UNIVERSITI TEKNIKAL MALAYSIA MELAKA

This report submitted in accordance with requirement of the Universiti Teknikal

Malaysia Melaka (UTeM) for the Bachelor Degree of Manufacturing Engineering

(Manufacturing Process) (Hons.)

by

MUHAMMAD YAZUAN BIN YAAKUP

B050810104

89080105069

FACULTY OF MANUFACTURING ENGINEERING

2012

PHYSICAL CHARACTERIZATION OF UREA BINDER EXTRUDE AT VARIOUS WEIGHT CONCENTRATION

BORANG PENGESAHAN STATUS LAPORAN PROJEK SARJANA MUDA

TAJUK: Physical Characterization of Urea Binder Extrude at Various Weight Concentrations

SESI PENGAJIAN: 2011/12 Semester 2 Saya MUHAMMAD YAZUAN BIN YAAKUP 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

TERHAD

TIDAK TERHAD

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

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

Alamat Tetap:

BATU 3 ½, KG. KUALA PAH,

71600, KUALA KLAWANG,

JELEBU, N.SEMBILAN

Disahkan oleh:

PENYELIA PSM

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.

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

DECLARATION

I hereby, declared this report entitled “Physical Characterization of Urea Binder

Extrude at Various Weight Concentration” is the results of my own research except as

cited in references.

Signature : ………………………………………….

Author’s Name : Muhammad Yazuan Bin Yaakup

Date : 29 June 2012

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 (Manufacturing Process) (Hons.). The member of the

supervisory committee is as follow:

………………………………...............

i

ABSTRAK

Tujuan kajian ini adalah untuk menentukan peranan sifat-sifat fizikal Urea pengikat

meleler pada pelbagai nisbah kepekatan. Analisis akan dilakukan dengan menggunakan

mesin Pemampatan, Penganalisis Saiz Butir dan Densimeter Elektronik di pelbagai

nisbah kepekatan. Hasil dari ujian pemampatan, analisis saiz butir dan ujian ketumpatan

akan memberitahu kita sifat-sifat fizikal Urea Pengikat. Parameter yang digunakan

dalam kajian ini adalah kepelbagaian nisbah kepekatan Urea Pengikat. Ujian

Pemampatan ini digunakan untuk melihat kekuatan menghancur butir Urea Pengikat.

Analisis saiz butir Urea Pengikat digunakan untuk mencari sama ada terdapat sebarang

butir bahan-bahan mentah yang hilang atau tidak hilang selepas proses penyemperitan.

Daripada analisis saiz butir, ia juga boleh menunjukkan sama ada bahan mentah telah

digabungkan dengan baik atau tidak baik. Keputusan bagi ujian ketumpatan Urea Binder

adalah untuk mencari sama ada terdapat mana-mana yang ketumpatan berbeza yang

terhasil akibat pelbagai nisbah kepekatan Urea Pengikat. Akhirnya data yang diperolehi

akan memberitahu kita hubungkait antara kekuatan menghancur butir Urea Pengikat,

saiz butir Urea Pengikat dan ketumpatan Urea Pengikat untuk memahami lebih lanjut

mengenai proses Butiran baja.

ii

ABSTRACT

The aim of this study is to determine the role on the physical properties of Urea Binder

extrude at various weight concentrations. The analysis will be done using the Compress

machine, Particle Size Analyzer and Electronic Densimeter at various weight

concentrations. The result from compress test, particle size analysis and density test will

tell us the physical properties of Urea binder.The parameters that are used in this study

are concentration of Urea binder. The compress test is used to look the granule crushing

strength of Urea binder. The analysis of particle size is to find whether there is any

particle of raw materials lost or not after extrusion process. From particle size analysis it

also can show either the raw materials had combined and granule well or not. The results

for density test is to find whether there is any different of density occur because of the

various weight concentration of Urea binder. Finally the data obtained will tell us the

correlation between granule crushing strength, particle size and density in order to

understand more about the fertilizer granulation process.

iii

DEDICATION

I especially dedicate this report to my father and my mother.

