Project Final 18.10.2018

DEPARTMENT OF TEXTILE ENGINEERING
Course No.: Tex 400
Course Title: Project Work
Academic Semester: Fall 2017
Project Report on
Study on crease recovery finish of silk fabric with Citric acid and DMDHEU as
finishing agent
Submitted by
Name of the student Student ID No.
Mizanur Rahman Parvez 14.01.06.004
Tausif Mahmud Siam 14.01.06.044
Md.Faisal Ahmed 14.01.06.097
Md.Arif Anwar 10.02.06.018
Supervised by
Ms.Shaima Islam Ms. Nahida Akter
Assistant Professor Assistant Professor
Ahsanullah University of Science and Technology
November, 2018
ii
Study on crease recovery finish of silk fabric with Citric acid and DMDHEU as finishing agent
i
ACKNOWLEDGMENTS
All praise to the Almighty Allah, the omnipresent and the most merciful for giving us the
strength and ability to complete our project work successfully.
We would like to express our thankfulness to the most precious person in our lives, our
parents for their moral and financial support.
We convey our eternal gratitude to our project supervisor Ms. Shaima Islam, Assistant
professor, Department of Textile Engineering, Ahsanullah University of Science and
Technology (AUST), for her immense support, for providing us with necessary information
related to our project work, for her continuous encouragement and valuable suggestions.We
would also like to manifest our earnest thanks to our Co-supervisor Ms. Nahida Akter,
Assistant Professor, Department of Textile Engineering, Ahsanullah University of Science
and Technology (AUST), for her support and constructive critisism.Without their kind
direction, proper guidance this project would have been a little success.
Our heartiest thanks to Dr. Lal Mohan Baral, Professor and Head of the Department of
Textile Engineering, Ahsanullah University of Science and Technology (AUST), for his co-
operation and support.
We would like to express our special thanks to Dr. Mustafizur Rahman, Professor,
Department of Textile Engineering, (AUST) for always inspiring and motivating us to our
studies.
We would also like to manifest our thankfulness to Mr. Nirjhar Ahmed, Assistant Professor,
National Institute of Textile Engineering and Research (NITER) for allowing us to carry
some of our tests of the project at their renowned institute. We would also like to thank our
lab assistants for their co-operation.
Lastly, we would like to acknowledge that we remain responsible for all the errors and
inadequacies which might certainly remain.
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Table of Contents
Chapter 1: Introduction ......................................................................................................... 1
1.1 Introduction ...................................................................................................................... 2

1.2 Objectives ....................................................................................................................... 3
1.3 Background study/ previous work ................................................................................... 4
Chapter-2: Literature Review ................................................................................................ 5
2.1 Silk ................................................................................................................................... 6

2.2 History of silk .................................................................................................................. 6
2.2.1 The origins ................................................................................................................ 6

2.2.2 Silk production outside china .................................................................................... 7
2.3 Properties and composition of silk................................................................................... 7
2.3.1 Physical properties of silk ......................................................................................... 8

2.3.2 Chemical properties of silk ....................................................................................... 9
2.3.3 Chemical composition of silk ................................................................................. 10
2.3.4 Amino acid composition of sericin and fibrion ...................................................... 12
2.4 Pretreatment of silk ........................................................................................................ 13
2.4.1 Objectives of pretreatment ...................................................................................... 13

2.4.2 Pretreatment process ............................................................................................... 13
2.5 Crease............................................................................................................................. 14
2.5.1 Reasons behind crease formation in silk ................................................................. 14

2.5.3 Mechanism of crease formation .............................................................................. 15
2.5.4 Creases and Wrinkles .............................................................................................. 17
2.6 Finishing ........................................................................................................................ 18
2.6.1 Types of textile finishing ........................................................................................ 18
2.7 Resin finish .................................................................................................................... 19
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2.7.1 History of resin finish ............................................................................................. 19
2.7.2 Fundamentals of silk finishing with resin ............................................................... 20
2.7.3 Effect of resin .......................................................................................................... 20
2.8 Crosslinking Agents ...................................................................................................... 20
2.8.1 DMDHEU ............................................................................................................... 21

2.8.2 Effect of DMDHEU on fabric ................................................................................. 22
2.8.3 Citric Acid ............................................................................................................... 22
2.8.4 Citric Acid for crease resistant finishes .................................................................. 22
2.8.5 Effect Of Citric Acid on Silk .................................................................................. 23
2.9 Catalysts ......................................................................................................................... 23
2.9.1 Magnesium chloride ................................................................................................ 24

2.9.2 Sodium Hypophosphite ........................................................................................... 24
2.9.3 Effect of curing temperature and time .................................................................... 25
2.10 Softener ........................................................................................................................ 25
2.10.1 Types of Softeners ................................................................................................ 25

2.10.2 Function of Softeners ............................................................................................ 26
2.11 Padding ........................................................................................................................ 26

2.12 Drying .......................................................................................................................... 27
2.13 Curing .......................................................................................................................... 28
Chapter 3: Materials & Methods ......................................................................................... 29
3.1 Materials ........................................................................................................................ 30
3.1.1 Fabric ...................................................................................................................... 30
3.2 Pre-Treatment Chemicals .............................................................................................. 31

3.3 Finishing Chemicals ...................................................................................................... 32
3.4 Experimental Equipments .............................................................................................. 34
3.4.1 Padding Machine .................................................................................................... 34

3.4.2 Stenter Machine ...................................................................................................... 35
3.4.3 Electric Weight Balance.......................................................................................... 35
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3.4.4 Hand Dryer.............................................................................................................. 36
3.5 Testing Equipments ....................................................................................................... 36
3.5.1 Spectrophotometer .................................................................................................. 36

3.5.2 Tearing strength Tester ........................................................................................... 37
3.5.3 Crease Recovery Tester .......................................................................................... 37
3.5.4 Titan Universal Strength Tester .............................................................................. 38
3.6 Methods ......................................................................................................................... 39
3.6.1 Methodology ........................................................................................................... 39

Step:1 Determination of Suitable Temperature and Time ............................................... 39
Step:2 Determination of Suitable Concentration of Citric Acid & Resin (DMDHEU) .. 40
3.6.2 Recipe for degumming of silk ................................................................................. 41
3.6.3 Recipe for resin finish ............................................................................................. 41
3.7 Testing Methods ............................................................................................................ 44
3.7.1 Determination of the recovery from creasing of a horizontally folded specimen by

measuring the angle of recovery. ..................................................................................... 44
3.7.2 Tear properties of fabrics -- Part 1: Determination of tear force using ballistic
pendulum method (Elmendorf) ........................................................................................ 45
3.7.3 Breaking Force and Elongation of Textile Fabrics by Grab Method. ..................... 46
3.7.4 Determination of Whiteness Index ......................................................................... 46
Chapter 4: Results and Discussions...................................................................................... 48

Chapter 5: Conclusion ........................................................................................................... 89
5.1 Key Findings .................................................................................................................. 90

5.2 Limitations ..................................................................................................................... 91
5.3 Conclusion ..................................................................................................................... 91
References ............................................................................................................................... 93
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List of Figures
Chapter 2:
Figure 2.1: The structure of raw silk fibre ............................................................................... 11
Figure 2.2: Mechanical influences on crease resistance and recovery .................................... 17
Figure 2.3: Types of Textile Finishing ................................................................................... 18
Figure 2.4: Molecular structure of DMDHEU ......................................................................... 21
Figure 2.5 : Citric Acid ............................................................................................................ 22
Figure 2.6 : Magnesium Chloride ............................................................................................ 24
Figure 2.7: Sodium Hypophosphite ......................................................................................... 24
Figure 2.8: Types of Dryers .................................................................................................... 28
Chapter 3:
Figure 3.1:Horizontal Padding machine .................................................................................. 34
Figure 3.2: Laboratory Stenter Machine .................................................................................. 35
Figure 3.3: Electric Precision Balance ..................................................................................... 35
Figure 3.4: Hand Dryer ............................................................................................................ 36
Figure 3.5: Spectrophotometer................................................................................................. 36
Figure 3.6: Tearing Strength Tester ......................................................................................... 37
Figure 3.7: Crease Recovery Tester ......................................................................................... 37
Chapter 4:
Figure 4.1: Crease Recovery Angel of Silk Fabric after the Application of Citric acid .......... 50
Figure 4.2: Crease Recovery Angel of Silk Fabric after the Application of Resin ................. 52
Figure 4.3: Whiteness Index after Citric Acid Application ..................................................... 54
Figure 4.4: Whiteness Index of Silk Fabric after Resin Application ....................................... 56
Figure 4.5: Tear Strength Retention (%) of Warp after Citric Acid Application ................... 58
Figure 4.6: Tear Strength Retention (%) of Weft after Citric Acid Application ................... 59
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Figure 4.7: Tear Strength Retention (%) of Warp after Resin Application ............................ 61
Figure 4.8: Tear Strength Retention (%) of Weft after Resin Application ............................. 62
Figure 4.9: Tensile Strength Retention (%) of Warp after Citric Acid Application ................ 64
Figure 4.10: Tensile Strength Retention (%) of Weft after Citric Acid Application .............. 65
Figure 4.11: Tensile Strength Retention (%) of Warp after Resin Application...................... 67
Figure 4.12: Tensile Strength Retention (%) of Weft after Resin Application ....................... 68
Figure 4.13: Crease Recovery Angle of Silk Fabric after the Application of Citric Acid at
Various Concentration ............................................................................................................. 70
Figure 4.14: Crease Recovery Angle of Silk after the Application of Resin at Various
Concentration ........................................................................................................................... 72
Figure 4.15:Whiteness Index of Silk after Citric Acid Application at Various Concentration74
Figure 4.16:Whiteness Index of Silk after Resin Application at Various Concentration ........ 76
Figure 4.17: Tear Strength Rentention (%) of Silk after Application of Citric Acid at Various
Concentration ........................................................................................................................... 78
Figure 4.18: Tear Strength Retention(%) after Application of Resin at Various Concentration
.................................................................................................................................................. 81
Figure 4.20: Tensile Strength Retention (%) of Silk Fabric after the Application of Resin at
Various Concentration ............................................................................................................. 87
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List of Tables
Chapter 2:
Table 2.1: Physical Properties of Different Type of Silk Fibre ................................................. 9

Table 2.2: Amino Acid Composition of Sericin and Fibrion.................................................. 12
Chapter 3:
Table 3.1: Specification of Fabric ............................................................................................ 30

