SWELLING BEHAVIOR OF NATURAL RUBBER VULCANIZATE FILLED WITH CARBONIZED GROUNDNUT HUSK AND CARBON BLACK

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    SWELLING BEHAVIOR OF NATURAL RUBBER VULCANIZATE FILLED WITH

    CARBONIZED GROUNDNUT HUSK AND CARBON BLACK

    BY

    ELETA KATE WILLIAMS

    MATRIC NO AST/2161208034

    SUBMITTED TO THE DE ARTMENT OF OLYMER TECHNOLOGY

    SCHOOL OF A LIED SCIENCE AND TECHNOLOGY AUCHI OLYTECHIC!AUCHI!

    EDO STATE

    IN ARTIAL FULFILLMENT OF THE RE"UIREMENTS FOR THE AWARD OF

    HIGHER NATIONAL DI LOMA #HND$ IN OLYMER TECHNOLOGY

    S%&'%()%* 2014

    i

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    CERTIFICATION

    This is to certify that this project work on swelling behavior of natural rubber (NR) vulcanizate

    filled with carbonized groundnut husk was performed and written by ELETA KATE

    WILLIAMS of department of polymer technology of higher national diploma (HN )

    certificate

    !!!!!!!!!!!!!!!!!!!!!! !!!!!!!!!!!!!!!!!!

    DR MRS F+A+ AK A "T#

    ($R%'T $#R*+%R)

    !!!!!!!!!!!!!!!!!!!!!! !!!!!!!!!!!!!!!!!!!

    MRS UGBESIA! S+O "T#

    $R%'T '%,%R +N"T%R

    !!!!!!!!!!!!!!!!!!!!!!! !!!!!!!!!!!!!!!!!!!!

    MR IDIAGHE , +A "T#

    (H#" %- #$"RT.#NT)

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    ii

    # +'"T+%N

    This project wok is dedicated to /od most high whose divine grace is unspeakable to my

    success in life0

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    iii

    ACKNOWLEDGEMENT

    The long year dream is now a reality my first gratitude go to my lord /od almighty 1 for his

    guidance1 protection 1 substance 1 provision and all for giving me divine health1 wisdom1

    knowledge and understanding favor1 encouragement throughout the course of study0

    .y thank also goes to my supervisor D* M*-+ F+ A +O AK A 0 .y profound gratitude goes to

    M*+ E.%) % L +O for his full support throughout my project and for his contribution during

    the course of my study0 "lso my gratitude to #ngr "2% " " for his support1 .R FESTUS

    INEGBEDION 0 .y thank also goes to MR IKHIDE his for help and assistance ! MR

    MOMOH F+ ! .y thanks also goes to all the staff of polymer technology department that

    influence and contribute to my academic success0 .ost especially MR EKEBAFE +L +O .ay

    /od enriches you with your heart desires0 "men

    .y gratitude goes to the head of the department MR IDIAGHE , +A 0

    "m ever indebted to my mother MRS ANTHIANS +O+ for her support1 spiritually1 prayerfully1

    financially1 love and care + pray the 3ord enlarge her coast0 "lso MR WILSON ONORIADE

    and MR MIKE IRALE for their support for the success for my academic work0

    -inally1 + appreciate and acknowledge the presence of /od in my life4 spirit1 soul1 and body

    for give me favors ability and enablement to pass through the program successfully0 + also

    acknowledge the assistance of all my course mate 567585679 scission0

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    ABSTRACT

    This research work is aimed at studying the swelling behavior of natural Rubber (N0R)vulcanizates filled with groundnut husk carbon and carbon black respectively0 #ight formulationtables were drawn1 four containing carbon black and four containing carbonized groundnut husk at different loading capacity0 The vulcanizates were prepared based on the formulations0 Theswelling behavior vulcanizates were studied using the solvents: petrol1 diesel1 kerosene1 andwater to determine the swelling inde; at 766ml of each of the solvent0 The essence of the test isto determine the stability of the vulcanizates to attack by these solvents and other material alike1which the vulcanizates may come in contact with in every day application0 -rom the resultobtained1 it was observed that vulcanizates with low filler loading have very high swellinginde; obviously due to low interaction between the filler and the polymer matri; leading to verylow cross link density0

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    5076 .ain effect of filler characteristics on vulcanizate properties 7B

    5077 source of filler 7B

    5075 Rubber 'ompounding +ngredients 56

    CHA TER THREE>06 materials and method 59

    >07 material and sources 59

    >05 .ethod 5?

    >0> preparation of carbonized groundnut husk powder as filler 5?

    >09 characterizations of the fillers ('D >>6 and '/NH) 5?

