Thermal Absorption Properties Of Spent Tea Leaf Filled Polyurethane Composite Material.

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

THERMAL ABSORPTION PROPERTIES OF SPENT TEA LEAF FILLED
POLYURETHANE COMPOSITE MATERIAL

This report submitted in accordance with requirement of the Universiti Teknikal
Malaysia Melaka (UTeM) for the Bachelor Degree of Manufacturing Engineering
(Engineering Materials) (Hons.)

by

SITI AISYAH BINTI SAFUAN
B051010180
890425-10-5092

FACULTY OF MANUFACTURING ENGINEERING
2013

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

BORANG PENGESAHAN STATUS LAPORAN PROJEK SARJANA MUDA

TAJUK: Thermal Absorption Properties of Spent Tea leaf filled Polyurethane
Composite Material
SESI PENGAJIAN: 2011/12 Semester 2
Saya SITI AISYAH BINTI SAFUAN
mengaku membenarkan Laporan PSM ini disimpan di Perpustakaan Universiti
Teknikal Malaysia Melaka (UTeM) dengan syarat-syarat kegunaan seperti berikut:
1. Laporan PSM adalah hak milik Universiti Teknikal Malaysia Melaka dan penulis.
2. Perpustakaan Universiti Teknikal Malaysia Melaka dibenarkan membuat salinan
untuk tujuan pengajian sahaja dengan izin penulis.
3. Perpustakaan dibenarkan membuat salinan laporan PSM ini sebagai bahan
pertukaran antara institusi pengajian tinggi.
4. **Sila tandakan (√)

SULIT

(Mengandungi maklumat yang berdarjah keselamatan
atau kepentingan Malaysiasebagaimana yang termaktub
dalam AKTA RAHSIA RASMI 1972)

TERHAD


(Mengandungi maklumat TERHAD yang telah ditentukan
oleh organisasi/badan di mana penyelidikan dijalankan)

TIDAK TERHAD
Disahkan oleh:

Alamat Tetap:

Cop Rasmi:

No. 7 Jalan Joran Satu,
19/24 A, Seksyen 19
40300, Shah Alam, Selangor
Tarikh: _________________________

Tarikh: _______________________

** Jika Laporan PSM ini SULIT atau TERHAD, sila lampirkan surat daripada pihak berkuasa/organisasi
berkenaan dengan menyatakan sekali sebab dan tempoh laporan PSM ini perlu dikelaskan sebagai

SULIT atau TERHAD.

APPROVAL

This report is submitted to the Faculty of Manufacturing Engineering of
UTeM as a partial fulfillment of the requirements for the degree of Bachelor
of Manufacturing Engineering (Engineering Materials) (Hons.). The members
of the supervisory committee are as follow:

………………………………
(Principal Supervisor)

………………………………
(Co-Supervisor)

ABSTRAK

Pemuliharaan tenaga merupakan isu semakin serius bagi sektor kediaman pada masa
kini. Oleh itu, prestasi termal bahan sistem penebat haba untuk bangunan semakin
bertambah kebelakangan ini. Laporan ini dibuat untuk menganalisis kebolehan bahan

polimer komposit menyerap haba dengan mancampurkan pelbagai jenis gred dan
komposisi gentian dalam polimer komposit. Tujuan kajian ini dijalankan adalah untuk
mencirikan dan menyiasat pelbagai jenis gred gentian dari segi sifat fizikal, kimia dan
termal termasuklah ketumpatan gentian, hubungan kimia gentian, dan juga perubahan
fasa gentian serta kadar pengaliran haba pada berlainan suhu (50,70,90,110°C). Terdapat
tiga jenis gred gentian iaitu BM-FAE dan SW-BHE daripada batang daun pokok teh
serta Fiber-FAE daripada daun teh. Polimer komposit (PU/STL) telah dibentuk melalui
proses kisar dan ‘open molding’ dengan komposisi gentian 5,10,15 dan 20%. Keputusan
menunjukan gentian BM-FAE adalah gentian yang kurang tumpat dengan ketumpatan
1.441g/cm3disebabkan dari pada bahagian batang daun. Kehadiran komposisi lignin juga
hadir dalam lingkugan 1650cm-1 ke 1380 cm-1 melalui FTIR. Untuk suhu perubahan
fasa, suhunya berada diantara 70°C ke 80°C. Bagi kadar pengaliran haba pula, PU/BMFAE komposit menunjukkan kadar pengaliran haba rendah jika dibandingkan dengan
gentian yang lain disebabkan kanduangan liang yang ada dalam gentian tersebut.
Daripada kajian ini, dapat dilihat bahawa dengan penambahan gentian, kadar pengaliran
haba rendah bagi komposit (PU/STL). Dapat dilihat juga bahawa melebihi suhu
perubahan fasa, kadar pengaliran haba meningkat disebabkan berlakunya perubahan fasa
polyurethane.