Table 3.2:Specification of Wetting Agent ............................................................................... 31
Table 3.3: Specification of sequestering Agent ....................................................................... 31
Table 3.4 Specification of soap ................................................................................................ 31
Table 3.4: Specification of Citric Acid .................................................................................... 32
Table 3.5: Specification of DMDHEU .................................................................................... 32
Table 3.6: Specification of Silicone softener ........................................................................... 33
Table 3.7: Specification of Padding Mangle........................................................................... 34
Table 3.8: Specification of Stenter Machine........................................................................... 35
Table 3.9: Specification of Electric Precision Balance ............................................................ 35
Table 3.10: Specification of Hand Dryer ................................................................................. 36
Table 3.11: Specification of Datacolor SF650 Benchtop Spectrophotometer ......................... 36
Table 3.12: Specification of Crease Recovery Tester .............................................................. 37
Table 3.13: Recipe of Degumming .......................................................................................... 41
Table 3.14: Recipe of Resin Finish With DMDHEU & Softener............................................ 41
Table 3.15: Parameters For Resin Finishing ............................................................................ 42
Chapter 4:
Table 4.1: Crease Recovery Angle of Silk Fabric after the Application of Citric Acid .......... 49
Table 4.2: Crease Recovery Angle of Silk Fabric after the Application of Resin ................... 51
Table 4.3: Whiteness Index of Silk Fabric after Application of Citric acid ............................ 53
Table 4.4: Whiteness Index of Silk Fabric after Application of Resin .................................... 55
Table 4.5: Tear Strength of Silk after the Application of Citric Acid ..................................... 57
Table 4.7: Tensile Strength of Silk Fabric after the Application of Citric Acid ...................... 63
Table 4.8: Tensile Strength Retention (%) of Silk Fabric after the Apllication of Resin ........ 66
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Table 4.9: Crease Recovery Angle of Silk after Citric Acid Application at Various
Concentration ........................................................................................................................... 69
Table 4.10: Crease Recovery Angle of Silk after Resin Application at Various Concentration
.................................................................................................................................................. 71
Table 4.11: Whiteness Index of Silk after Citric Acid Application at Various Concentration
................................................................................................................................................. .73
Table 4.12: Whiteness Index of Silk after Resin Application at Various Concentration ........ 75
Table 4.13: Tear Strength Retention (%) of Silk after Citric Acid Application at Various
Concentration ........................................................................................................................... 77
Table 4.14: Tear Strength Test of Silk after Resin Application at various concentration ....... 79
Table 4.16 :Tensile Strength of Silk after the Application of Resin at Various Concentration :
.................................................................................................................................................. 85
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Abstract
In this project work crease resistance finishes on silk fabric were studied. Here silk fabric was
treated with citric acid and dimethylol dihydroxy ethylene urea (DMDHEU) as finishing
agents, varying curing time (1,2,3 and 4 min) and curing temperature (130° C,140° C,150°
C,160° C,170° C).The concentration of both finishing agents were also varied in a manner,
citric acid (40g/l, 70g/l, 100g/l, 130g/l) & DMDHEU (60g/l, 80g/l, 100g/l, 120g/l).Sodium
hypophosphite (𝐍𝐚𝐏𝐎𝟐 𝐇𝟐 ) and Magnesium Chloride (𝐌𝐠𝐂𝐥𝟐 ) were used as catalyst for
citric acid and resin (DMDHEU) respectively. This study reports that 150°C curing
temperature and 2 minutes curing time is suitable for both citric acid & resin (DMDHEU) as
with increasing curing temperature and time reduces whiteness index. Samples treated with
dimethylol dihydroxy ethylene urea (DMDHEU) shows better crease recovery angle (121°-
177°) than citric acid (122°-156°).The finished fabric treated with citric acid retained 83.10
% to 97.77% breaking strength and there was an increase of 101% to 115% in its tear
strength. Where the finished fabric treated with dimethylol dihydroxy ethylene urea
(DMDHEU) retained 89.12% to 99.95% breaking strength and shows an increase of 111% to
118% in its tear strength retention (%).
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Chapter 1: Introduction
1
1.1 Introduction
Silk is one of the most luxurious and beautiful natural fibers, possessing excellent luster, wearing
comfort, soft handle, good air permeability, excellent draping quality and aesthetic appearance in
materials, and has been known as the ‘queen of fibers’ since its discovery, silk is produced in
small quantities: about 130,000 tons per year and has remained a special fiber the human skin,
hence it can also be used in biomedical applications such as sutures, prosthetic arteries and
bandages [1].The poor wet resiliency of silk is caused by the structure of the fiber. Unlike wool
keratin, silk fibroin has no cystine residue, so that there are no chemical cross-linkages between
the protein polymers. When the fiber absorbs water and swells, the salt linkages between
polymers, which give the fiber high dry wrinkle recovery, are broken. Because there are no
chemical cross-linkages which do not break easily in water, thus the silk fiber has poor wet
wrinkle resistance. Adding chemical cross-linkages to the structure restrict the relative
movement of the polymers of silk fiber for use in high value textiles. The amino acid
composition of silk protein is close to that of water, therefore the resiliency of silk can be
improved [2].
2
1.2 Objectives
a) To improve the crease recovery of silk in an eco-friendly way.
b) To study the effect of Citric acid and dimethylol dihydroxy ethylene urea on silk fabric.
c) To investigate Crease recovery angle, tensile strength, tearing strength, whiteness, after
operations.
3
1.3 Background study/ previous work
Y.Yang and S. Li studied about a non-formaldehyde crease-resistant finishing method for silk.It
has been developed using citric acid as a crosslinking agent. Both the dry and wet resiliency of
finished silk were remarkable increased [9].
P.K. Hari, M.L. Gulrajani & N.K. Pal studied to improve the crease recovery of silk fabrics,
dimehylol ethylene urea (DMEU) was applied to control, photo-graded and esterified silk
fabrics. The effect of crosslinking was evaluated qualitatively by creasing the fabtic and
recovering the resin periods. The results indicate that although there is some improvemnt in the
immediate recovery, none of the samples is crosslinked with DMEU [11].
Choi HM, Park M, Oh KW used Glyoxal as a crosslinking agent for silk. They used acid
pretreatment or addition of a Bronsted-Lowry acid such as sulfuric acid or formic acid in the bath
to improve conditioned wrinkle recovery angle (CRA) of the treated silk [35].
4
Chapter-2: Literature Review
5
2.1 Silk
Silk is one of the oldest fibres known to man. It is an animal fibre produced by certain insects to
build their cocoons and webs. Although many insects produce silk, only the filament produced
by the mulberry silk moth Bombyxmori and a few others in the same genus is used by the
commercial silk industry. Over the centuries, silk has been regarded as a highly valued textile
fibre. Its qualities of strength, elasticity, softness, absorbency, affinity for dyes and adaptability to
various forms of twisting continue to meet various applications. Because of its high (tensile)
strength, lustre, durability and ability to bind chemical dyes, silk is still considered a leading
textile material [1].
The quantity of silk produced is so small as to amount to only about 0-25 per cent of the total
fibre production. But silk has always held a special position as a quality fibre, and sustains a high
price by comparison with other fibres [2]..
2.2 History of silk
Silk is one of the oldest known textile fibers According to the Chinese, it was used as long ago as
the twenty-seventh century BC. Silk is originally native to China; for many centuries, the
production of silk was a secret process known only to the Chinese. China successfully guarded
the secret until 300 AD, when Japan and India discovered it [3].
2.2.1 The origins
According to Confucius, the discovery of silk goes back to 2640 bc. Legends say that a Chinese
princess, Xi Lin Shi, was drinking tea in a mulberry garden when a cocoon dropped into her cup.
The hot tea dissolved the hard outer layer of the cocoon. In trying to extract it with her long
finger nail, she discovered that the cocoon contained a continuous filament. As she kept pulling
on the thread, it continued to unwind. The princess had just invented the first technique of reeling
silk. At that time in China’s history, weaving was already well-established, so it was possible to
convert this new-found fibre into fabric.
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2.2.2 Silk production outside china
Although silk fabrics were exported from China throughout south-east and central Asia, the most
important fact for the future of silk was the loss of China’s production monopoly. Silk as we
know it is produced by the domesticated silkworm, Bombyx mori,which originated in the wild,
but numerous other varieties of wild silkworm existed in various countries, notably India, which
is still the world’s major producer of wild silk. Bombyx mori sericulture is thought to have
spread to India through Khotan in Chinese Turkestan around 140 BC.
Sericulture was introduced to Korea by Chinese immigrants in about 1200 BC and from there it
reached Japan.
Seven Roman legions under the command of Marcus Licinius Crassus, their lines of
communication stretched to the limit, came into conflict with an army composed of Parthian
tribesmen near the city of Carrhae (today, Harran in Turkey).The result of the battle was a
disastrous defeat for the Roman army and the death of its commander. Apart from the terrible
efficiency of the Parthian archers, one of the factors which contributed to the utter
demoralization of the legionaries was the sight and sound of the banners which the Parthians
unfurled near the end of the day. These brilliantly colored and embroidered banners were the first
contact the Romans had with silk. From then on, silk was to become a feature of Roman life,
either through trade or as the spoils of more successful campaigns beyond the eastern reaches of
the Empire [4].
2.3 Properties and composition of silk
The important physical characteristics of different silks include the silk filament length, fiber
fineness, and fiber density. On the other hand Raw silk is composed of two important proteins:
fibroin (the silk filament) and sericin (the gum). Each raw silk strand in the cocoon is known as
“bave”; it is composed of two fibroin filaments called “brin” that are held together by sericin
gum [3].
7
2.3.1 Physical properties of silk
The physical characteristics are determined by the structure of the macromolecule composing the
fibroin. Part of the macromolecule is made up of amino acids with a low molecular weight,
offering a series of crystalline regions which confer a high degree of tenacity on the fibre. The
rest of the macromolecule is characterized by the presence of amorphous areas enclosing amino
acids of a relatively higher molecular weight. The presence of both crystalline and amorphous
zones makes for a combination of strength, flexibility and elasticity [4].
Tensile strength
Tensile Strength Silk is a strong fibre. It has a tenacity usually of 30.9-44.1 cN/tex (3.5-5.0
g/den). Wet strength is (75-85)% of the dry strength
Elongation
Silk filaments have an elongation at break of (20-25)% under normal conditions.
Elastic Properties
The elastic recovery of silk after spinning is not good as that of wool, but is superior to that of
cotton or rayon. Once it has stretched by about 2 % of its original length, silk tends to remain
permanently stretched. There is a slow elastic recovery or creep after extension, but the silk does
not regain its original length.
Specific Gravity
Degummed silk is less dense than cotton, flax, rayon or wool. It has a specific gravity of 1-25.
Silk fabrics are often weighted by allowing the filaments to absorb heavy metallic salts; this
increases the density of the material and affects its draping properties
8
Effects of Moisture
Like wool, silk absorbs moisture readily. It can take up a third of its weight of water without
feeling wet to the touch. Silk has a regain of 11.0% [2].
Physical properties of different type of silk fibre
The Physical properties of different type of silk fibre was shown in the Table 2.1
Table 2.1: Physical Properties of Different Type of Silk Fibre
Types of silk cocoon Fibre density Fibre NBFL (m) Total