    >0@ compounding of N0R at varying filler loading 5B>0A modification of formulation >6

    >0B stages of processing >6

    >0C molding and vulcanization >7

    CHA TER FOUR

    906 Result >>

    907 test >>

    CHA TER FIVE

    ?06 iscussion1 'onclusion and recommendation >B

    ?07 iscussion >A

    ?05 'onclusion >C

    ?0> recommendation >C

    REFERENCE

    vii

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    CHA TER ONE

    1+0 INTRODUCTION

    .any people have tried to use various agricultural by,products as fillers in compounding0

    These fillers are either use raw or modified0 +n this work1 the carbonized groundnut shell are

    compare with carbon =black to see the comparative study of thermal stability of compounded

    rubber0 The rapid increase in the range of manufactured products following world war (5) two

    resulted directly from the development of broad range of new fibers1 plastic elastomers1

    adhesive1 and resins0 These new material are polymers and their impact on our way of life is

    almost incalculable Eallcock and lampe7CC6F0 The demand for polymers in many applications

    has e;perience a steady growth over the years0 +n developed countries of #urope and "merica1

    the volume of polymer used is more than that of metals or ceramics E"kpa566?F0 Rubber1 being

    a major form of polymers has not been left out0 Rubber in its raw state have virtually no

    engineering application1 it is necessary to appropriately compound them in order to obtain good

    processing characteristics1 and the desire cure properties in the finished products Ecatchy 5666F0

    +t is not surprising1 therefore that more than ?6G of all chemist and chemical engineers1 large

    numbers of physicist and mechanical engineers and nearly all materials scientists and te;tile

    technologist are involved with research or development work with polymers0

    7

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    Rubber as one of the classes of polymers have found great valued in many application including

    engineering1 sport and leisure and domestic0 +n its raw state1 rubber may not be good enough for

    any useful application1 so there is the need for the addition of additives which help to enhance

    the properties0 "mong the additives are filler0 'arbon black is the major filler used in rubber

    industry0 Today there are lots of research going on to find an alternative (local source) for it0

    "dvances are being made into the use of other agricultural by,products1 such as rice husk1

    groundnut shell1 rubber seed shell1 etcEDryson 7C??F0 These materials are used in their raw form

    or they are modified before used0

    1+1 UR OSE/OB,ECTIVE OF STUDY

    1+ $reparation of carbonized groundnut husk2+ 'haracterization of carbonized groundnut husk3+ The use of carbonize groundnut husk to compound natural rubber 4+ The determination of the swelling properties of the vulcanizate

    The purpose of this study is to study the swelling behavior of the carbonized groundnut

    shell and carbon black filled natural rubber compounds

    1+2 STATEMENT OF ROBLEM

    "part from the base polymer1 fillers are the ne;t material in terms of volume that is

    re uired in the rubber industry0

    5

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    The most commonly use fillers include carbon black1 china clay1 calcium carbonate1 etc

    of all these fillers1 carbon black is the one that is mostly used for rubber products e;pect where

    colour is of priority0

    This carbon black is mostly imported which make it to be e;pensive due to our weak

    naira and secondly1 it is from petroleum a source which is non,renewable and between the ne;t

    7? years coming it may get e;hausted0 There is the need to sort for alternate material from local

    material with little modification0

    1+3 SIGNIFICANCE OF THE STUDY

    The significance of this study is to assess the swelling behavior of natural rubber vulcanizate

    filled with carbonized groundnut husk as to provide an alternative to carbon black by using

    locally sourced fillers0

    1+4 SCO E OF STUDY

    This work is limited to swelling behavior of natural rubber vulcanizate filled with carbon black

    and carbonized groundnut husk in solvents

    >

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    CHA TER TWO

    2+0 LITERATURE REVIEW

    2+1 NATURAL RUBBER

    IRubberJ also I+ndia RubberJ redirect here for other uses0 Rubber is generally classified

    as natural and synthetic rubber a gummy substance1 isolated from the white fluid of rubber trees

    with minor impurities of other organic compounds plus water forms of poly,isoprene that are

    useful as natural rubber are classified as elastomeric0 Rubber is harvested mainly in the form of

    late; from certain trees0 The late; is a sticky1 milky colloid drawn off by making incision into

    the bark add collecting the fluid in vessels in a process called ItappingJ0 The late; then is

    refined into rubber1 rubber ready for commercial processing0 Natural rubber is used e;tensively

    in many application and products1 either alone or in combination with other materials0 +n most

    of its useful forms1 it has a large stretch ratio1 high resilience1 and is e;tremely water proof (9)0

    NR is hydrocarbon with empirical formula (' ?HB) n where n is C?1666 to 761?660 The

    (' ?HB) is gutta,percha in contrast to natural rubber however1 gutta,percha is hard and very

    brittle at home temperature and this noticeable difference is attributed to the structural

    arrangement about the double bonds in the two (' ?HB) +somers0

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    CH3

    CH2 = C - CH = n( Isoprene) ( Poly-isoprene

    2+2 SOURCES OF NATURAL RUBBER

    ometimes called ($ara rubber) is the tree Hevea brasiliensis0 The only other place under

    cultivation as a commercial rubber source is guayule (parthenium argentatum)1 shrub native to

    the arid region of .e;ico and the < nited tates0

    2+3 METHOD OF RODUCING NATURAL RUBBER

    +n the collection of natural rubber late;1 the hevea brasiliensis tree wounded by cutting

    the late; vessel in the bank1 by a controlled operation called T"$$+N/0 The most common

    tapping method used is the half spiral system1 from left to right way around the tree trunk at an

    angle of >6 o to the horizontal0

    ?