i


ABSTRACT

Energy conservation is an increasingly important issue in the residential sector.
Therefore, attention towards the thermal performance of building materials, particularly
thermal insulation systems for building has grown in recent years. This report describes
the thermal absorption behavior of polyurethane composites reinforced with different
grades of spent tea leaves (STL) fibers at various fibers loading. The objectives of this
study were to characterize the spent tea leave fibers in terms of its physical, chemical,
and thermal properties as well as the rate of heat transfer of the spent tea leaves filled
polyurethane (PU/STL) composite at various temperatures (i.e. 50, 70. 90, and 110°C).
There were three grades of STL fibers, which are BM-FAE and SW-BHE obtained from
the stalk while Fiber-FAE extracted from the leave of a tea plant. The PU/STL
composite was fabricated via granulation and open molding with fiber loading ranging
from 5, 10, 15, and 20% wt%. Results showed that BM-FAE has the lowest density,
1.441g/cm3 as it comes from the stalk. These three grades of fiber have showed the
presence of lignin at the wavenumber range between 1650 cm-1 and 1380 cm-1 from
FTIR. For the glass transition temperature (Tg) of fibers, the value was in between 70°C
and 80°C. In terms of thermal absorption behavior, it was observed that at temperature
70°C (Tg of composite), PU/BM-FAE composite showed lower heat absorption than
other composites due to the porous media in fiber. It was also perceived that the addition

of fiber loading reduced the heat absorption of the composite. Above the Tg of
composite (90 and 110°C), the rate of heat transfer becomes higher due to the phase
change of the polyurethane.

ii

DEDICATION

To my beloved family and my siblings

iii

ACKNOWLEDGEMENT

Completion of this project report was made possible because of numerous supports and
helps given to me when I was working on it. Thus, it is a great pleasure for me to write
this special acknowledgement to every single individual that helped and inspired me to
finish this project. I would like to express my highest gratitude to all of them.
First and foremost, I would like to express my thankfulness and appreciation to my
supervisor, Miss Chang Siang Yee, for her supervision, guidance, understanding and

patience throughout this research work. Also, I would like to thank her for her precious
time. Special thanks also goes to my co-supervisor, Prof. Dr. Qumrul Ahsan, for his
support and encouragement. All valuable information provided by him is much
appreciated. Not to forget to other lecturers, friends and lab technicians for sharing their
experiences, skills, opinions, advises and guidance in handling the equipments
throughout the study.
Lastly, my sincere appreciation is dedicated to my parents for their love, encouragement
and continuous support particularly when I am having difficulties.

iv

TABLE OF CONTENT

Abstrak

i

Abstract

ii


Dedication

iii

Acknowledgement

iv

Table of Content

v

List of Tables

x

List of Figures

xii


List of Abbreviations, Symbols, and Nomenclatures

xv

CHAPTER 1: INTRODUCTION

1

1.1

Background Study

1

1.2

Problem Statement

3


1.3

Objectives

3

1.4

Scopes

4

CHAPTER 2: LITERATURE REVIEW

5

2.1

Introduction


5

2.1.1

Thermal Insulation

5

2.1.2

Properties and Performance of Insulating Materials

6
v

2.1.3
2.2

2.3

2.4

Commercial Thermal Insulation Materials

8

Thermal Insulation of Synthetic Materials

10

2.2.1

Fiberglass

10

2.2.2

Expanded Polystyrene (EPS)

10

2.2.3

Rock wool

11

2.2.4

Polyurethane (PU)

12

2.2.4.1 Isocyanate

13

2.2.4.2 Polyol

14

2.2.4.3 Blowing Agent

14

Thermal Insulation of Composite Materials

15

2.3.1

Composite

15

2.3.2

Synthetic Fiber-Reinforced Composite

15

2.3.3

Natural Fiber-reinforced Composite

17

2.3.4

Tea Leaves Composite

23

Effect of Fiber-Loading on Composite Materials

26

2.4.1

Physical Properties

26

2.4.2

Thermal Properties

27

2.4.2.1 Influence of the cell gas

27

2.4.2.2 Influence of density

27

2.4.2.3 Influence of temperature

28

2.4.2.4 Influence of water absorption after immersion in water

28

vi

CHAPTER 3: REEARCH METHODOLOGY

29

3.1

Raw Materials

29

3.1.1

Polyurethane (PU)