g/cm3 fineness Filament
Non Breaking
(den) Length (m)
Filament
length)
Mulberry(biovoltine) 1.34 2-3 700-800 1200-1600
Mulberry(multivoltine) 1.34 2-3 400-600 900-1200
Tasar 1.31 8-12 100-250 750-900
Oak Tasar 1.31 3-5 300-450 800-100
2.3.2 Chemical properties of silk
Because silk is a protein fiber, it is composed of different amino acids. The properties of proteins
depend primarily on the properties of the reactive groups of their constituent amino acids
combined with the properties associated with the size of the protein. Amino acids are bi
functional,i.e., they contain both acidic carboxyl(COO–) and basic amino (𝐍𝐇𝟑 +) group in their
molecular structure, thereby acting as a zwitterion [3].
9
Effect of Acids
The fibroin of silk can be decomposed by strong acids into its constituent amino acids. In
moderate concentration, acids cause a contraction in silk; this shrinkage is used to bring about
crepe effects in silk fabrics
Effect of Alkalis
Silk is less readily damaged by alkali than is wool. Tussah silk is particularly resistant. Weak
alkalis such as soap, borax and ammonia cause little appreciable damage. More concentrated
solutions of caustic alkalis will destroy the luster and cause loss of strength.
Effect of Organic Solvents
Silk is insoluble in the dry-cleaning solvents in common use.
Electrical Properties
Silk is a poor conductor of electricity, and tends to acquire a static charge when it is handled.
This causes difficulties during manufacture, particularly in a dry atmosphere [2].
2.3.3 Chemical composition of silk
Silk cocoons are composed of proteins, which account for more than 95% of its content; other
impurities, such as waxes, mineral salts, and ash, constitute about 4–5%.[3]. Silk filament
contains the following (by total weight):
 72–81% fibroin;
 19–28% sericin;
 0.8–1.0% fat and wax and
 1.0–1.4% colouring matter and ash [1].
10
Figure 2.1: The structure of raw silk fibre
The silk fiber after degumming contains fibroin protein. Both fibroin and sericin are protein
substances built up of 16-18 amino acids, out of which only glycine, alanine, serine and tyrosine
make up the largest part of the silk fibre and the remaining amino acids containing bulky side
groups are not significant. Glycine (about 44%), followed by alanine (about 29%), are the main
amino acids present in the mulberry silk fibroin; whereas in wild silks, alanine (about 40%),
followed by. glycine (about 25%), are the highest amino acid present.[3] Textile silk from the
moth Bombyxmori has a much simpler protein composition. There is no cystine to crosslink
chains. About 80% consists of amino-acid residues with the three simplest side-groups, –H, –
𝐂𝐇𝟑 and – 𝐂𝐇𝟐 𝐎𝐇 [6]
11
2.3.4 Amino acid composition of sericin and fibrion
The amino acid composition of sericin and fibroin was shown in the Table 2.2 [5]
Table 2.2: Amino Acid Composition of Sericin and Fibrion
Amino acids Side groups Sericin (% mol) Fibrion (% mol)
Glycine H− 14.75 45.21
Alanine 𝐂𝐇𝟑 − 4.72 29.16
Serine 𝐂𝐇𝟐 (𝐎𝐇) − 34.71 11.26
Tyrosine 𝐎𝐇𝐂𝟔 𝐇𝟒 𝐂𝐇𝟐 − 3.75 5.14
Component (%) Mulberry Tusser Muga Eri
Fibroin 66-72 78-85 80-86 82-88
Sericin 25-32 14-17 12-16 11-13
Wax 0.3-0.4 1-2 0.5-1 1.5-2.2
Minerals,Ash and 0.7-0.8 3-4 2-3 2-3

others
12
2.4 Pretreatment of silk
For perfect coloration of substrate, it is necessary that all the impurities be removed from the
surface so that the colorants can perfectly sit on the surface or penetrate inside the substrate as
required by the particular system. The colorants should also be clearly visible without
interference by the color of impurities.
2.4.1 Objectives of pretreatment
1. To convert the fabric from hydrophobic to hydrophilic state.
2. To remove dust, dirt etc. from the fabric.
3. To prepare the fabrics for the subsequent process.
The aim of pretreatment is to treat the goods by standard procedures so that they are brought to a
state in which they can be dyed, printed or finished without showing any fault or damage on the
material.
2.4.2 Pretreatment process
Degumming or boiling-off is the process employed to remove the silk gum (sericin) enveloping
the two raw silk threads (fibrion).The gum is not completely removed in every case. The extent
of degumming gives rise to different varieties of silk.
Degumming of silk with soap
Degumming is effected by careful boiling-off in soap baths which should be slightly alkaline.
The fibre is treated with soap solution to give a pH around 10.0 at 90-95°C for 1.5-2 hours.In
order to avoid lien soap deposits and resulting stains, the water should be properly softened.
Sequestering agent may be added in the bath to correct the hardness of water [11].
13
2.5 Crease
Crease is a fold in fabric introduced unintentionally at some stages of processing. Creasing or

crushing of a textile material is a complex effect involving tensile, compressive, flexing and
torsional stresses [7].
Whereas crease resistance is the ability of a material to resist, or recover from, creasing. Crease
recovery is a specific measurement of crease resistance that determines the crease recovery
angle. It is therefore a quantitative method of analysis [10].
2.5.1 Reasons behind crease formation in silk
The main reasons for the formation of crease are the low crystallinity and high void content of
silk fibroin, and the large number of hydrogen bonds and salt bonds between the silk fibers.
Under an external force, the silk fibers can slip and form hydrogen bond in new positions. When
the external force is removed, the fibers do not recover completely, resulting in crease formation.
Crease-resistant finishes function by filling the amorphous regions with resin and inducing
chemical cross linking to prevent the silk fibers from slipping [8].
Silk has low wet resiliency. It causes considerable inconvenience in the use of silk textiles'
because it creases easily during home laundering or when wet. The poor resiliency of silk is
caused by the structure of the fiber. Unlike wool keratin, silk fibroin has no cysteine residue, so
that there are no chemical cross linkages between the protein polymers. When the fiber absorbs
water and swells, the salt linkages between polymers, which give the fiber high dry wrinkle
recovery, are broken. Because there are no chemical cross linkages which do not break easily in
water, the silk fabric has poor wet crease resistance [9].
2.5.2 Crease formation in cotton
Crease formation of the fabric is one of the most important factors that influences the quality of
the fabric. The appearance of a garment and its care characteristics during wearing or after
frequent washing will produce an uneven surface on the cloth which is not desired. This uneven
14
area on the garment surface is known as the crease. Creases are are of greatest concern in the
sports and leisure and clothing market sectors, but also relevant to the interiors market sector.
Creases may be unslightly, and usually reduce the lifespan of a textile by making it more
susceptible to abrasion. [31].
2.5.3 Mechanism of Crease Formation
The primary cause of the shrinkage of cellulosic fibers is the fact that these fibers can readily
absorb moisture. This absorbed moisture facilitates internal polymer chain movements in the
amorphous fiber areas by lubrication. It disrupts the internal hydrogen bonding between these
polymer chains. When a moisture laden cellulosic fiber is stressed, the internal polymer chains of
the amorphous areas are free to move to relieve that stress. Hydrogen bonds can reform between
the polymer chains in their shifted positions, in effect locking in the new configuration. With no
restoring forces available, a newly formed crease will remain until additional processes (ironing
for example) apply adequate moisture and mechanical forces to overcome the internal forces
[32].
Figure 2.2: Mechanism of crease formation
15
During washing or folding, the remaining hydrogen bonds break easily and after drying new
hydrogen bonds form with the chains in their new position and creases are stabilized. When a
cotton cloth is folded and pressed. Some of the hydrogen bonds at the boundary of the crystalline
and amorphous region break. Hydrogen bonding forces are fairly weak, simultaneously free
hydroxyl in the amorphous region approach to other free hydroxyl groups and when they are
sufficiently close to each other they get bound. These newly formed hydrogen bonds bind the
molecules and prevent unfolding crosslink between the polymer chains can be introduced by
crosslinking chemicals, then it reinforced the cotton fibers and prevent the permanent
displacement of the polymer chains when the fibers are stressed. It is therefore much more
difficult for creases to form or for the fabic to shrink on washing [33].
16
2.5.4 Creases and Wrinkles
There are numerous mechanical factors that influence crease resistance and recovery, described
below in Figure 2.2-
Mechanical
influences on
crease
resistance and
recovery
Fabric
Fibre property
construction
Coefficient of Bending Bending Yarn Type of

friction modulus recovery construction weave/knit
Bending
recovery of a Filament-to-
High inter- single fibre filament
fibre friction High modulus has the friction Tightness of
will not allow fibres less greatest between yarns weave/knit
fabric to likely to bend. influence on will prevent influences
reshape the recovery return to the recovery
of the whole original linear
fabric construction
Figure 2.2: Mechanical influences on crease resistance and recovery
17
2.6 Finishing
Textile Finishing is a process used in manufacturing of fiber, fabric, or clothing. In order to

impart the required functional properties to the fiber or fabric, it is customary to subject the
material to different type of physical and chemical treatments. For example wash and wear finish
for a cotton fabric is necessary to make it crease free or wrinkle free. In a similar
way, mercerizing, singeing, flame retardant, water repellent, water proof, antistatic finish, peach
finish etc are some of the important finishes applied to textile fabric.
2.6.1 Types of textile finishing
Textile
Finishing
Chemical Mechanical
Finishing Finishing
Temporary Permanent
Reactive Type Deposition Finish Finish
Of Finish Type Of Finish Eg.Calendering Eg.Sanforising
1.Anti Shrink Crease

Optical
2.Flame Resistance
Brightening
Retardant Finishing
Figure 2.3: Types of Textile Finishing