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    Tapping is achieved with a special curved knife (tapping knife) which flow along the

    groove to the end of the cut where spout conduct it to a collecting cup attached to the tree0 The

    cup may contain a preservative such as "mmonia (NH>) to prevent the late; from coagulating

    at the late; receiving station0 The late; is strained through a sieve to remove coagulum and bark

    particle as well as dirt0 The late; is then transferred to the main factory for onward preparation

    to dry rubber0

    2+4 ROCESSING OF NATURAL RUBBER

    Natural rubber is coagulated late; from certain types of rubber tree e0g0 hevea brasiliensis

    and manufactured in a factory0 Rubber got its name when #nglish scientist &oseph $riestly

    observed that it could KLruboutLL pencil marks (source: R.")0

    Rubber is a polymer1 which is a chain of monomers or small molecules0 Natural rubber

    has only monomers of isoprene0 C1 0 0 inventor 'harles /ood year

    determined that heating rubber with surfer resulted in a stronger product that was more stable

    over a wide range of temperatures0 He called this process vulcanization and further discovered

    that he could uicken the process by adding other substances0 *ulcanization strengthens rubber

    into a stronger matri;0 Natural rubber is processed by first taking the sap from a cut in the tree1

    ne;t1 processors flatten it into sheets0

    @

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    To make the sheets workers blend1 late; from various sources and sometime mi; with water and

    coagulants0 Then the late; is passed through grooved rollers to produce sheets of rubber that are

    allowed to dry0 %n small rubber plantations1 these sheets are visually inspected4 they are tested

    technically in large operations0 "fter imperfections are removed1 the sheets are baled together

    with talc in between to keep them from sticking to each other0 Dlock rubber goes through the

    same initial stages1 but is chopped up and pressed into bales (source: "'T" )0

    ynthetics rubber is made by mi;ing two by = product of petroleum fining1 butadiene and

    styrene0 They are mi;ed with soapsuds to make li uid late;1 which as then dried into bits and

    passed into bales0 "bout A6 percent of all rubber is synthetic0 The industry can vary the

    chemical formula of synthetic rubber to adapt it to different applications (source: R.")

    2+ RO ERTIES / A LICATION OF NATURAL RUBBER

    Rubber e;hibits uni ue physical and chemical properties0 RubberLs stress strain behavior

    e;hibits the .ullins effect and the $ayne effect1 and is often modeled as hyper,elastic0

    Rubber strain crystallizers

    %wing to the presence of a double bond in each repeat unit1 Natural rubber is susceptible to

    vulcanization and sensitive to ozone cracking0

    A

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    The two main solvents for rubber are turpentine and naphtha (petroleum)0 The former has been

    in use since 7C@9 when /iovanni -ibroins is credited with the discovery of naphtha as a rubber

    solvent in 7AAC0

    Decause rubber does not dissolve easily1 the material is finely divided by shredding prior to its

    immersion0

    "n ammonia solution can be used to prevent the coagulation of raw late; while it is being

    transported from its collection site0

    2+6 FILLERS

    These are usually solid additives that are incorporated into polymer to modify its physical

    (mechanical) properties0 -illers help to increase modulus and hardness and to reduce creep and

    most time to reduce the cost of end product0 +t also help in electrical in solution and heat

    deformation resistance0 They are powdered or short fibred materials such as wood flow1 glassfibred1 silicon and silicates0 'a'o51 .g'o5 as be stores e0t0c0 others may be rein,enforcing e0g0

    carbon black and also groundnut shell0 $lastics that are used as structural engineering materials

    contained rein,enforcing agent and a more recently use rein,enforcing agent is graphic fibred

    which is a common additive used in application call for a proved mechanical properties (5)

    B

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    2+ CHARACTERISTIC OF FILLER

    The interaction of particular filler with an elastomeric is dependent on a number of

    factors0

    Namely:

    70 +ntensity50 #;tensity>0 /eometrical1+ INTENSITY

    The intensify factor is the specific activity of this solid surface per s uare centimeter

    interface1 determined by the physical chemical nature of the filler surface and to some e;tent

    that of the elastomers (>)