29

3.1.2

Spent Tea Leaves

31

3.2

3.3

3.4

Characterization of Raw Materials

32

3.2.1

Digital Imaging Microscopy

32

3.2.2

Scanning Electron Microscope (SEM)

33

3.2.3

Fourier Transform Infrared Spectroscopy (FTIR)

34

3.2.4

Density Measurement

35

3.2.5

Differential Scanning Calorimetry (DSC)

36

3.2.6

Thermogravimetry Analysis

36

Fabrication of Spent Tea Leaves Filled Polyurethane Composite

37

3.3.1

Preparation of Spent Tea Leaves

37

3.3.2

Fabrication of Spent Tea Leaves Filled Polyurethane Composite

38

3.3.3

Sample Preparation

39

Sample Characterization

40

3.4.1

Density Measurement

40

3.4.2

Water Absorption

40

3.4.3

Differential Scanning Calorimetry (DSC)

41

vii

3.5

Sample testing

42

3.5.1

42

Thermal Test Measurement

3.6

Microscopic Observation

43

3.7

Flow Chart of methodology

44

CHAPTER 4: RESULTS AND DISCUSSION

45

4.1

Characterization of Raw Material

45

4.1.1

Digital Imaging Microscopy (DIM)

45

4.1.2

Particle Size Analyzer (PSA)

47

4.1.3

Density Measurement

48

4.1.4

Fourier Transform Infrared Spectroscopy (FTIR)

50

4.1.5

Differential Scanning Calorimetry (DSC)

53

4.1.6

Thermogravimetry Analysis (TGA)

55

4.1.7

Scanning Electron Microscopy (SEM)

56

4.2

Characterization of Composite

58

4.2.1

Physical Properties

58

4.2.1.1 Density Measurement

58

4.2.1.2 Water Absorption

59

Thermal Properties

65

4.2.2.1 Differential Scanning Calorimetry (DSC)

65

4.2.2

viii

4.3

Testing
4.3.1

66
Thermal Test

66

CHAPTER 5: CONCLUSION AND FUTURE WORK

70

5.1

Conclusion

70

5.2

Future Work

72

REFERENCES

73

APPENDICES
A

Gantt Charts

ix

LIST OF TABLES

2.1

Properties and performance of insulating materials (Pasanen et al., 2000)

2.2

Density and thermal conductivity of expanded polystyrene
(Yucel et al., 2009)

2.3

7

11

Density and thermal conductivity result of different type of rock wool
(Itewi, 2011)

12

2.4

Different types of polyurethane foams (Polymer Foams Handbook, 2010)

13

2.5

Thermal conductivity of the polyester resin and fiber glass percent and hardness
(Almtori et al., 2010)

2.6

Advantages

16

and disadvantages of using natural fiber in composites

(Pickering, 2008)

18

2.7

Effect of density on different properties (Luamkanchanaphan et al., 2012)

19

2.8

Thermal conductivity of various materials (Luamkanchanaphan et al.,2012)

19

2.9

Thermal conductivity of banana/sisal composites (Indicula et al., 2006)

20

3.1

Physical and chemical properties of Polyurethane (KNT Edge, Malaysia)

30

3.2

Nomenclature and compositions of PU/STL composite

39

x

4.1

Measurement of STL fibers for BM-FAE, SW-BHE and Fiber-FAE

46

4.2

Density of STL fibers; BM-FAE, SW-BHE and Fiber-FAE.

49

4.3

Table 4.3: FTIR Adsorption Bands Typical of Celluign Materials.
Adapted from: Camposo et al. (2013)

51

xi

LIST OF FIGURES

2.1

Classification of the most used insulating materials (Papadopoulus, 2004)

8

2.2

Density of PU/coir at different fiber wt% (Azmi et al., 2005)

20

2.3

Maximum force of PU/coir panel at different fiber wt%
(Azmi et al., 2005)

21

2.4

Shear stress of PU/coir panel at different fiber wt% (Azmi et al., 2005)

21

2.5

(a) Untreated coir fiber surface at 75x magnification; (b) Treated coir
fiber surface at 75x magnification and (c) Treated coir fiber surface
at 200x magnification (Azmi et al., 2005)

22

2.6

Composition of tea leaves (O-CHA, 2010)

24

2.7

DTA-TG curves of the PWT material (Demir, 2006).