Without their patience, understanding, support, and most of all love, the completion of

this study would not have been possible.

I also dedicate this report to my friends no matter where they are now.

We have built this tight relationship and being together for many years.

Without all of you, surely I could not all the challenges.

And most special thanks to my supervisor for his advices and guidance.

iv

ACKNOWLEDGEMENT

Firstly I would like to take this chance to thank all lecturer and friend for giving an

advice and support since the beginning of Final Year Project1 until today Final Year

Project 2. A very thankful for my Supervisor, Mr. Mohd Fairuz Bin Dimin @ Mohd.

Amin for giving me much support and guidance in order to complete this project and

report within the given period. He gave me so many ideas and suggestions in order to

perform well along this period.

I also would like to thank all my friends for giving an opinion and helping me in

searching for information and guidelines for my study. I believed that all the knowledge

I got here might be useful later in my career. I would like to convey my appreciation to

all Manufacturing Engineering Faculty Lecturers and staff for being so kind and helpful

along this period of studies. Without all of them, I am nothing and my four years studies

may be useless.

v

TABLE OF CONTENT

Abstrak i

Abstract ii

Dedication iii

Acknowledgement iv

Table of Content v

List of Tables viii

List of Figures ix

List of Abbreviations, Symbols and Nomenclature x

1.0 INTRODUCTION 1

1.1 Background 1

1.2 Problem Statement 2

1.3 Objectives 2

1.4 Scopes 3

2.0 LITERATURE REVIEW 4

2.1 Fertilizer 4

2.2 Urea Fertilizer 5

2.3 Urea Manufacturing Process 6

2.3.1 Synthesis 6

2.3.2 Purification 6

2.3.3 Concentration 7

2.3.4 Granulation Process 7

2.3.4.1 Wet Granulation 8

2.3.4.2 Dry Granulation 8

2.4 The Physical Characteristic of Urea 9

2.4.1 Particle Size 10

vi

2.4.1.1 Effects on Agronomic Response 10

2.4.1.2 Effects on Granulation and Process Performance 11

2.4.1.3 Effects on Storage, Handling, and Application Properties 11

2.4.1.4 Effects on Blending Properties 12

2.4.1.5 Particle Size Analysis 14

2.4.2 Density 14

2.4.2.1 Bulk Density 14

2.4.2.2 Apparent Density 15

2.4.2.3 True Density 15

2.4.3 Granule Hardness 16

2.4.3.1 Crushing Strength 16

2.4.3.2 Abrasion Resistance 17

2.4.3.3 Impact Resistance 18

2.5 The Parameters in Urea 18

2.5.1 Concentration of Urea 18

3.0 METHODOLOGY 20

3.1 Planning of the Study 20

3.2 Flow Chart of Methodology 21

3.3 Machines and Equipment 22

3.3.1 Extruder machine 22

3.3.2 Particle Size Analyzer 24

3.3.3 Electronic Densimeter MD-300S 26

3.3.4 Compression Tester 28

3.4 The Materials 30

3.4.1 Pure Urea (CH4N2O) 30

3.4.2 Soy Bagasse 31

3.4.3 Wheat Flour 32

4.0 RESULT AND DISCUSSION 33

4.1 Results of Experiment 33

vii

4.1.1 Compression Test 35

4.1.2 Density Test 37

4.1.3 Particle Size Analysis 38

4.2 Discussion 41

5.0 CONCLUSIONS AND RECOMMENDATIONS

5.1 Conclusions 44

5.2 Recommendations 45

REFERENCES 46

APPENDICES

A Gantt chart for PSM 1

B Gantt chart for PSM 2

C Parts of Extruder machine

D Parts of Extruder machine

E Parts of Extruder machine

F Parts of Compression tester

viii

LIST OF TABLES

3.1 Sample Ratio by Gram 23

3.2 Sample Ratio by Percentage 23

4.1 Result of Compression test 35

4.2 Result of Density test 36

4.3 The Range size of Soy Bagasse for Particle Size analysis 38

4.4 The Range size of Wheat Flour for Particle Size analysis 39

4.5 The Range size of Urea for Particle Size analysis 40

4.6 The Range size of sample D for Particle Size analysis 41