    50 T % E TENSITY FACTOR is the total amount surface area of the filler per cubic

    centimeter compound in contact with that elastomer03+ GEOMETRICAL FACTOR (a) The surface of the filler1 which can be determined by it empty (void) volume under

    standardized packing conditions0

    C

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    (b) The porosity of filler usually a minor factor which can varied over a wide range with

    carbon black because the weight of the individual spongy particles is lower than those of the

    solid particles0 The number of particles sizes per cubic centimeter of

    'ompound at a given weight loading is greater for spongy particle than the solid particle (>)

    2+8 USES OF FILLERS

    -iller are used in various forms for various $urposes0 Defore the application of fillers1

    much consideration such as cost1 process ability1 compatibility and ability to withstand adverse

    condition must be evaluated for better product property0 -iller cannot be used to the best

    advantage in polymer unless there is a good adhesion between them0 +n particular1 the filler

    particle polymer interface will not be stress bearing and therefore provides a point of

    mechanical weakness1 fillers can be used to achieve the following effect0

    + COST REDUCTION

    'ertain filler can be applied to reduce cost in opa ue $0*0' 'ompounds for mi;ing and

    processing0 #;amples of filler used are coconut shell1 wood flour1 rice husk1 groundnut shell0 +n

    other words filler are used as cheapeners for products0

    76

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    )+ HARDNESS AND MODULUS

    The hardness of a material gives a measure of the modulus at low strain and usually

    e;pressed in +0R0H0 particulate fillers play an important role in the hardness and modulus of a

    vulcanisate0 /enerally fillers especially reinforcing fillers increase the modulus and hardness of

    a *ulcanisate0

    5+ STRENGTH

    -illers are useful in impacting the product property of strength when incorporated into

    polymers such as NR1 DR1 low gum strength polymer re uire fine particle size carbon black

    and silicaLs give the highest Mstrength for rubber especially when they are well dispersed0

    + ABRASION AND TEAR RESISTANCE

    -illers are used in areas where resistance to abrasion and tear are desired1 as the

    resistance to abrasion increases with optimum resistance occurring in the region of ?%phr1 non,

    black filler can also give this effect0

    %+ ELECTRICAL RO ERTIES

    -illers can be used to improve electrical insulation properties clay and carbon blacks1

    are e;ample of fillers applicable for this purpose0

    77

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    + DEFORMATION RESISTANCE

    -illers are also used to improve heat deformation resistance of cables in its manufacture

    to lengthen its service life0

    7+ BRITTLENESS

    The incorporation of filler such as glass fibred1 wood flour in high impact polystyrene

    can help to reduce brittleness in the compound0

    + MACHINE ABILITY

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    TY ES OF FILLER

    These are the three main types of fillers1 these include:

    7) $articulate filler 5) Ruinous filler >) -ibrous filler

    ARTICULATE FILLER

    $articulate filler are divided into reinforcing filler and inert fillers0 The inert filler may affect

    the physical properties when incorporate into a polymer0 e0g0 the addition of inert filler onto

    plasticized $*' compound will reduce die swell on e;tension1 increase modules and hardness1

    improve electrical insulation properties and reduces tackiness0 +nert fillers will also usually

    reduce the cost of a compound to greater e;tent0 "mong the filler used such filler should be

    insoluble in any li uid with which the polymer compound is liable in contact0 'hemicals type of

    filler is available in a numbers of grades and differs in the following ways:

    (7) $article shape and porosity

    (5) "verage particle size and size of the surface

    (>) 'hemical nature of the surface

    (9) +mpunities

    7>

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    +t has been observed that when employed in the elastomeric system the finer the particles size1

    the higher the value of such properties as tensile strength modules1 and hardness0 They can

    function in a number of ways in a polymer matri;0

    (7) +mprove where an abrasion characteristics of the matri;

    (5) +ncrease the heat deformation temperature of the matri;

    (>) Reduce solvent and gas permeability in the matri;

    (9) +ncreasing lubrication properties of the matri;

    (?) #lectrical insulation properties (reduces)

    (@) *iscosity increase

    (A) pecific gravity increase

    (B) Transparency (decrease)

    RESINGEOUS FILLER

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    The resinous have a further advantage1 testing of the rubber compound is little affected0 There is

    e ually little or no heart build up the case with the particle filler as loading is increased0

    The resinous filler commonly used are1

    tyrene,butadiene (?68?6 resin)

    $henolic phenol formaldehyde resin0

    FIBROUS FILLER

    There are generally fibers of cotton rayon1 wood1 carbon asbestos etc0 the fiber used have a

    higher modulus than resin in which they are embedded so that when the composite of resin

    fiber is stained +n the place of the fibrous layer1 the bulk of the stress is taken out by the fiber0

    REINFORCING FILLER

    /enerally1 reinforcing filler re those additions which increase the tensile strength1 tear strength1

    modulus1 hardness and abrasion resistance of rubber compound vulcanization in which are

    incorporated0

    7?