25

3.1

Polyurethane (PU)

30

3.2

The three grades of STL obtained from BOH Sdn Bhd, Cameron
Highland, Pahang, Malaysia: (a) BM-FAE, (b) SW-BHE, (c) Fiber-FAE

31

3.3

Digital Imaging Microscopy (MeijiTechno, Japan)

32

3.4

SEM machine (INCAX-sight, U.K)

33

3.5

Pulverization (Pulverisette 14, Germany)

34

3.6

FTIR spectrometer (Perkin Elmer Precisely Spectrum 100, U.S.A)

35

3.7

Gas pycnometer (InstruQuest, United States)

35
xii

3.8

Drying oven (Memmert, Germany)

37

3.9

Process fabrication of the composite

38

3.10

Non-standard procedure for thermal testing

42

4.1

Particle size result for BM-FAE, SW-BHE and Fiber-FAE fiber.

47

4.2

FTIR Spectrums of Spent Tea-Leaf Fibers with BM-FAE, SW-BHE,
and FIBER-FAE

50

4.3

Phase changes from solid to glass transition temperature of STL Fibers

53

4.4

Degradation temperature for STL fibers; Fiber-FAE by TGA

55

4.5

Measured PU/STL composite density at different types of fiber
and loading

4.6

Effect of fiber type for same fiber loading: (a) 5%, (b) 10%, (c) 15%,
(d) 20%

4.7

61

Effect of fiber loading for same fiber type: (a) BM-FAE, (b) SW-BHE,
(c) Fiber-FAE

4.8

58

63

Colour water after water absorption test for Fiber-FAE:
(a) Pure polyurethane, (b) 5% of fiber, (c) 10% of fiber, (d) 15% of fiber,
(e) 20% of fiber

4.9

Phase change from solid to glass transition temperature of PU100 and
PU/BM-FAE-20 composite

4.10

64

65

Figure 4.10: The rate of thermal gradient for different fiber
loading at test temperature of 50, 70, 90 and 110°C:
(a) PU/BM-FAE, (b) PU/SW-BHE, (c) PU/Fiber-FAE

67

xiii

4.11

5.1

The rate of thermal gradient for different type of fiber at test temperature
of 50, 70, 90 and 110°C: (a) 5% fiber loading, (b) 20% fiber loading