ix

LIST OF FIGURES

2.1 Schematic representation of Urea synthesis 5

3.1 Flow Chart for Methodology 21

3.2 Extruder machine 22

3.3 Particle Size Analyzer 24

3.4 Flow Chart for Particle Size Analyzer 25

3.5 Electronic Densimeter 26

3.6 Flow Chart for Electronic Densimeter 28

3.7 Compression Tester 28

3.8 Flow Chart for Compression Tester 30

3.9 Pure Urea (CH4N2O) 30

3.10 Soy Bagasse 31

3.11 Wheat Flour 32

4.1 Sample A (Soy Bagasse 50%: Wheat Flour 25%: Urea 25%) 33

4.2 Sample B (Soy Bagasse 25%: Wheat Flour 50%: Urea 25%) 34

4.3 Sample C (Soy Bagasse 25%: Wheat Flour 25%: Urea 50%) 34

4.4 Sample D (Soy Bagasse 33.34%: Wheat Flour 33.34%: Urea 33.34%) 35

4.5 Graph of Compression test 36

4.6 Graph of Density test 37

4.7 Graph of Soy Bagasse for Particle Size analysis 38

4.8 Graph of Wheat Flour for Particle Size analysis 39

4.9 Graph of Urea for Particle Size analysis 40

4.10 Graph of sample D 41

x

LIST OF ABBREVIATIONS, SYMBOLS AND

NOMENCLATURE

C - Carbon

H - Hydrogen

He - Helium

ISO - International Organization for Standardization

K Potassium

MTPD - Mertic Tonne per Day

N - Nitrogen

Ne - Neon

No.exp - Number of experiment

O - Oxygen

P - Phosphorus

QC - Quality control

R - Correlation coefficient

R2 -

The value of coefficient of determination

UPM - Universiti Putra Malaysia

USM - Universiti Sains Malaysia

UTeM - Universiti Teknikal Malaysia Melaka

UTP - Universiti Teknologi Petronas

1

CHAPTER 1 INTRODUCTION

Fertilizer is known as a catalyst or supply the plant nutrient essential to growth the plant.

Typically the term of fertilizer is used to refer to the industry of agriculture that

researches, designs, manufactures, operates, and maintains the growth of the plant on the

earth. Fertilizer is very important in agriculture industry because it also contribute in the

economy of country. These specifications narrowed the manufacturing processes of

fertilizer of Urea.

1.0 Background

OneBaja group that contains four Universities that is UTP, UPM, USM, and UTeM had

been assigned a Project entitle “Next Generation Green and Economical Urea” under

Kementerian Pengajian Tinggi Malaysia. UTeM will be doing research about

“Biodegradable Urea Granules”. Physical characterization of Urea binder extrude at

various weight concentration is one of minor scope that will be review. A single line

urea granulation plants nowadays have reached capacities of more than 3,500 MTPD.

With increasing environmental and health awareness, more and more attention is paid to

the insoluble binder being used in the urea granules and the ammonia emissions from

such plants. These nondegradable binders such as formaldehyde may well be absorbed

by the plant and get into the food cycle. If large amount is consumed and untreated in a

prolong period of time it may cause a detrimental effect to human. The challenge is to

come up with a new biodegradable binder for the urea granulation process with

2

comparable quality and cost against the current available technology. A compound

fertilizer is a complex homogenous product containing two or more of nutrients that has

undergone chemical interaction during the manufacturing process. The chemical

compounding is followed by the process of granulation with the addition of anti caking

agents to form free-flowing compound granules. One of the processes in fertilizer

manufacturing is blending process. In this process, Urea will be blended in various

weight concentrations. The types of the processing parameters are various weight

concentrations. This process is done to combine Urea and binder to produce fertilizer.

