effects of Durable Press finishing on cotton material (105 g/m2) treated conventionally

Bath Treatment pH WRA TS WICIE Formaldehyde

α60 W+F (º) (%) (ppm)
/ Untreated / 110 100,0 75,45 0
1 DMDHEU 5,55 215 48,7 74,36 1600
2 Etherified DMDHEU 6,73 195 66,0 75,34 300
3 DMGU 6,47 149 77,5 74,17 0
4 BTCA 2,33 202 66,3 72,31 0

Tab. 3 Effects of Durable Press finishing on cotton material (105 g/m2) treated by microwaves

Bath Treatment pH WRA TS WICIE Formaldehyde

α60 W+F (º) (%) (ppm)
/ Untreated / 110 100,0 75,45 0
1 DMDHEU 5,55 238 61,5 72,71 750
2 Etherified DMDHEU 6,73 209 62,0 75,23 150
3 DMGU 6,47 181 83,6 74,71 0
4 BTCA 2,33 225 80,2 72,00 0
 Tab. 4 Effects of water and oil-repellent finishing on both cotton materials treated conventionally

Bath Treatment Water Repellency Oil Repellency

Du Pont method AATCC 118 method
105 g/m2 250 g/m2 105 g/m2 250 g/m2
* * * *
5 FC 7 7 10 10 6 6 6 6
Washing 6 7 5 7 6 6 6 6
Dry-cleaning 6 7 6 6 6 6 6 6
* Additional thermal treatment

Tab. 5 Effects of water and oil-repellent finishing on both cotton materials treated by microwaves

Bath Treatment Water Repellency Oil Repellency

Du Pont method AATCC 118 method
2 2 2 2
105 g/m 250 g/m 105 g/m 250 g/m
* * * *
5 FC 8 10 10 10 6 6 6 6
Washing 6 9 3 6 6 6 3 5
Dry-cleaning 8 7 6 7 6 6 6 6
* Additional thermal treatment

Tab. 6 Effects of flame retardant finishing on cotton material (250 g/m2) treated conventionally

Bath Treatment Time of: after flame tf after Char length (mm)
glow tg (s)
/ Untreated tf = 21 , tg= 56 burned completely
6 OF / MF neither burn nor glow 55
OF / MF –1 washing neither burn nor glow 75
7 OF / BTCA neither burn nor glow 49
OF/BTCA –1 washing neither burn nor glow 54

Tab. 7 Effects of flame retardant finishing on cotton material (250 g/m2) treated by microwaves

Bath Treatment Time of: after flame tf after Char length (mm)
glow tg (s)
/ Untreated tf = 21 , tg= 56 burned completely
6 OF / MF neither burn nor glow 60
OF / MF –1 washing neither burn nor glow 140
7 OF / BTCA neither burn nor glow 62
OF/BTCA –1 washing neither burn nor glow 103

About the Authors:

Prof. Drago Katovic, Sandra Bischof Vukusic and Sandra Flincec Grgac are associated with the Faculty of
Textile Technology, University of Zagreb, Department of Textile Chemistry and Ecology.

This paper is original scientific paper, UDK.

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