18
2.7 Resin finish
In polymer chemistry and materials science resin is a “solid or highly viscous substance”, which
is typically convertible into polymers. Such viscous substances can be plant derived or synthetic
in origin, and they are often mixtures of organic compounds. Resin finishing is also termed as
wash-and-wear finish, anti-crease finish, crease-resistant finish, durable press finish or wrinkle-
free finish [11]
The terms easy care, wrinkle resistant, wash and wear, no-iron, durable press and permanent
press have all been applied to this type of finish and although they maydenote different levels of
performance, they are often used interchangeably. They function by introducing cross-links
between the cellulose molecules of cotton and rayon and by so doing reduce the swell ability and
extensibility of the fibers but increase their resilience. The crosslinking results in a fabric with a
“memory” that tends to return to the state it was in when the cross-links were introduced. Thus if
a fabric is smooth and flat when cross-linked it will tend to return to a smooth, flat state after
wrinkling or laundering. Likewise if the fabric is creased when cross-linked it will tend to retain
the crease through wear and laundering [30].
2.7.1 History of resin finish
In the mid 1920s, Tootal Broadhurst Lee Co. Ltd. Asked research chemists to make cotton fabric
as wrinkle resistant as silk. It was known that formaldehyde would react with cellulose; however
formaldehyde is not a pleasant material to work with as it irritates mucus membranes, causing
runny noses and watery eyes. The chemists discovered that phenol-formaldehyde condensates
would cross-link cotton and at the same time reduce the formaldehyde risks. Unfortunately, the
phenol-formaldehyde resins severely discolored the cotton fabrics and made it excessively stiff.
Soon thereafter, it was discovered that urea-formaldehyde resins also improved crease recovery
and did so without discoloring the fabric. While not completely free of formaldehyde odor, these
resins could be handled on commercial equipment. From the 1930s until 1961, cotton fabrics
were cross-linked with a number of N-methylol compounds to give wash-and-wear or easy-care
finish on the fabrics [11].
19
2.7.2 Fundamentals of silk finishing with resin
The finish must take into account the following aspects:
l.Silky handle and draping properties of the silk should be retained
2.The right combination and sequence of the finishing machines should be chosen depending on
the silk article
3.The drawbacks of the properties of silk should be rectified and improved by finishing
techniques [12].
2.7.3 Effect of resin
 Flexibility, tensile strength, tear strength and abrasion resistance of the fabric is usually
decreased.
 Swelling in water is inhibited, and the fibers are less absorbent.
 Crosslinking helps to trap dye molecules in the fiber and can thereby enhance the wash
fastness of the dye.
 Resins sometimes cause a color change in dyed fabrics.
 Some dyes are sensitive to durable press resins and may change shade when the finish is
applied.
 Some resins may cause a fishy odor.
 Light fastness may be decreased for using catalyst on durable press finishing.
 Resins may accentuate soil retention by the fabric [34].
2.8 Crosslinking Agents
Resin finishing is carried out with products known as crosslinking agents. These change woven
and knitted fabrics in such a way that the resulting textiles are easier to care for. The first resin-
finishing agents – developed in the 1930s to improve the poor wet strength of viscose staple
fabrics – were compounds of formaldehyde and urea.Since practically all effective resin-
finishing agents are based on formaldehyde, they have Become part of the public debate about
20
the toxicity of this substance. This debate has strongly influenced and stimulated the
development of crosslinking agents in recent years the crosslinking agents that result in the
permanent press finish are often derivatives of urea. A popular agent is DMDHEU,dimethylol
dihydroxy ethylene urea [10].
2.8.1 DMDHEU
This chemical is a low-formaldehyde type of textile resin for "wash and wear" colored and white
fabrics.
Dimethylol dihydroxy ethylene urea (DMDHEU) and modified dimethylol dihydroxy ethylene
urea (modified DMDHEU) are compounds which contain N-methylol and mainly N-alkoxy
methyl groups and they are extensively used in textile industry as durable press finishers.
DMDHEU is a highly effective durable press finishing agent with excellent laundering
durability, little fabric yellowing effects and good fabric hand properties. However, it has
fundamental disadvantages due to formaldehyde-release and severe decrease in fabric
mechanical strength [19]
Structure:𝐂𝟓 𝐇𝟏𝟎 𝐍𝟐 𝐎𝟓
Molecular weight: 178.144 g/mol
The molecular structure of DMDHEU was shown in the Figure 2.4 below-
Figure 2.4: Molecular structure of DMDHEU

21
2.8.2 Effect of DMDHEU on fabric
The effectiveness of DMDHEU is based on its two methylol groups, which releases free
formaldehyde vapor from treated fabrics during industrial production and home treatments such
as laundering and ironing.The ether linkages of DMDHEU gradually hydrolyze to become N-
methylol groups. Consequently free formaldehyde is released continuously during the entire life
of the finished garment.Both textile workers and consumers are subjected to the health risk
caused by formaldehyde vapor released during industrial production and consumer use of
durable press finished garments [21].
2.8.3 Citric Acid
Citric acid is a weak organic acid that has the chemical formula C6H8O7. It occurs naturally
in citrus fruits. In biochemistry, it is an intermediate in the citric acid cycle, which occurs in
the metabolism of all aerobic organisms.
More than a million tons of citric acid are manufactured every year. It is used widely as
an acidifier, as a flavoring and chelating agent [30].
Figure 2.5 : Citric Acid
2.8.4 Citric Acid for crease resistant finishes
Poly carboxylic acids such as citric acid and butane tetra carboxylic acid have been proposed as
cross-linkers for easy care finishes with catalysts such as hypophosphite salts being used to form
ester cross-links.
22
The compounds with three or four carboxyl groups are the most effective crosslinking agents,
and sodium hypophosphite is the best catalyst. Since the prices of the tetra-carboxylic acids, such
as 1,2,3,4,-butanetetracarboxylic acid (BTCA) and cyclo pentane tetra carboxylic acid, are
relatively high, their popularity is limited. It seems reasonable to consider citric acid as a lower
priced substitute to the tetra carboxylic acids. In fact, its price is similar to that of dimethylol
dihydroxy ethylene urea (DMDHEU). Citric acid is currently used for the formaldehyde-free DP
[9].
2.8.5 Effect Of Citric Acid on Silk
The crease recovery increased with the increasing concentration of citric acid due to the increase
in the cross-linkages between the silk polymer molecules. However, when the concentration is
too high, the finish reacts too severely with the fiber and formed a thick layer on the surface of
the fabric. This can reduce the resiliency of the fabric. For the same reason, use of too much
finish reduced the whiteness of the silk fabric [9].
2.9 Catalysts
Catalysts accelerate external and internal cross-links.Many catalysts have been used to cure the
cross-linkers of easy care finishes, but those based on magnesium chloride are most widely used.
Almost any acid or acid salt will catalyze the cross-linking reaction, but many such compounds
are unsuitable because they are too strong, too weak, or present environmental problems [30].
23
2.9.1 Magnesium chloride
Figure 2.6 : Magnesium Chloride
Magnesium chloride is often used alone, but it can be combined with organic acids such as citric
acid, or more acidic salts such as aluminum chloride, to provide “hotter” catalysts which cure the
cross-linkers at lower temperatures or in shorter times than pure magnesium chloride [23].
2.9.2 Sodium Hypophosphite
Figure 2.7: Sodium Hypophosphite
The main role of catalysts as sodium hypophosphite could be related to some acceleration in the
formation of a cyclic anhydride from a poly carboxylic acid [24].
24
2.9.3 Effect of curing temperature and time
At higher curing temperature the increase in stiffness, yellowness and decrease in whiteness
index results with irrespective of the finishing conditions used. This shows that higher
temperature and long curing time are not favorable [23].
2.10 Softener
Softener is an auxiliary that, when applied to textile materials bring about an alteration in the
handle, resulting in the goods being more pleasing to the touch. The more pleasing feel is a
combination of a smooth sensation, characteristic of silk, and of the material being less stiff [15].
With chemical softeners, textiles can achieve an agreeable, soft hand (supple, pliant, sleek and
fluffy), some smoothness, more flexibility and better drape and pliability. Finishing with
softeners can overcome this deficiency and even improve on the original suppleness. Other
properties improved by softeners include the feeling of added fullness, antistatic properties and
sew ability [13].
2.10.1 Types of Softeners
 Anionic
(a) Sulphates
(b) Sulphonates
(c) Sulphosuccinates
 Cationic
(a) Quaternary ammonium salts
(b) Amino-amides
(c) Cyclic cationics (e.g. imidazolines)
25
 Amphoteric
(a) Sulphobetaines
(b) Fatty amino acids
(c) Amine oxides
 Nonionic
(a) Ethoxylates
(b) Esters
(c) Polyethylenes
(d) Silicones
(e) Waxes [11]
2.10.2 Function of Softeners
Softener has the stability to withstand shear forces. Softeners are used for wovens, knit goods
and terry toweling made of cellulosic and synthetic fibers and their blends. Itcan be applied by
Padding, slop padding or exhaust processes (including drum washing units)
2.11 Padding
A padder consists of a trough and a pair of squeeze rolls (mangle). The fabric passes under a
submerged roll in the trough filled with the treatment bath and then through squeeze rolls. The
process is called padding.
Three factors control the amount of solution remaining on the fabric, squeeze pressure (which is
influenced by the composition of the rolls), fabric construction (the solution resides in the
capillary spaces between yarns and fibers), and the absorptive nature of the fiber. All fabrics
have upper and lower wet pick-up limits. Within these limits, adjustments in wet pick-up can be
26
made by increasing or decreasing the squeeze pressure. If the squeeze pressure is too low,
puddles of solution will remain on the surface of the fabric. When this is dried, excess chemical
will deposit in the overly wet areas resulting in non-uniform treatment [15].
It is one of the most familiar technique for use in dyeing, pre-treatment or finishing. It is used for
application of chemicals or even dyes to the fabric in a uniform manner in open width form. The
completion of the reaction or dye fixing is carried out by batching, steaming, curing etc [25].
2.12 Drying
The term drying is commonly used to describe the process of thermally removing the volatile
substances from a product [26]. In textiles, the term is more generally used to mean the
dewatering of a product. Mechanical dewatering is generally much less expensive than thermal
drying. Thus, as much water as possible is usually removed mechanically. Approximately 25%
of the energy used in wet processing is consumed in drying [27].
The drying or dewatering processes can be classified either as pre drying and final drying or as
mechanical and thermal drying. Pre drying is accomplished using either mechanical or thermal
processes whereas final drying is achieved using thermal processes. Pre drying is the lowering of
the moisture regain to some predetermined level.This is followed by the final-drying step in
which the moisture regain is lowered to the desired level.
Considering points for selecting a dryer: Following points should consider during buy a dryer.-
1. Heating methods: The textile fabrics may be heated by gas burner or steam.
2. Chamber: Number of chamber.
3. Burner: Number of burner [28]
27
Different types of dryers are shown in the Figure 2.7 below-
Dryers
Mechanical Conductio Convection Infrared