68

Sandwich structure of PU/STL composite

72

xiv

LIST OF ABBREVIATIONS, SYMBOLS, AND
NOMENCLATURE

BM

-

Broken mat

CFC

-

Chlorofluorocarbon

CO

-

Carbon oxide

CO2

-

Carbon dioxide

DSC

-

Differential Scanning Calorimetry

EPS

-

Expanded Polystyrene

FTIR

-

Fourier Transform Infrared

HC

-

Hydrocarbon

HCFC

-

Hydrochloroflourocarbon

HCN

-

Hydrogen cyanide

HFC

-

Fycroflourocarbon

HRR

-

Heat release rate

iPP

-

Isotactic polypropylene

KBr

-

Potassium Bromide

MDI

-

Di-phenyl methane di-isocyanate

NaOH

-

Sodium Hydroxide

NFC

-

Natural Fiber Composite

NO

-

Nitrogen oxide
xv

OH

-

Hydroxyl group

PALF/LDPE

-

Pine apple leaf fiber/Low density polyethylene

PE

-

Polyethylene

pMDI

-

Polymeric by product

PP/OMMT

-

Polypropylene/organophilic montmorillonite

PSMA

-

Polystyrene maleic anhydride

PU100

-

Pure PU

PU

-

Polyurethane

PU/BM-FAE

-

BM-FAE type of fiber filled polyurethane composite

PU/SW-BHE

-

SW-BHE type of fiber filled polyurethane composite

PU/Fiber-FAE

-

Fiber-FAE type of fiber filled polyurethane composite

PU/STL

-

Spent tea leaves filled polyurethane

SE

-

Secondary electron

SEM

-

Scanning Electron Microscope

STL

-

Spent tea leaves

SW

-

Sweeping

TDI

-

Tolune di-isocyanate

TGA

-

Thermogravimetric analysis

TI

-

Thermal insulation

WTL

-

Waste tea leaves

WTLB

-

Waste tea leaves particleboard

xvi

°C

-

degree Celcius

g

-

gram

g/cm3

-

gram per centimeter cube

g/ml

-

gram per milliliter

µm

-

micrometer

%

-

percent

λ

-

Thermal conductivity, k-value

wt%

-

weight percentage

K

-

Kelvin

l

-

length

mm

-

millimeter

nm

-

nanometer

rpm

-

revolution per minute

Tg

-

Glass transition temperature

t

-

thickness

W/mK

-

Watt per meter Kelvin

W

-

Watt

w

-

width

xvii

CHAPTER 1
INTRODUCTION

1.1

Background of study

As global warming has become a major concern for human beings nowadays, the use of
thermal insulation (TI) structure in building construction is burgeoning. TI structure is
regarded as one of the most energy efficiency improvements in buildings and also an
important factor to achieve thermal comfort for building occupants. In fact, the thermal
insulation structure is not an independent energy production or conservation system, but
part of the complex structural elements which form a building’s shell. Commercial TI
structures are commonly made from synthetic materials such as fiberglass, mineral wool,
expanded polystyrene (EPS) and polyurethane (PU) foams. Although these materials
have good physical properties such as low thermal conductivity, good moisture
protection and fire resistance, they can be hazardous to human health and environment
(Demant, et al. 1994). Fiberglass has an adverse effect on human health. When
fiberglass is handled, cut or otherwise disturbed, people may be exposed to airborne
fiber and resulted in skin and eye irritation or emphysema and lung cancer through
inhalation
The hazard of using commercially available TI materials made of synthetic materials has
spurred interest in other renewable green materials as alternative. Over the years, several
researches have succeeded in developing TI materials using lignocellulosic fibers.
Various lignocellulosic fibers that have been investigated as raw materials for TI
1

purpose are coconut husk (Viswanathan et al. 2000; Van Dam et al. 2004), kenaf core
(Xu et al. 2004), cotton (Alma et al. 2005), bagasse (Widyorini et al. 2005), oil palm
(Feng et al. 2001; Khalil et al. 2007; Suradi et al.2010)1, flax and hemp (Kymalainen
and Sjoberg, 2008), wood, (Kawasaki and Kawai, 2006; Azizi and Faezipour, 2006;
Akgul et al. 2007; Loh et al. 2010), coffee husk and hulls (Bekalo and Reinhardt, 2010),
and papyrus (Tangjuank, 2011). Among these fibers, fiberboard fabricated from papyrus
fiber reinforced natural rubber latex showed the most promising result with thermal
conductivity values of 0.029 W/mK. This is comparable to commercially available
insulating concrete foams made of EPS which shows a thermal conductivity values of
0.033 W/mK.). Despite the low thermal conductivity behavior, lignocellulosic fibers
also outweigh other commercial synthetic thermal insulation materials in the regard of
density. The density of natural fiber is 1.15 – 1.50 g/cm3 whereas 2.4 g/cm3 for
fiberglass. Research shows that decreasing of the density of TI materials reduced the
thermal conductivity value (Luamkanchanaphan et al., 2012)
It is undeniable that natural fibrous materials exhibit numerous advantages to be
functioned as TI material. A tropical country like Malaysia is rich in the production of
crops such as coconut, pineapple, banana, palm oil, and rice. Tea leaves (Camellia
Sinensis) is one of the fibrous plants available in abundance which can be found at
Cameron Highlands, Pahang and Ranau, Sabah. Therefore, this study attempts to
investigate on the feasibility of incorporating spent tea leaves (STL) as an alternative
lignocellulosic material to produce TI materials.

2

1.2

Problem Statement

Natural fibers have shown to possess low thermal conductivity and density which is
advantageous for thermal insulation purpose. However, when dealing with these natural
fibers, an undesirable attribute of the fiber is their ability to absorb moisture from the
atmosphere in comparatively large quantity (Chawla, 1998). Upon moisture absorption,
most of these fibers swell and become prone to microbial attack as well as biological
decay. In most buildings, the building materials are exposed to moisture due to high
humidity due in the weather or the use of the air-conditioning system. The presence of
moisture encourages the growth of moss or algae which may disfigure and deteriorate
the properties of the building materials made of natural fibers. Spent tea leaves obtained
from tea producing factories are optimistically considered as a new resource because it
exhibits antimicrobial properties. Spent tea leaves are expected to show higher durability
in thermal insulation applications than other natural fibers owing to the high phenolic
extractive content which retards the growth of moss or algae. Hence, spent tea leaves
serve a scope for further research as thermal barrier component.

1.3

Objectives

The objectives of this project were as follows:
1. To characterize various grade of spent tea leaves extracted from different parts of
tea plant in terms of physical, chemical and thermal properties.
2. To fabricate thermal insulation board using various grades of spent tea leaves
filled polyurethane composite through open molding technique.
3. To investigate physical and thermal properties of spent tea leaves filled
polyurethane composite.
3