From this process, there are some physical properties that being used which are

hardness, particle size and density. This three characteristic are used to see whether there

is changes when Urea binder is blend in various weight concentrations. Besides, the

compress test, particle size analysis and densitometer are the tools that being used to test

the hardness, particle size and density of Urea binder.

1.2 Problem statement

(a) The physical properties of Urea binder extrude at various weight concentrations.

(b) Hence this study, will determine whether there is any changes when the granule

crushing strength, particle size and density against various weight concentrations.

1.3 Objectives

The objectives of this study are:

(a) To determine the physical characterization of Urea binder extrudes at various weight

concentrations.

(b) To deliver the granule crushing strength, particle size and density of Urea binder

using Compression machine, Particle Size Analyzer and Densimeter when extrude at

various weight concentrations.

3

(c) To analyze the correlation between the granule crushing strength, particle size and

density against various weight concentrations whether, if there is any changes in the

physical properties of Urea binder.

1.4 Scope

The aim of this project is to determine the physical characterization of Urea binder

extrudes at various weight concentrations. Parameter that will be used is various weight

concentrations of Urea binder will eventually influence the quality of the product

produced. The Urea binder characteristic which is physical properties will be analyzed

using Compression test, Particle size Analyzer and Densimeter.

4

CHAPTER 2 LITERATURE REVIEW

2.1 Fertilizer

Fertilizers are soil amendments applied to promote plant growth. The main nutrients

added in fertilizer are nitrogen, phosphorus, potassium, and other nutrients are added in

smaller amounts. Collectively, the main nutrients vital to plants by weight are called

macronutrients, including nitrogen, phosphorus, and potassium. Ammonia is main

source of nitrogen. Urea is the main product for making nitrogen available to plant.

Phosphorous is made available in form of super phosphate, Ammonium phosphate.

Potassium Chloride is used for supply of potassium. Synthetic macronutrient fertilizer

can be referred to as artificial or straight, where the product predominantly contains the

three main nutrients. Compound fertilizers are N-P-K fertilizers with other elements

purposely intermixed. Fertilizers are classified according to the content of these three

elements. Labeling is according to relative amounts of each of the three elements by

weight Nitrogen percentage is reported directly, however phosphorus is reported as the

mass fraction of phosphorus pentoxide and potassium is reported as the mass fraction of

potassium oxide (Mayer, 1996).

5

2.2 Urea Fertilizer

Urea (NH2CONH2) is very importance to the agriculture industry as a nitrogen-rich

fertilizer. Ammonia and carbon dioxide are the two elements that are produced Urea in

two equilibrium reactions. The ammonia and carbon dioxide are fed into the reactor at

high pressure and temperature, and the urea is formed in two steps reaction:

2NH3 + CO2 NH2COONH4 (ammonium carbamate)

NH2COONH4 H2O + NH2CONH2 (urea)

Unreacted NH3 and CO2 and ammonium carbamate are the several elements that is

contains in urea. The ammonia and carbon dioxide are recycled as the pressure is

reduced and heat applied the NH2COONH4 decomposes to NH3 and CO2. The urea

solution is then concentrated to give 99.6% w/w molten urea, and granulated for use as

fertiliser and chemical feedstock (Copplestone and Kirk, 1991).

Figure 2.1: Schematic representation of Urea synthesis (Copplestone and Kirk, 1991).

6

2.3 Urea manufacturing process

2.3.1 Synthesis

Ammonium carbamate is form from the reaction of a mixture of compressed CO2 and

ammonia at 240 barg. This is an exothermic reaction, and heat is recovered by a boiler

which produces steam. The first reactor achieves 78% conversion of the carbon dioxide

to urea and the liquid is then purified. The solution from the decomposition and

concentration sections are recycle after second reactor receives gas from the first reactor.