Dewatering n Dryers Dryers Dryers
Vacuum Hot- Circulatin Through-

Squeezin Centrifug Impingemen
Extractio Cylinder g-Air Air
g e t Dryers
n Drying Dryers Dryers
Figure 2.8: Types of Dryers
2.13 Curing
A process carried out after the application of a finish to a textile fabric in which appropriate
conditions are used to effect a chemical reaction. Usually, the fabric is heat treated for several
minutes. However, it may be subject to higher temperatures for short times (flash curing) or to
low temperatures for longer periods and at higher regain (moist curing) [29].
28
Chapter 3: Materials & Methods
29
3.1 Materials
3.1.1 Fabric
The fabric was collected from Sopura Silk.
Table 3.1: Specification of Fabric
Type Woven Fabric
Ends Per Inch(EPI) 130
Picks Per Inch (PPI) 120
Before degumming Warp Yarn Count (denier) 21.62
Before degumming Weft Yarn Count (denier) 27.02
After degumming Warp Yarn Count (denier) 16.68
After degumming Weft Yarn Count (denier) 21.71
Before degumming G.S.M 24
After degumming G.S.M 21
30
3.2 Pre-Treatment Chemicals
Table 3.2: Specification of Wetting Agent
Particulars Specification
Commercial Name Imerol PCLF
Physical Form Viscous liquid
Solubility Miscible with water in all properties
Manufacturer Acrhroma
Table 3.3: Specification of Sequestering Agent
Commercial Name Sirrix 2UD
Physical Form White liquid
Solubility Miscible with cold water in all properties
Manufacturer Archroma
31
3.3 Finishing Chemicals
Table 3.4: Specification of DMDHEU
Commercial name Fixapret ECO
Chemical nature Modified dimethylol dihydroxy ethylene urea
Physical form Clear, aqueous solution
pH value 4.0 – 5.5
Density 1.3 g/cm3 at 20 °C
Manufacturer Archroma
Table 3.5: Specification of Citric Acid
Formula 𝐂𝟔 𝐇𝟖 𝐎𝟕 .H20
Color White to almost white or colorless
Appearance Crystalline
Odor Odorless
Mass 210.14 g/mol
Melting point 153 °C
Boiling 310 °C
32
Table 3.6: Specification of Magnesium Chloride
Formula MgCl2
Color White
Appearance Crystalline
Melting point: 714 °C
Boiling point 1,412 °C
Molar mass 95.211 g/mol
Table 3.7: Specification of Sodium Hypophosphite
Formula NaPO2H2
Color White
Molar mass 87.98 g/mol
Density 800 kg/m³
Solubility in water Soluble
Melting point 90 °C
Solubility in water Soluble
33
Table 3.8: Specification of Silicone softener
Form Supplied White Dispersion
pH 4-6
Ioncity weakly cationic
Manufacturer BASF
Country of origin Germany
3.4 Experimental Equipments
3.4.1 Padding Machine
Table 3.9: Specification of Padding Mangle
Particulars Specification Figure
Name Horizontal Padding Machine
Company Guangzhou Hongtong Textile

Machinery Co. Ltd.
Brand Name Mathis
Origin China Figure 3.1:Horizontal

Padding machine
34
3.4.2 Stenter Machine
Table 3.10: Specification of Stenter Machine
Name Laboratory Stenter Machine
Company Guangzhou Hongtong Textile

Machinery Co. Ltd.
Brand Name Mathis
Country of Origin China Figure 3.2: Laboratory

Stenter Machine
3.4.3 Electric Weight Balance
Table 3.11: Specification of Electric Precision Balance
Brand A & D weighting
Model Ek 600i
Capacity 600 g
Readability 0.1 g
Figure 3.3: Electric
Weight 1.3 kg /2. Lb Precision Balance
35
3.4.4 Hand Dryer
Table 3.12: Specification of Hand Dryer

Brand Miyako
Model MHD-1200
Origin China
Figure 3.4: Hand Dryer
3.5 Testing Equipments
3.5.1 Spectrophotometer
Table 3.13: Specification of Datacolor SF650 Benchtop Spectrophotometer
Model Data color SF650
Instrument Type Dual-beam spectrophotometer
Geometry d/8° (Viewing angle 8° from the

Abbreviation normal)
Figure 3.5:Spectrophotometer
36
3.5.2 Tearing strength Tester
Table 3.14: Specification of Tearing Strength Tester
Pendulum Capacity 200gf, 400gf, 800gf, 1600gf,

3200 gf, 6400 gf
Gas Source 0.6 Mpa
Tearing Arm 104±1mm
Figure 3.6: Tearing Strength

Tearing Initial Angle 27.5±0.5o
Tester
3.5.3 Crease Recovery Tester
Table 3.15: Specification of Crease Recovery Tester
Loading Device 10N and 19.63N weights
Specimen Tweezers Metal
Specimen Tweezers Plastic

Figure 3.7: Crease Recovery
Specimen Template 50 mm x 25mm Tester
37
3.5.4 Titan Universal Strength Tester
Table 3.16: Specification of Titan Universal Strength Tester
Particular Specification Figure
Name Titan Universal

Strength Tester
Brand Name Titan
Manufacturer James H. Heal
Figure 3.8: Titan Universal Strength

Origin England Tester
38
3.6 Methods
3.6.1 Methodology
Step:1 Determination of Suitable Temperature and Time
Collection of raw silk fabric and all other Chemicals
Degumming of fabric
Treating silk fabric with Resin Treating silk fabric with Citric Acid
(DMDHEU) keeping the concentration keeping the concentration of Citric
of resin & catalyst same Acid and catalyst same
Padding
Drying at 90 C°
Curing carried out at varying Temperature (130,

140, 150, 160, 170)°C and Time (1,2,3 & 4)min
Crease Recovery Angle measurement Whiteness Index
Tensile Strength Test Tearing Strength Test
Analyzing Data
Determination of Suitable Curing Time & Temperature
39
Step:2 Determination of Suitable Concentration of Citric Acid & Resin (DMDHEU)
Treating silk fabric with Resin Treating silk fabric with Citric
(DMDHEU) varying the concentration Acid varying the concentration of
of Resin (DMDHEU) & catalyst Citric Acid and catalyst
Padding
Drying at 90 C°
Curing at previously determined suitable Time & Temperature
Crease Recovery Angle measurement Whiteness Index
Tensile Strength Test Tearing Strength Test
Analyzing Data
Result
40
3.6.2 Recipe for degumming of silk
Table 3.17: Recipe of Degumming
Chemicals Amount
Wetting Agent 1 g/l
Sequestering Agent 1 g/l
Soap 5-8 g/l
pH 10 (adjusted)
Temperature Boiling
Time 90
M:L 1:100
3.6.3 Recipe for resin finish
Table 3.18: Recipe of Resin Finish With DMDHEU & Softener
Chemicals Amount
Resin (Fixarpret) 80 g/l
Catalyst (𝐌𝐠𝐜𝐥𝟐 ) 20 g/l
Silicone softener 20 g/l
41
Table 3.19: Recipe of Resin Finish with Citric Acid and Softener
Chemicals Amount
Citric Acid 70 g/l
Catalyst (Sodium Hypophosphite) 60 g/l
Silicone Softener 30 g/l
Table 3.20: Curing Time and Temperature
Factors Level
Curing Temp (°C) 130 140 150 160 170
Curing Time (Min) 1 2 3 4 1 2 3 4 1 2 3 4 1 2 3 4 1 2 3 4
Table 3.21: Recipe For Resin Finishing with various concentration
Chemicals Concentration of Chemicals (g/l)
Resin (DMDHEU) 60 80 100 120
Magnesium Chloride (Catalyst) 10 20 30 10 20 30 10 20 30 10 20 30
Citric Acid 40 70 100 130
Sodium Hypophosphite (Catalyst) 10 20 30 10 20 30 10 20 30 10 20 30
42
At first,the degummed silk fabric was treated with resin (DMDHEU) and citric acid according to
recipe given on the Table 3.18 and Table 3.19 respectively varying curing time and temperature
on Table 3.20.Here total 40 samples (20 treated with DMDHEU & 20 treated with citric acid)
were treated and analyzing the test results suitable curing time and temperature were fixed. Then
varying the concentration of resin (DMDHEU),citric acid and catalyst given on Table 3.21,
again 24 samples were treated to optimize the concentration of catalyst &finishing agents.
Table 3.22: Others Finishing Parameters
Parameters Unit Amount
Liqour pick up % 95
Drying Temperature °C 100
Drying Time Min 1
Padding Pressure Kpa 0.3
Padding Speed RPM 30
Padding Cycle 2 dip 2 nip
43
3.6.4 Process flowchart for application of resin in silk fabric
Treating the fabric

with DMDHEU &
Citric Acid
Drying in 90°C for

1 min
Curing
Figure 3.9: Process Flowchart For Resin Application
3.7 Testing Methods
3.7.1 Determination of the recovery from creasing of a horizontally folded specimen by

measuring the angle of recovery.
Test Method:ISO 2313-1972
Sample Size:50 mm X 25 mm
Procedure:
1.The specimen is cut by template and carefully creased by folding in half.
2.The crease is imparted on fabric by placing it between two glass plates and adding to 500gm
weight on it.
44
3.After 1 min the weight is removed and the creased side is clamped on the instrument.
4.Then it is allowed to recover from the crease. The recovery time may vary to suit particular
creases. Usually it is 1 min
5.When crease recovers the dial of the instrument is rotated to keep the free edge of the specimen
in line with the knife edge.
6.The recovery angle is read from the engraved scale.
7.In this way 10 tests are done in warp way and 10 for weft way.
8.The mean value of recovery angle is taken and thus crease recovery is measured.
3.7.2 Tear properties of fabrics -- Part 1: Determination of tear force using ballistic
pendulum method (Elmendorf)
Test Method:ISO 13937-1:2000
Sample Preparation:
1. First we take specimen of (100 ×75)mm2
2. The template is placed on the specimen and cut according to the template.
3. A slit is created at the middle point of the specimen, which range is 20 mm.
4. In the test, the Elmendorf continuous to tear the fabric from the end of the slit to the opposite
edge distance of 43mm.
5. Pendulum lever principle is used here
Working Procedure:
1. The apparatus consists of a sector shaped pendulum carrying a moving sample clamp & a
fixed clamp on the frame.
45
2. When the pendulum is in the raised to starting position, the specimen is transferred between
the two clamps.
3. The tear is started by a slit cut in the specimen between the clamps.
4. The pendulum is then released & the specimen is torn as the moving clamp, moving away
from the fixes clamp.
5. The pointer attached to the pendulum, which is graduated to read the tearing force directly.
3.7.3 Breaking Force and Elongation of Textile Fabrics by Grab Method.
Test Method: ASTM D5035
Procedure:
1. The top and bottom jaw was mounted in their position properly. It was ensured that jaws are
firm and tight. Gauge length should be 180 mm.
2. All the fabric sample was extended in a direction parallel to the direction of warp and weft
respectively. Using an indelible fine marker mark to the size of 100 mm X 180 mm.
3. The prepared fabric specimen was secured in suitable jaw.
4. After completion of test the result was shown in the control unit.
5. After the test result were displayed the bottom jaw returned back to its original position.
6. The test for all the warp and weft specimen was repeated.
3.7.4 Determination of Whiteness Index
Test method: AATCC 110-2000
White objects have high reflectance at all wavelengths in the visible region of the
electromagnetic respectively stimulus appear to void of any hue and greyness.
46
Spectrophotometric analysis has proven to be the ideal evaluation technique when assessing the
degree of whiteness and yellowness of materials. Objective measurement and meaningful
numerical expression of the condition has proved technically complex. None of the various
whiteness equations has proved to be superior to others. The CIE expression for a whiteness
index has been available, in the form of the equation given, only since 1982.
𝐖 = 𝐘 + 𝟖𝟎𝟎(𝐱𝐧 − 𝐱) = 𝟏𝟕𝟎𝟎 (𝐲𝐧 − 𝐲)
It represents whiteness in terms of colorimetric values for the sample and the chromaticity
coordinates of the illuminant. Yis the sample’s Y tristimulus value, x and y are its chromaticity
coordinates, and xn and yn the chromaticity coordinates of the illuminant, for either of the
standard observers using illuminant D65,xn and yn are the coordinates of the light source. For D65
illumination, for 10° observer and D65 illumination xn=0.3138, yn=0.3309. The higher value of
W, the greater degree of whiteness is obtained. Generally, W ≥ 65 is acceptable for the
coloration of most shades.
47
Chapter 4: Results and Discussions
48
Table 4.1: Crease Recovery Angle of Silk Fabric after Citric Acid Treatment
Finishing Type Curing Curing Time Crease Recovery