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    NON BLACK REINFORCING FILLER

    However for light color product meeting specification was very tasking as the non black filler

    up to 7C9? were non reinforcing1 hence1 it become imperative than non black filler use for light

    color goods give more reinforcing properties in other to be used in non,self reinforcing

    elastomers such DR1 NDR1 #$ .0

    The e;perience as resulted in the development of non black filler for the production of rubber

    article with improved physical properties such as

    +ncreasing hardness1 tensile1 strength1 tear strength and operation resistance0

    The following constitute some of the non black reinforcing filler presently in use in the rubber

    industry are silica1 zinc o;ide natural silica1 hydrated precipitated silica1 Hydrated aluminum

    hydro;ide etc0

    NON BLACK NON REINFORCING FILLER

    These are the inner material (dilutes) mainly used reduce compounding cost and cheapen or

    e;tend the material0 #;ample include

    BARITES9

    "n inner material used to reduce cost: it is an attractive candidate for chemical resistance

    compound for tank lining0

    7@

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    TALCUM #TALC FRENCE CHALK$

    .ica powder naturally washed and grounded to about 566,>660 ue to its lamellar structure

    can substantially reduce gas permeation and also impact good resistance to heart0 This consists

    mainly of silicate of magnesium and aluminum used as inert filler in heat resistance compound

    for gasket battery cases and auto clawing joints0 Talc is now mostly used as a dusting agent to

    prevent uncured stock from sticking to themselves and other surfaces0

    NON BLACK SEMI REINFORCING FILLER

    ome of these include:

    TREATED WHITINGS

    These are precipitate 'a'o >0The particle of which has been coasted with >G of a serrate0 They

    are uite valuable materials to fill gap between non reinforcing whiting at one hand and

    reinforcing silicon on the other hand0

    "s semi , reinforcing filler1 giving product of moderate cost goods appearances with fairly

    high resistance and tears strength0 They are used in the high grade colour mechanical goods0

    %thers include a timony trio;ide ma;imum flame resistance and precipitated whiting at high

    loading0

    7A

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    %thers include wood flour1 asbestos which are naturally occurring siliceous fibers both the

    shorter fibers and the grounded material as filler for flame (0heat resistance material) like gasket

    and shoe0

    FILER FROM ORGANIC MATERIAL

    #;ample of filler source from organic material are phenolics resins1 doka nut shell1 rice husk

    etc0 the source doka shell is dried and grounded to a fine powder1 sieve to particles size between

    A?,7?6mm0 others includes coconut fiber1 mango shaft etc0

    ERSITENT STRUCTURE

    "n increase in persistence structure (omisionery) results in lower e;trusion shrinkage1

    higher modulus at low and medium strain up to >66G1 higher viscosity1 higher hysteresis and

    longer incorporation time0 Higher electrical conductivity is found for higher structure blacks0

    This property is interrelated with surface activity0 tructure changes on filler without surfaceactivity (graphitized black)1 showing the effects indicated above only rather faulty at constant

    high activity0 The structural effects are pronounced0

    OROSITY

    $orosity results in higher viscosity and higher electrical conductivity in the case of

    carbon black0

    7C

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    2+12 RUBBER COM OUNDING INGREDIENTS

    The manufacture of rubber products re uired the addition of many different types of

    chemical compounds and materials to the rubber0 These additional materials are called

    compounding ingredients or rubber additives0 'ompounding therefore is the operation of

    bringing together all the ingredients re uired to mi; a batch of rubber compound0 They are

    often added to facilitate processing1 improve the properties of the rubber and reduce cost0 The

    rubber in its raw state is not suitable for use in any given application0 Rubber is1 for e;ample1

    visco,elastic in nature0 They have a tendency towards both plastic and elastic behaviorsL0 This

    tendency gives rise to IcreepJ which is adverse to engineering and other application0 Rubbers

    are also very sensitive to changes in temperature0 They e;hibit thermo plasticity within a limited

    range of temperature most rubbers are soluble in a wide range of organic solvents0 These factors

    impose severe limitations on the usefulness of the rubber material for a particular application

    the base polymer or blend has to be selected according to the final properties re uired0 ome of

    the compounding ingredients are:

    I+ RUBBER

    Raw rubber1 whether it is the natural hydrocarbon or synthetic1 in the dry or late; form1 is

    compound with various other materials to change it from a soft plastic material to a strong1 non,

    plastic and even hard ubstance0 " blend of two rubbers may also be used in the rubber

    compound formulation0

    56

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    ii0VULCANIZING AGENT

    *ulcanization is a chemical process1 which brings about the formation of cross,links

    between the long polymer chains0 The three,dimensional structure produced restricts the free

    mobility of the molecules and gives products having reducing tendency to crystallize improved

    elasticity and substantially increased modulus and hardness0 The original and more commonly

    used vulcanizing agents are organic pero;ides such as dicumyl pero;ide and benzyl pero;ides1

    metal o;ide such as zinc o;ide and magnesium o;ide0

    $oly,functional amines are used in the vulcanization of fluorocarbon rubber0 The process

    of sulphur vulcanization is only possible if raw rubber has double bond or unsaturation in its

    molecules0 -or saturated rubbers1 a small amount of unsaturation is usually introduced to make

    it sulphur *ulcanizable0

    :::+ ACCELERATORS

    "ccelerators are compounding ingredients used to speed up the rate of cure1 they are

    added to reduce cure time to an economic level e;amples are biphenyl,guanidine ( $/)1

    mercaptobenzothiazole (.DT) Oinc diethyl dithiocarbonate (O ')0

    :;+ ACTIVATOR

    "ctivators are compounding ingredients which activate the accelerator and make them

    more soluble and efficient during vulcanization0

    57

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    They consist of organic activator (zinc o;ide) and organic activator (stearic acid)0 The

    zinc o;ide is soluble in the stearates which act as a vehicle0 These increase cross link density

    but do not speed up the rate of cure0

    ;+ ANTIDEGRADANTS

    "nti,degradant is a general term used to describe materials added to rubber which retard

    deteriorates of rubber product during service life0 ouble bond although vital for sulphur

    vulcanization of rubber provides the weak link as far as degradation by o;ygen and ozone is

    concerned0 Rubber containing high amount of unsaturation such as NR1 DR1 are more prone to

    %;idative degradation or attack by ozone than elastomer containing low amount of unsaturation

    such as #$ .0 The groups of protective agents used in the rubber industry fall into:

    70 "mines and their derivatives e0g0

    a0 $henyl P ", napthylamine ($"N)

    b0 $henyl P D, naphitonlamine ($DN)

    c0 N1 iso, propyl N,phenyl1 $,phenylene diamine (+$$ )0

    50 $henol and their derivative e0g0 Dis (5 P hydro;yl P >, t,buty7 P ? methyl phenyl)

    methane0

    55

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    ;:+ LASTICIZER

    These are materials used in rubber to facilitate the mi;ing and processing of rubber

    compounds0 They act as4 lubricants during processing operation and accelerate the plasticization

    of the raw rubber0 These materials include resins1 mineral and vegetable oils1 wa;es and organic

    peptizing agent: $lasticizers must be compatible with the rubber so as to function effectively

    into the compound0

    5>CHA TER THREE

    3+0 MATERIALS AND METHOD

    3+1 MATERIAL AND SOURCES

    8N% ."T#R+"3 % R'#

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    a muffle furnace0 The carbonize groundnut husks were grinded pass through a metal sieves in

    order of 7?6 micro (um) with a shaker1 the fine powder particle for the carbonize groundnut

    husks that passes through the sieves were collected and characterized before used for

    compounding and also with carbon black in order to compared the swelling behavior with

    different solvent

    3+4 CHARACTERIZATION OF THE FILLER

    -iller are characterized in terms of $ H1 Dulk density determination1 +odine adsorption1 loss on

    ignition0

    &H D%'%*(:< ':=<The pH of the carbonized groundnut husk ('/NH) samples were

    etermined using " T. 7?75 method1 7CB> by immersing 706g samples in ?606ml of

    5?

    deionised water in a 5?6ml beaker0 The mi;ture stirred for 7?minutes and both the filler andwas heated for 5?minutes and added to cool before adding another ?6ml of deionizer water

    making it 766ml and was stirred of ?minutes0The pH meter was inserted on both the filler todetermine the reading and values were read0 Transfer the results to the chapter for results and

    discussion -or carbon black

    A0C5pH

    -or carbonized groundnut husk

    B077$hASH CONTENT

    The weight of the crucible were noted before the test sample were filled to the crucible and

    were place inside the oven at a temperature of 966 o c for hours0 "t the e;piration of the time1

    the crucible (moisture cans) were removed from the oven and place into a dissector to before it

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    was re,weighed and the valves were noted for both carbon black and carbonized groundnut

    husk filler0

    B>?. D% at 75? S '0 This method was used to

    determine the percentage of water in a sample by drying the sample to a constant weight0 The

    water content is e;pressed as the percentage1 by weight1 of the dry sample0 The moisture sample

    was determined by weighing the rubber seed shell and record as Iwet weight of sampleJ4 the

    wet sample was dried to a constant weight1 at a temperature not e;ceeding 77?S' using suitable

    http://en.wikipedia.org/wiki/Analytical_chemistryhttp://en.wikipedia.org/wiki/Mineralhttp://en.wikipedia.org/wiki/Ignitionhttp://en.wikipedia.org/wiki/Cruciblehttp://en.wikipedia.org/wiki/Mufflehttp://en.wikipedia.org/wiki/Mineralhttp://en.wikipedia.org/wiki/Ignitionhttp://en.wikipedia.org/wiki/Cruciblehttp://en.wikipedia.org/wiki/Mufflehttp://en.wikipedia.org/wiki/Analytical_chemistry

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    drying e uipment (drying oven)0 The sample was allowed to cool and then weighed again1 and

    recorded as the Idry weight of sampleJ

    'alculation

    The moisture content of the sample is calculated using the following e uation:

    G< " , D U766 ,,,,,,,,,,,,,,,,,,,,,,,,, 5

    !!!!!