Conversion of carbon dioxide to urea is approximately 60% at a pressure of 50 barg. The

solution is then purified in the same process as was used for the liquid from the first

reactor (Copplestone and Kirk, 1991).

2.3.2 Purification

Water from the urea production reaction and unconsumed reactants (ammonia, carbon

dioxide and ammonium carbamate) are the major impurities in the mixture at this stage.

The unconsumed reactants are removed in three stages. Firstly, the solution is heated

after the pressure is reduced from 240 to 17 barg, which causes the ammonium

carbamate to decompose to ammonia and carbon dioxide:

NH2COONH4 2NH3 + CO2

At the same time, some of the ammonia and carbon dioxide will be flashed off. With

more ammonia and carbon dioxide being lost at each stage, the pressure is then reduced

to 2.0 barg and finally to -0.35 barg,. Then, after the mixture is at the level of -0.35 barg,

the solution of urea dissolved in water and free of other impurities remains. The

unconsumed reactants are absorbed into a water solution which is recycled to the

secondary reactor at each stage. The excess ammonia is purified and used as feedstock to

the primary reactor (Copplestone and Kirk, 1991).

7

2.3.3 Concentration

75% of the urea solution is heated under vacuum, which fade off some of the water and

increase the urea concentration from 68% w/w to 80% w/w. At this stage some urea

crystals also form. The solution is then heated from 80 to 110°C to redissolve these

crystals prior to evaporation. In the evaporation stage molten urea (99% w/w) is

produced at 140°C. The remaining 25% of the 68% w/w urea solution is processed under

vacuum at 135°C in a two series evaporator-separator arrangement (Copplestone and

Kirk, 1991).

2.3.4 Granulation process

Granulation is the process of collecting particles together by creating bonds between

them. Bonds are formed by compression or by using a binding agent called as binder.

The granulation process combines one or more powders and forms a granule that will

allow the tablet process to be predictable and will produce quality tablets within the

required tablet-press speed range. A tablet formulation contains several ingredients, and

the active ingredient is the most important among them. The remaining ingredients are

necessary because a suitable tablet cannot be composed of active ingredients alone. The

tablet may require variations such as additional bulk, improved flow, better

compressibility, flavoring, improved disintegration characteristics, or enhanced

appearance. If the active ingredient in a formulation represents a very small portion of

the overall tablet, then the challenge is to ensure that each tablet has the same amount of

active ingredient. Sometimes, blending the ingredients is not enough. The active

ingredient may segregate from the other ingredients in the blending process. The

ingredients may be incompatible because of particle size, particle density, flow

characteristics, compressibility, and moisture content. These incompatibilities can cause

problems such as segregation during blending or during transfer of the product to the

press as well as separation of the active on the tablet press. Two basic techniques are

8

used to prepare powders for compression into a table that is wet granulation and dry

granulation (Tousey, 2002).

2.3.4.1 Wet Granulation

Wet granulation, the process of adding a liquid solution to powders, is one of the most

common ways to granulate. The process can be very simple or very complex depending

on the characteristics of the powders, the final objective of tablet making and the

equipment that is available. Some powders require the addition of only small amounts of

a liquid solution to form granules. The liquid solution can be either aqueous based or

solvent based. Aqueous solutions have the advantage of being safer to deal with than

solvents. Although some granulation processes require only water, many actives are not

compatible with water. Water mixed into the powders can form bonds between powder

particles that are strong enough to lock them together. However, once the water dries,

the powders may fall apart. Therefore, water may not be strong enough to create and

hold a bond. In such instances, a liquid solution that includes a binder (pharmaceutical

glue) is required. The existing binder that had been use in Urea NPK is Formaldehyde

(Tousey, 2002).