Temperature (°C) (min) Angle(°)
(Warp+Weft)
1 122
2 122
130
3 125
4 125
1 124
2 127
140
3 130
4 139
1 138
2 147
Citric Acid 150
3 152
4 153
1 149
2 156
160
3 150
4 144
1 140
2 139
170
3 133
4 134
Untreated N/A 114
49
180
160
140
Crease Recovery angle
120
100
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Untreated 1 min 2 min 3 min 4 min
Figure 4.1: Crease Recovery Angel of Silk Fabric after Citric Acid Treatment
Discussion:The above bar diagram illustrates that, after treating silk fabric with citric acid
the creased recovery angle increased gradually. With increasing time and temperature crease
recovery angle increased up to 150° and then start to decrease with few exception.
50
Table 4.2: Crease Recovery Angle of Silk Fabric after Resin (DMDHEU) Treatment
Finishing Type Curing Curing Time (min) Crease Recovery

Temperature (°C) Angle (°)
(Warp + Weft)
1 121
2 139
130
3 138
4 130
1 121
2 149
140
3 155
4 157
1 160
2 173
Resin 150
3 177
(DMDHEU) 4 176
1 150
2 147
160
3 146
4 140
1 146
2 139
170
3 144
4 136
Untreated N/A 114
51
200
180
160
Crease REcovery angle
140
120
100
80
60
40
20
0
Untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.2: Crease Recovery Angel of Silk Fabric after Resin (DMDHEU) Treatment
Discussion:Here,Samples treated with Resin (DMDHEU) and Magnesium Chloride where

concentration was fixed but time and temperature was different. The above bar diagram
illustrates that, with increasing time and temperature crease recovery angle increased up to
150° and then start to decrease with few exception.
52
Table: 4.3: Whiteness Index of Silk Fabric after Citric Acid Treatment
Finishing Type Curing Temp (°C) Curing Time (min) Whiteness Index
1 53.46
2 53.30
130
3 50.63
4 48.97
1 52.48
2 51.88
140
3 47.55
4 48.88
1 51.06
Citric Acid 2 51.94
150
3 49.67
4 43.75
1 49.70
2 46.54
160
3 44.01
4 43.28
1 47.05
2 42.10
170
3 41.17
4 40.92
Untreated N/A 53.45
53
60
50
40
Whiteness Index
30
20
10
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.3: Whiteness Index of Silk Fabric after Citric Acid Treatment
Discussion: This diagram illustrates that the whiteness index of after Citric acid and Sodium
Hypophosphite application. Here, we can see, whiteness index decreases with increasing
curing time and temperature. Reduction in whiteness index was higher after 150°C. We
found the lowest whiteness index at the curing temperature of 170° C and at curing time of
4 minute and the highest whiteness index at 130 °C at curing time of 1 minute.
54
Table 4.4: Whiteness Index of Silk Fabric after Resin (DMDHEU) Treatment
Finishing Type Curing Temp (°C) Curing Time (min) Whiteness Index
130 1 52.25
2 49.23
3 49.00
4 48.63
140 1 51.40
2 48.96
3 47.09
4 48.37
150 1 51.08
Resin 2 47.90
3 45.48
(DMDHEU)
4 47.36
160 1 46.11
2 45.95
3 43.14
4 41.32
170 1 46.71
2 44.10
3 39.09
4 38.72
Untreated N/A 53.45
55
60
50
Whiteness Index
40
30
20
10
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.4: Whiteness Index of Silk Fabric after Resin (DMDHEU) Treatment
Discussion: This above bar diagram illustrates the whiteness index of after the application
of Resin (DMDHEU) and Magnesium Chloride. Here, we can see, whiteness index
decreases with increasing curing time and temperature.Reduction in whiteness index was
higher after 150°C. We found the lowest whiteness index was at the temperature of 170° C
and at curing time of 4 minute and the highest whiteness index at 130 °C and at curing time
of 1 minute.
56
Table 4.5: Tear Strength of Silk Fabric after Citric Acid Treatment
Finishing Curing Curing Time Tearing Strength (N) Strength Retention

Type Temp (°C) (min) (%)
Warp Weft Warp Weft
1 4.53 5.64 113 111
2 4.58 5.70 114 112
130
3 5.57 5.72 114 112
4 5.63 5.75 115 113
1 5.59 5.77 114 113
2 5.64 5.81 115 114
140
3 5.63 5.81 115 114
4 5.68 5.86 116 115
1 5.54 5.77 113 113
2 5.59 5.88 114 115
Citric Acid 150
3 5.54 5.88 113 115
4 5.58 5.87 114 115
1 5.58 5.76 114 113
2 5.53 5.80 113 114
160
3 5.52 5.80 113 114
4 5.58 5.89 114 115
1 5.59 5.82 114 114
2 5.54 5.81 113 114
170
3 5.60 5.86 114 115
4 5.64 5.87 115 115
Untreated N/A 4.90 5.09 100 100
57
140
120
Tear Strength Retention (%)
100
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.5: Tear Strength Retention (%) in Warp after Citric Acid Treatment
Discussion: This diagram illustrates that the tear strength retention (%) in warp direction after
citric acid and sodium hypophosphite treatment.Here,we can see that with the increase of curing
time and temperature the tear strength as well as tear strength retention (%) doesnot show any
particular pattern.The tearing strength and its strength retention (%) is almost same for different
time & temperature.
58
140
120
Strength Retention (%)
100
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.6: Tear Strength Retention (%) in Weft after Citric Acid Treatment
Discussion This diagram illustrates that the tear strength retention (%) in weft direction after
citric acid and sodium hypophosphite treatment.Here,we can see that with the increase of curing
time and temperature the tear strength as well as tear strength retention doesnot show any
time & temperature.
59
Table 4.6: Tear Strength of Silk Fabric after Resin (DMDHEU) Treatment
Finishing Type Curing Curing Tear Strength (N) Strength Retention

Temp (°C) Time (%)
(min) Warp Weft Warp Weft
1 5.43 5.85 111 115
2 5.48 5.90 112 116
130
3 5.50 5.90 112 116
4 5.53 5.92 113 116
1 5.53 5.91 113 116
2 5.52 5.94 113 116
140
3 5.58 5.92 114 116
4 5.60 5.95 114 117
1 5.61 5.97 114 117
Resin
2 5.49 6.00 112 118
150
3 5.59 6.01 114 118
(DMDHEU)
4 5.62 6.03 114 118
1 5.48 6.01 112 118
2 5.53 6.00 113 118
160
3 5.52 6.00 113 118
4 5.59 6.05 114 119
1 5.53 5.98 113 117
2 5.59 6.02 114 118
170
3 5.62 6.01 114 118
4 5.65 6.04 115 118
Untreated N/A 4.90 5.09 100 100
60
140
120
Strength Retention (%)
100
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.7: Tear Strength Retention (%) in Warp after Resin (DMDHEU) Treatment
Discussion: This diagram illustrates that the tear strength retention (%) in warp direction after
resin (DMDHEU) and magnesium chloride application.Here,we can see that with the increase of
curing time and temperature the tear strength as well as tear strength retention doesnot show any
time & temperature.
61
140
120
Tear Strength Retention (%)
100
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.8: Tear Strength Retention (%) in Weft after Resin (DMDHEU) Treatment
Discussion:Here,we can see that with the increase of curing time and temperature the tear
strength as well as tear strength retention doesnot show any particular pattern.The tearing
strength and its strength retention (%) is almost same for different time & temperature.
62
Table 4.7: Tensile Strength of Silk Fabric after Citric Acid Treatment
Finishing Type Curing Curing Tensile Strength Retention Percentage

Temp ° C Time (N) (%)
(min)
Warp Weft Warp Weft
1 70.17 72.94 97.40 99.77

2 68.03 72.54 94.43 99.23
130
3 67.35 71.96 93.48 98.44
4 65.22 71.23 90.53 97.87
1 68.88 68.95 95.61 94.32
2 67.58 67.26 93.80 92.01
140
3 65.27 65.23 90.59 89.23
4 64.34 64.89 89.29 88.76
1 68.98 68.21 95.74 93.31
2 67.70 66.88 93.97 91.49
150
3 65.27 64.61 90.59 88.38
Citric Acid 4 63.90 63.14 86.18 86.37
1 67.76 67.56 94.04 92.42
2 66.43 65.36 92.19 89.41
160
3 64.23 63.21 89.14 86.47
4 63.62 61.94 88.29 84.73
1 66.54 65.87 92.35 90.10
2 64.29 64.66 89.22 88.45
170
3 63.45 62.45 88.06 85.43
4 61.63 60.75 85.53 83.10
Untreated 72.05 73.10 100
63
120
100
Tensile Strength Retention (%)
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
1 min 2 min 3 min 4 min
Figure 4.9: Tensile Strength Retention (%) in Warp after Citric Acid Treatment
Discussion: The Tensile strength retention (%) of silk fabric in warp direction after citric acid
treatment is depicted in the graphs. No doubt, there is a substantial strength retention was found
after the treatment. We found approximately strength loss of 15% in warp direction at the highest
temperature.It can be noted that,with increase in time and temperature,the tensile strength as well
as strength retention (%) decreases.
64
120
100
Tensile Retention Percentage(%)
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°C
Temperature
Figure 4.10: Tensile Strength Retention (%) in Weft after Citric Acid Treatment
Discussion: The Tensile strength retention (%) in weft direction after citric acid application is
depicted in the graph. No doubt, there is a substantial strength retention was found after the
treatment. There is a 17 % loss in strength at the highest temperature. With increase in time and
temperature the tensile strength retention (%) decreases.
65
Table 4.8: Tensile Strength Retention (%) of Silk Fabric after Resin (DMDHEU)
Treatment
Finishing Curing Curing Tensile Strength(N) Retention Percentage