    "

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    tearic acid ? ? ? ?Oinc o;ide >0? >0? >0? >0?T.T 70? 70? 70? 70?.DT > > > >$rocessing oil ? ? ? ?T.Q 70? 70? 70? 70?

    -iller('D)N>

    >%

    56 >6 96 ?6

    ulphur >0? >0? >0? >0?

    5B

    -ormulation used for compounding N0R ingredient of carbonized groundnut husk0 '/NH

    $$HR

    +N/R# +#N

    T

    " D '

    Natural rubber 766 766 766 766tearic acid ? ? ? ?

    Oinc o;ide >0? >0? >0? >0?T.T 70? 70? 70? 70?.DT > > > >

    processing oil ? ? ? ?T.Q 70? 70? 70? 70?-iller('/NH) 56 >6 96 ?6

    ulphur >0? >0? >0? >0?

    3+6 COM OUNDING OF NATURAL RUBBER AT VARYING FILLER LOADING+

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    The design of the formulation for the compounding is shown in table above0 The fillers used

    were varied with different loading capacity to check on their influence on the natural rubber

    product0

    5C

    3+ MODIFICATION OF FORMULATION

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    5+ COM OUNDING

    The compounding ingredients were added to the masticated rubber in a se uential order0

    The ingredients were added to the rubber bank that is formed on the nip of the rolls0 The mi;ing

    operation was done with the following order as shown below

    >6tages of mi;ing time of mi;ing (minutes)

    .astication ?On% >

    tearic acid >

    Half filler and processing oil >Remaining half filler and processing oil 9T.Q 5.DT and sulphur >

    uration 5?minutes

    "fter proper mi;ing the compound was than sheeted out from the rolls and live for a

    minimum of 59 hours for proper homogenization of the compounding ingredient before curing0

    3+8 MOULDING AND VULCANIZATION

    The compression molding system was used in the curing of the material fed into the

    mould cavity is soften1 shaped and vulcanized in the mould0 The mould was preheated and

    robs with silicon oil to act as mould releasing agent0 The material was fed into the mould

    cavity and placed in the hydraulic pressing machine (7?tonnes)0 Temperature was applied for

    @ minutes for flat sheets and the mould was however1 opened for an instant1 to allow for

    escape of any entrapped gas produced during cross linking 0

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    >7

    The cure test pieces were removed from the mould after the stipulated time and allowed

    to cool after a week the test piece produce were cut by a cutter machine in a round tin circle

    and was ready for testing0

    >5

    CHA TER FOUR 4+1 TEST4+2 SOLVENT TEST T*

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    olvents used in the assessing the swelling behavior of the vucanizate are petrol 1 diesel 1

    kerosene and water the test sample that were cut were weighed to know their initial weight and

    were immersed into 766ml of the different solvents with a sealed containers for 59hours0

    >

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    A(70) B(140) C(210) D(280)0

    10

    20

    30

    40

    50

    60

    CARB !I"#D$R %!D!%& H%' CARB ! B AC

    FIGURE 2.UPTAKE OF SOLVENT IN THE VULCANIZATE IN DIFFERET

    FILLER LOADING IN DIESEL

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    A(70) B(140) C(210) D(280)0

    1

    2

    3

    4

    5

    6

    7

    8

    *

    10

    CARB !I"#D$R %!D!%& H%' CARB ! B AC

    >?

    FIGURE 3+ U TAKE OF SOLVENT IN THE VULCANIZATE IN DIFFERENTFILLER LOADING INKEROSENE

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    A(70) B(140) C(210) D(280)0

    5

    10

    15

    20

    25

    30

    35

    40

    CARB !I"#D$R %!D!%& H%' CARB ! B AC

    FIGURE4+ U TAKE OF SOLVENT IN THE VULCANIZATE IN FILLER LOADINGIN WATER

    A(70) B(140) C(210) D(280)0

    0+05

    0+1

    0+15

    0+2

    0+25

    0+3

    0+35

    CARB !I"#D$R %!D!%& H%' CARB ! B AC

    >@

    CHA TER FIVE

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    +1 DISCUSSION! CONCLUSION AND RECOMMENDATIONS+2 DISCUSSION

    EFFECT OF SOLVENT TREATMENT /DIMENSIONAL CHANGES OF

    VULCANIZATES

    The effect of solvent treatment on e uilibrium swelling of the vulcanizates in various