2.3.4.2 Dry Granulation

The dry granulation process is used to form granules without using a liquid solution

because the product to be granulated may be sensitive to moisture and heat. Forming

granules without moisture requires compacting and densification the powders. Dry

granulation equipment offers a wide range of pressures and roll types to attain proper

densification. This equipment is loud and dusty compared with other process machinery.

Material feed rates are critical for attaining the final objective. The process may require

repeated compaction steps to attain the proper granular end point. Typically, a

percentage of products does not get compacted and may require screening to remove

9

excessive fines. Again, successful compaction depends on the compatibility of the

products being compressed. If fines are not removed or reprocessed, then the batch may

contain too many of them, a situation that can contribute to capping, laminating, weight,

and hardness problems on the tablet press. The need for screening large amounts of fines

is common to roller compaction, and the degree to which it can be managed depends on

the nature of the ingredients. Any product that is removed from the rest of the batch

because of particle size must be analyzed to determine what is being removed (Tousey,

2002).

2.4 The Physical Characteristic Of Urea

Sastry and Fuerstenau (1973) detailed the mechanisms for granule growth (granulation)

which included: nucleation; growth; random coalescence; pseudo-layering, and crushing

and layering. Litster and Liu (1989) in their studies on the granulation of fertilizer have

found that coalescence is the most probable mechanism for low-temperature fertilizer

granulation using a feed with a broad particle size distribution. To establish an

understanding of the fundamental mechanisms of granule formation, the forces involved

in the collision of two spherical particles were investigated by a number of researchers.

The capillary and viscous contributions were both found to significantly affect the

bonding mechanism of colliding particles and were correlated using the viscous number.

The regime map theory of Iveson and Litster (1998) postulates that the type of granule

growth behavior is a function of the amount of granule deformation during collision and

the maximum pore saturation. The amount of granule deformation has been

characterized by Tardos et al. (1998) as a Stokes deformation number. The maximum

pore saturation and the Stokes deformation number characterize the growth regime in

which granulation takes place. The exact boundary between the regimes depends on the

type of granulation equipment and properties of the binder such as viscosity. Miyazaki et

al. (1998) had stated that in order to obtain solid granules, it is important to pay

sufficient attention to the viscosity of the solvent and surface tension.

10

2.4.1 Particle Size

Particle size distribution of Urea fertilizer products or Urea raw materials is defined as

the particle diameter range of the material. Particle size analysis is typically measured by

sieving, a process of separating a mixture of particles according to their size fraction.

Particle size affects agronomic response, granulation and process performance, and

blending, storage, handling, and application properties. Some of the reasons for size

control follow (Hoffmeister, 1979).

2.4.1.1 Effects on Agronomic Response

Hoffmeister (1979) had stated that fertilizer of very low water solubility generally must

be ground to small particle size to ensure sufficiently rapid dissolution in the soil and

utilization by plants. For example, the effectiveness of raw phosphate rock generally

increases with fine grinding down to a particle diameter of about 150 μm; below that,

little further benefit has been established. Other materials of low solubility that require

relatively fine grinding include basic slag, limestone, dolomite, dicalcium phosphate,

and fused phosphates. Micronutrient or secondary nutrient sources of low solubility,

such as sulfur, metallic oxides, and glasses, likewise require fine grinding. The fine

grinding required for these materials often results in undesirable dustiness and other

handling difficulties. Therefore, some research and development has been directed

toward retranslating the pulverized materials. For example, in the United States, there

are currently a few small commercial limestone granulation plants. Method of dust

control other than granulation includes spraying the pulverized materials lightly with oil,

water, or amine formulations. Others fertilizer that benefit agronomical from particle

size control is some of the sparsely soluble slow release nitrogen fertilizers such as urea

formaldehyde, isobutylidene diurea, and oxamide. The rate of dissolution and hence the

rate of nitrogen availability from these materials, has been shown to be dependent on

particle size; the larger the particles, the slower the release.