Type Temperature Time (%)
(°C) (min) Warp Weft Warp Weft
1 72.01 76.28 99.95 105.80

2 70.13 74.33 97.34 100.03
130
3 69.58 73.15 96.58 101.52
4 71.36 74.23 99.05 103.02
1 70.59 72.99 97.98 101.30
2 68.36 70.26 94.88 97.52
140
3 65.16 68.58 90.44 95.19
4 69.93 69.33 97.06 96.23
1 68.15 68.16 94.59 94.70
2 66.59 66.25 92.43 91.96
Resin 150
3 65.55 65.05 90.98 90.29
4 66.88 67.25 92.83 93.34
1 66.29 69.13 92.01 95.95
2 65.48 65.26 90.89 90.58
160
3 64.15 63.47 89.04 88.10
4 66.59 65.15 92.43 90.43
1 65.47 63.23 90.87 87.76
2 64.21 62.25 89.12 86.40
170
3 62.77 60.38 87.13 83.81
4 64.21 64.29 89.12 89.23
Untreated 72.05 73.10 100 100
66
120
100
Tensile Strength Retention (%)
80
60
40
20
0
untreated 130°C 140°C 150°C 160°C 170°
Temperature
untreated 1 min 2 min 3 min 4 min
Figure 4.11: Tensile Strength Retention (%) in Warp after Resin (DMDHEU) Treatment
Discussion:The Tensile strength retention (%) for 20 silk samples in warp direction after resin
(DMDHEU) treatment is depicted in the graph. Here,good percentage of strength retention was
found after the resin (DMDHEU) treatment.Unlike the citric acid treatment,at highest
temperature the strength loss was merely 12 %.
67
120
100
Tensile Strength Retention(%)
80
60
40
20
0
untreated 130 140 150 160 170
Temperature
Figure 4.12: Tensile Strength Retention (%) in Weft after Resin (DMDHEU) Treatment
Discussion:The Tensile strength retention (%) in weft direction of silk fabric after Resin
(DMDHEU) application is depicted in the graph. Here,the strength retention (%) was much
better than that of citric acid treatment.The strength retention (%) decreases with the increase of
curing time and temperature.
68
Table 4.9: Crease Recovery Angle of Silk Fabric after Citric Acid Treatment at Various
Concentration
Finishing Curing Curing Concentration Crease Recovery

Type Temp. Time
Angle (°)
(°C) (Min) Citric Acid Sodium
(Warp+Weft)
Hypophosphite
(g/l)
(g/l)
40 50 130
40 60 134
40 70 137
70 50 145
70 60 144
Citric acid 150 2
70 70 149
100 50 155
100 60 155
100 70 156
130 50 158
130 60 159
130 70 161
Untreated N/A 114
69
180
160
140
Crease Recovery Angle
120
100
80
60
40
20
0
untreated 40g/l 70g/l 100g/l 130g/l
Concentration of Citric Acid

untreaed catalyst 50g/l catalyst 60g/l catalyst 70g/
Figure 4.13: Crease Recovery Angle of Silk Fabric after Citric Acid Treatment at Various
Concentration
Discussion: From the diagram, we can see that, after treating silk with the Citric Acid and
Sodium Hypophosphite the crease recovery angle increased than the untreated silk fabric.
70
Table 4.10: Crease Recovery Angle of Silk Fabric after Resin (DMDHEU) Treatment at
Various Concentration
Finishing Curing Curing Concentration Crease Recovery

Type Temp. Time Angle (°)
(°C) (Min) ( Warp+Weft)
DMDHEU Magnesium
(g/l) Chloride (g/l)
60 10 162
60 20 163
60 30 164
80 10 173
80 20 175
Resin 150 2
80 30 176
100 10 181
100 20 183
100 30 183
120 10 188
120 20 188
120 30 189
Untreated N/A 114
71
200
180
160
Crease Recovery Angle
140
120
100
80
60
40
20
0
untreated 60 g/l 80g/l 100g/l 120g/l
Concentration of Resin (DMDHEU)
untreated catalyst 10g/l catalyst 20g/l catalyst 30g/
Figure 4.14: Crease Recovery Angle of Silk after Resin Treatment at Various
Concentration
Discussion: From the diagram, we can see that, after treating silk with the resin (DMDHEU) and
Magnesium Chloride the crease recovery angle increased considerably comparing to the
untreated silk fabric. We can also see that, with the increase of concentration the crease recovery
angle increased.
72
Table 4.11: Whiteness Index of Silk after Citric Acid Treatment at Various Concentration
Finishing Curing Curing Time Concentration

Type Temp. (Min)
(°C)
Citric Acid Sodium
Whiteness Index
(g/l) Hypophosphite
(g/l)
40 50 53.34
40 60 52.28
40 70 51.13
70 50 51.19
70 60 48.30
Citric 150 2
70 70 46.89
Acid
100 50 42.68
100 60 41.57
100 70 40.89
130 50 38.49
130 60 37.68
130 70 37.63
Untreated N/A 53.45
73
60
50
Whiteness Index
40
30
20
10
0
Concentration
untreated catalyst 50g/l catalyst 60g.l catalyst 70g/l
Figure 4.15:Whiteness Index of Silk Fabric after Citric Acid Treatment at Various
Concentration
Discussion :From the table and graph it is shown that, as the concentration of Citric Acid and
Sodium Hypophosphite increased the whiteness decreased. Silk fabric samples provided the
lowest whiteness index at a concentration of 130 g/l (Citric Acid) and 70 g/l (Sodium
Hypophosphite).
74
Table 4.12: Whiteness Index of Silk Fabric after Resin (DMDHEU) Treatment at Various
Concentration
Finishing Curing Curing Time Concentration

Type Temp. (Min)
(°C)
DMDHEU Magnesium
Whiteness Index
(g/l) Chloride
(g/l)
60 10 48:35
60 20 46.89
60 30 47.36
80 10 45.97
80 20 45.16
Resin 150 2 80 30 41.38
100 10 37.51
100 20 36.65
100 30 36.19
120 10 35.96
120 20 35.41
120 30 34.21
Untreated N/A 53.45
75
60
50
Whiteness Index
40
30
20
10
0
Concentration
untreaed 10g/l 20g/l 30g/l
Figure 4.16:Whiteness Index of Silk Fabric after Resin (DMDHEU) Treatment at Various
Concentration
Discussion:The above bar diagram shows that, as the concentration of Resin (DMDHEU) and
Magnesium Chloride increased the whiteness index of silk fabric samples decreased.Silk fabric
samples provided the lowest whiteness index at a concentration of 120 g/l (DMDHEU) and 30
g/l (Magnesium Chloride).
76
Table 4.13: Tear Strength Retention (%) of Silk after Citric Acid Treatment at Various
Concentration
Finishing Curing Curing Concentration Tearing Strength

Type Temp. Time Strength (N) Retention (%)
(°C) (Min)
Citric Sodium Warp Weft Warp Weft
Acid Hypophos
(g/l) phite (g/l)
40 50 5.43 5.70 111 112
40 60 5.46 5.80 111 114
40 70 5.45 5.87 111 114
70 50 5.63 5.90 115 116
70 60 5.66 5.93 115 116
Citric 150 2 70 70 5.65 5.95 115 116
Acid 100 50 5.73 6.00 117 118
100 60 5.75 6.10 117 120
100 70 5.83 6.09 119 120
130 50 5.88 6.07 119 120
130 60 5.92 6.04 121 119
130 70 5.90 6.17 121 119
Untreated N/A 4.90 5.09 100 100
77
140
120
Tear Strength Rentention (%)
100
80
60
40
20
0
Concentration of Citric acid
untreated catalyst 50g/l catalyst 60g.l catalyst 70g/l
Figure 4.17: Tear Strength Rentention (%) in Warp after Citric Acid Treatment at
Discussion:The above bar diagram shows that with a gradual increase in the concentration of
both citric acid and sodium hypophosphite the tearing strength retention (%) increases. It can be
observed that,the best tear strength retention (%) in warp direction was found at the highest
concentration of citric acid which was at 130 g/l.
78
140
120
100
80
60
40
20
0
Concentration of Citric acid
untreated catalyst 50g/l catalyst 60g/l catalyst 70g/l
Figure 4.18: Tear Strength Rentention (%) in Weft after Citric Acid Treatment at Various
Concentration
Discussion: The above diagram shows that with a gradual increase in the concentration of both
citric acid and sodium hypophosphite,the tearing strength retention (%) increases. It can be
observed that, the best tear strength (%) in weft direction was found at the highest concentration
of citric acid which was at 130 g/l.
79
Table 4.14: Tear Strength Retention (%) of Silk after Resin (DMDHEU) Treatment at
Finishing Curing Curing Concentration Tearing Strength

Type Temp. Time Strength (N) Retention (%)
(°C) (Min) DMDHEU Magnesi Warp Weft Warp Weft

(g/l) um
Chloride
(g/l)
60 10 5.78 5.95 118 117
60 20 5.83 6.00 119 118
60 30 5.88 6.02 120 118
80 10 5.77 6.15 118 121
80 20 5.78 6.21 118 122
80 30 5.84 6.20 119 122

Resin 150 2
100 10 5.89 6.22 120 122
100 20 5.90 6.21 120 122
100 30 5.92 6.15 121 121
120 10 5.93 6.19 121 122
120 20 5.91 5.70 121 112
120 30 5.93 6.28 121 123
Untreated N/A 4.90 5.09 100 100
80
140
120
100
80
60
40
20
0
untreated catalyst 10g/l catayst 20g/l catalyst 30g/l
Figure 4.19: Tear Strength Retention(%) in Warp after Resin (DMDHEU) Treatment at
resin (DMDHEU) and magnesium chloride the tearing strength retention (%) increases. It can be
observed that, the best tear strength (%) in warp direction was found at the highest concentration
of DMDHEU which was at 120 g/l.
81
140
120
100
80
60
40
20
0
untreaed catalyst 10g/l catayst 20g/l catalyst 30g/l
Figure 4.20: Tear Strength Retention(%) in Weft after Resin Treatment at Various
Concentration
resin (DMDHEU) and magnesium chloride the tearing strength retention (%) increases. It can be
observed that,the best tear strength (%) for weft direction was found at the highest concentration
of DMDHEU which was at 120 g/l
82
Table 4.15: Tensile Strength Test of Silk after Citric Acid Treatment at Various
Concentration
Finishing Curing Curing Concentration Tensile Strength