    solvents is presented in the -igures71 51 >1 and 9 above0 it was observed that in the vulcanizates

    containing carbon black filler1 the solvent up take was reduced from the filler loading A6 , 5B6

    and increase in from 796, 5761 why carbonized groundnut husk vulcanizate reduced in swelling

    inde; with filler loading from 796 ,5B6 and then increase from A6 , 576 due to the enhance

    interfacial bonding between the filler and the rubber EreferenceF 0 The nature of the fillers1 as

    well as the porosity of the filler1 e;tent of crosslink density characteristics were revealed from

    the solvent interaction with the vulcanizates0 Thus it is clear that e uilibrium solvent up take

    can provide information regarding the efficiency of interfacial bonding EreferenceF0 This is

    compared to the solvent up take of the vulcanizates containing carbon black0

    The percentage increase in the e uilibrium swelling for the vulcanizates cured at different

    filler loading at A61 7961 5761 and 5B6 at 766ml in petrol1 diesel1 kerosene and water are shown

    in the above graphs0

    >A

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    +t was observed that the petrol and diesel in the vulcanizates in carbonized groundnut

    husk has higher swlling inde; to that for carbon black in -igure 7 and 51 why in -igure > the

    vulcanizates in carbon black swells more than the vulcanizates in carbonized groundnut husk on

    filler loading in A6157615B6 why that of 796 the vulcanizates in carbonized groundnut husk

    swells more0 +n water it has e ual level of both the vulcanizates e;cept in 7961 and 576 of filler

    loading that have minor different in the vulcanizates0 The solvent can diffuse into the polymer

    mostly through a direction parallel orientation0 "t low filler loading (A6) the solvent absorption

    of the vulcanizates with carbon black in -igure 71 petrol was higher when compared with that of

    576 filler loading in the vulcanizates0 "s filler loading increases1 the number of filler in a unit

    volume increases and therefore the rate absorption also decreases and the penetrate molecule

    finds it difficult to diffuse into the polymer and therefore the swelling have better result in the

    loading of filler in vulcanizates of carbon black of 5B6 on petrol1 diesel and kerosene why that

    of the vulcanizates of carbonized groundnut husk in diesel of 576 have good swelling also why

    the other filler loading in the vulcanizates have poor swelling0 "lthough during swelling

    dimensional changes are shown by both the vulcanizates on carbon black and carbonized

    groundnut husk vulcanizates on the above -igure071 51 >1 and 90

    +2 CONCLUSION

    # uilibrium swelling observed in the vulcanizates with petrol1 diesel1 kerosene followed

    by water increases as the filler loading decreases showing increased filler polymer matri;

    interaction and hence increased cross link density0

    >B

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    The vulcanizates containing water absorbed less solvent compared to those of petrol1

    diesel and kerosene which absorbed higher solvent of the filler and rubber due to the bonding

    type between the water (hydrogen bonding) and the vulcanizates (covalent bonding)0

    The reason why the following solvent petrol1 diesel1 kerosene and water are use in the

    vulcanizates is to test for the interaction between the solvent and the vulcanizates i0e0 when it is

    use for automobile e uipment like tyre1 engine sitter e0t0c0 when come in contract with these

    solvent petrol1 diesel1 kerosene and water so as to know the interaction between the solvent and

    the vulcanizates0 The interaction determines the shelf life i0e0 to test how long the polymer is

    going to sustain it use as car tyre1 engine sitter e0t0c0 The swelling behavior of this vulcanizates

    determines the level of industrial and type of application of the vulcanizates0

    +3 RECOMMENDATION

    -urther work should be done in accessing the thermal stability of vulcanizates to determine the

    electrical properties of the vulcanizates and also to determine the ability of the vulcanizates to

    bio degradable when they come in contact with micro,organism0

    +t is recommended that for vulcanizates produced from groundnut husk shell high filler loading

    should in industrial application of the materials where they might come in contact with solvents

    and chemicals0

    >C

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    T % *% %*% rd edition Dutter worth 3ondon

    (7CA7)4 7ABA0 +diaghe &0" 5669 physical testing of polymer &onado computer "uchi pp 0B0 $rinciples and Techni ues of $olymer Dlends and 'omposites0 2ear $age BC0 'hika1 .0" (5667) tudent $roject (HN 77)1 "pplication of -iller .i;ture for the

    Thermal tability of Natural Rubber0 "uchi $olytechnic "uchi0 pp0760 olomon0 / and "merongen / & * 7C9B Rubb0 'hem0 Technol057,@A770"nsell .waikanmbo 3 25665 Title of article &0"ppl0 $olym 0 ci B9

    2our referencing is very few1 if you know what you are doing0 " project should have at least 56

    references at your level0 "dd more references from materials used and site them appropriately

    inside the work0

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    96

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