Type Temp. Time( Strength (N) Retention(%)
(°C) Min)
Citric Sodium Warp Weft Warp Weft
Acid Hypophosphite
(g/l) (g/l)
40 50 66.52 65.93 92.33 90.19
40 60 66.31 66.23 92.03 90.60
40 70 66.45 66.85 92.23 91.45
70 50 65.33 67.10 90.68 91.79
70 60 66.80 67.50 92.72 92.33
Citric 150 2 70 70 67.63 68.56 93.87 93.73
Acid 100 50 68.84 68.88 95.54 94.22
100 60 69.32 67.16 96.21 91.88
100 70 69.85 68.35 96.94 93.51
130 50 67.65 69.56 93.09 95.16
130 60 68.23 72.89 97.06 99.72
130 70 67.56 71.22 93.77 97.43
Untreated N/A 72.05 73.10 100 100
83
120
100
Tensile Strength Rentention (%)
80
60
40
20
0
Concentration of citric acid
Figure 4.21: Tensile Strength Retention (%) in Warp after the Application of Citric Acid
at Various Concentration
Discussion: The Tensile strength retention (%) of silk in warp direction after citric acid
application is depicted in the graph. No doubt, there is a substantial strength retention was found
after the treatment. From the graph and table, we can see that, there is no particular pattern in the
strength retention percentage.
84
120
100
80
60
40
20
0
Concentration of citric acid
untreaed catalyst 50g/l catalyst 60g/l catalyst 70g/l
Figure 4.22: Tensile Strength Retention (%) in Weft after the Application of Citric Acid at
Discussion: The Tensile strength retention (%) of silk in weft direction after citric acid
application is depicted in the graph. As like the warp direction, there is no particular pattern
found in this case also. The highest retention (%) was found at a concentration of 130 g/l.
85
Table 4.16: Tensile Strength of Silk Fabric after Resin (DMDHEU) Treatment at Various
Concentration
Finishing Curing Curing Concentration Tensile Strength

Type Temp Time Strength (N) Retention (%)
(°C) (min)
DMDHEU Magnesi Warp Weft Warp Weft
(g/l) um
Chloride
(g/l)
60 10 63.32 63.19 87.88 86.97
60 20 63.23 64.20 87.75 87.82
60 30 64.65 64.29 89.72 87.94
80 10 65.16 64.65 90.43 88.44
80 20 66.59 63.25 92.13 86.53

Resin 2
80 30 68.10 66.75 94.51 91.31
100 10 66.13 63.34 91.79 86.65
100 20 68.45 67.86 95.01 92.83
100 30 66.97 68.95 92.95 94.32
120 10 69.36 70.56. 96.26 96.52
120 20 64.09 69.06 88.96 94.48
120 30 66.60 67.87 92.44 92.85
Untreated N/A 72.05 73.10 100 100
86
120
100
80
60
40
20
0
untreaed catalyst 10g/l catalyst 20g/l catalyst 30g/l
Figure 4.23: Tensile Strength Retention (%) in Warp after Resin (DMDHEU) Treatment
at Various Concentration
Discussion: The Tensile strength retention (%) in warp and direction after resin (DMDHEU)
treatment is depicted in the graph. From the above bar diagram, we can see that, as the
concentration increased the retention percentage of silk fabric increased up to 80 g/l
concentration. But after that, with more increase in concentration the retention percentage
showed no particular pattern.
87
120
100
80
60
40
20
0
Figure 4.24: Tensile Strength Retention (%) in Weft after the Application of Resin
(DMDHEU) at Various Concentration
Discussion: The Tensile strength retention (%) of silk in weft direction after resin (DMDHEU)
treatment is depicted in the graph. From the graph, we can see that, just like the warp direction,
there is no particular pattern found. The highest retention percentage is found at a concentration
of 120 g/l.
88
Chapter 5: Conclusion
89
5.1 Key Findings
 Citric Acid
 The crease recovery of silk fabric treated with citric acid was improved considerably. The
highest crease recovery angle which was 161° from 114° obtained at the curing
temperature of 150°C and curing time of 2 minutes.
 The Whiteness Index decreased with the increase of curing time and temperature The
lowest whiteness index was found at 170°C and 4 minutes. Whereas with the change of
concentration of citric acid the whiteness index also decreased, the lowest whiteness
index was found for citric acid with the concentration of 130 g/l.
 Tearing Strength did not show any particular trends with the increase of time and
temperature. Almost same tear retention (%) was found for all curing time and
temperature. The change in tear retention (%) was negligible when silk fabric was treated
with different concentration of citric acid and sodium hypophosphite.
 Tensile strength decreased with the increase of curing time and temperature. The lowest
tensile strength retention (%) was found at the curing temperature of 170°C & curing
time of 4 minutes. The strength retention (%) increased with the continuous increase of
concentration of citric acid & the highest tensile strength retention (%) was found for
citric acid at the concentration of 130 g/l.
 Resin (DMDHEU)
 The crease recovery of silk fabric treated with citric acid was improved considerably. The
highest crease recovery angle which was 177° from 114° obtained at the curing
temperature of 150°C and curing time of 2 minutes.With the change in concentration of
resin crease recovery was increased further up to 189° at the concentration of resin
(DMDHEU) which was 120g/l
 The Whiteness Index decreased with the increase of curing time and temperature The
lowest whiteness index was 38.72 which was found at 170°C and 4 minutes.Whereas
90
with the change of concentration of resin (DMDHEU) the whiteness index also
decreased;the lowest whiteness index was found for resin (DMDHEU) with the
concentration of 120 g/l.
 Tearing Strength did not show any particular trends with the increase of time and
temperature. Almost same tear retention (%) was found for all curing time and
temperature. The change in tear retention (%) was negligible when silk fabric was treated
with different concentration of resin (DMDHEU)
 Tensile strength decreased with the increase of curing time and temperature. The lowest
tensile strength retention (%) was found at the curing temperature of 170°C & curing
time of 3 minutes. The strength retention (%) increased with the continuous increase of
concentration of resin & the highest tensile strength retention (%) was found for resin at
the concentration of 120 g/l.
5.2 Limitations
 As crease recovery angle was measured manually there may be a chance of error in the
reading of the data.
 The padding machine in our lab was not working properly during our project work so
there may be a chance difference in pick up ((%) of different silk fabric samples.
5.3 Conclusion
In this study, after treating silk fabric with both formaldehyde based and formaldehyde free
product, we can certainly come to a conclusion that resin (DMDHEU) treated silk fabric which is
a formaldehyde based product, showed better crease recovery angle. Though to improve the
crease recovery angle after treatment was our primary goal, but after considering about the
environment, we decided that, as Citric acid is non hazardous for environment and as it also
showed substantial amount of crease recovery, so it must be our first preference. Furthermore,
we also found a better whiteness index, tensile strength and tear strength in case of resin
(DMDHEU) finish however, it was not too good in comparison to Citric acid that we can pay no
91
attention to the environment. After considering all the facts and analyzing all the results, we
chose the best possible time and temperature and concentration for this treatment which was
150°C, 2 minutes and 100 g/l respectively.
92
References
93
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DEPARTMENT OF TEXTILE ENGINEERING

Course No.: Tex 400

Course Title: Project Work

Academic Semester: Fall 2017

Name of the student Student ID No.

Mizanur Rahman Parvez 14.01.06.004

Tausif Mahmud Siam 14.01.06.044

Md.Faisal Ahmed 14.01.06.097

Md.Arif Anwar 10.02.06.018

Ms.Shaima Islam Ms. Nahida Akter

Assistant Professor Assistant Professor

Ahsanullah University of Science and Technology

Chapter 1: Introduction ......................................................................................................... 1

1.1 Introduction ...................................................................................................................... 2

Chapter-2: Literature Review ................................................................................................ 5

2.1 Silk ................................................................................................................................... 6

2.2.1 The origins ................................................................................................................ 6

2.3 Properties and composition of silk................................................................................... 7

2.3.1 Physical properties of silk ......................................................................................... 8

2.4 Pretreatment of silk ........................................................................................................ 13

2.4.1 Objectives of pretreatment ...................................................................................... 13

2.5.1 Reasons behind crease formation in silk ................................................................. 14

2.6 Finishing ........................................................................................................................ 18

2.6.1 Types of textile finishing ........................................................................................ 18

2.7 Resin finish .................................................................................................................... 19

2.8 Crosslinking Agents ...................................................................................................... 20

2.8.1 DMDHEU ............................................................................................................... 21

2.9 Catalysts ......................................................................................................................... 23

2.9.1 Magnesium chloride ................................................................................................ 24

2.10 Softener ........................................................................................................................ 25

2.10.1 Types of Softeners ................................................................................................ 25

2.11 Padding ........................................................................................................................ 26

Chapter 3: Materials & Methods ......................................................................................... 29

3.1 Materials ........................................................................................................................ 30

3.1.1 Fabric ...................................................................................................................... 30

3.2 Pre-Treatment Chemicals .............................................................................................. 31

3.4.1 Padding Machine .................................................................................................... 34

3.5 Testing Equipments ....................................................................................................... 36

3.5.1 Spectrophotometer .................................................................................................. 36

3.6 Methods ......................................................................................................................... 39

3.6.1 Methodology ........................................................................................................... 39

3.7 Testing Methods ............................................................................................................ 44

3.7.1 Determination of the recovery from creasing of a horizontally folded specimen by

Chapter 4: Results and Discussions...................................................................................... 48

5.1 Key Findings .................................................................................................................. 90

Figure 2.1: The structure of raw silk fibre ............................................................................... 11

Figure 2.2: Mechanical influences on crease resistance and recovery .................................... 17

Figure 2.3: Types of Textile Finishing ................................................................................... 18

Figure 2.4: Molecular structure of DMDHEU ......................................................................... 21

Figure 2.5 : Citric Acid ............................................................................................................ 22

Figure 2.6 : Magnesium Chloride ............................................................................................ 24

Figure 2.7: Sodium Hypophosphite ......................................................................................... 24

Figure 2.8: Types of Dryers .................................................................................................... 28

Figure 3.1:Horizontal Padding machine .................................................................................. 34

Figure 3.2: Laboratory Stenter Machine .................................................................................. 35

Figure 3.3: Electric Precision Balance ..................................................................................... 35

Figure 3.4: Hand Dryer ............................................................................................................ 36

Figure 3.5: Spectrophotometer................................................................................................. 36

Figure 3.6: Tearing Strength Tester ......................................................................................... 37

Figure 3.7: Crease Recovery Tester ......................................................................................... 37

Figure 4.3: Whiteness Index after Citric Acid Application ..................................................... 54

Table 2.1: Physical Properties of Different Type of Silk Fibre ................................................. 9

Table 3.1: Specification of Fabric ............................................................................................ 30

2.2 History of silk