8
Industrial Crops and Products 39 (2012) 89–96 Contents lists available at SciVerse ScienceDirect Industrial Crops and Products journa l h o me page: www.elsevier.com/locate/indcrop Use of cellulose fibers from hemp core in fiber-cement production. Effect on flocculation, retention, drainage and product properties R. Jarabo a , E. Fuente a , M.C. Monte a,, H. Savastano Jr. b , P. Mutjé c , C. Negro a a Chemical Engineering Department, Complutense University of Madrid, Avda. Complutense s/n, Madrid 28040, Spain b Faculdade de Zootecnia e Engenharia de Alimentos, Universidade de São Paulo, Avenida Duque de Caxias Norte, 225, 13635-900 Pirassununga, SP, Brazil c Grup LEPAMAP, Universitat de Girona, Avd. Lluís Santaló S/N, 17071 Girona, Spain a r t i c l e i n f o Article history: Received 21 November 2011 Received in revised form 9 February 2012 Accepted 14 February 2012 Keywords: Fiber-cement Pulping conditions Hemp core Agricultural wastes Flocculation a b s t r a c t The aim of this paper is to study the feasibility of using cellulose fibers obtained from an agricultural waste, hemp core (Cannabis Sativa L.), through different new environmental friendly cooking processes for fiber-cement production. The physical and mechanical properties of the fiber reinforced concrete, which depend on the nature and morphology of the fibers, matrix properties and the interactions between them, must be kept between the limits required for its application. Therefore, the morphology of the fibers and how its use affects the flocculation, retention and drainage processes in the fiber-cement manufacture, and the mechanical and physical properties of the fiber-cement product have been studied. The use of pulp obtained by means of the hemp core cooking in ethanolamine at 60% concentration at 180 C during 90 min resulted in the highest solids retention and the best mechanical properties among the studied hemp core pulps. © 2012 Elsevier B.V. All rights reserved. 1. Introduction The use of agricultural wastes as reinforcement of composite materials is one of the most important targets in today’s materials research (Ahankari et al., 2011; Ashori and Nourbakhsh, 2010; Rabi et al., 2009). The present research is concerned with the use of the wastes from the industrial hemp, Cannabis Sativa L., to obtain useful cellulose fibers to manufacture fiber-cement products for roofing. Industrial hemp is one of the crops having a highest yield among those of temperate zones, being at the same time one of and less intensive ones. It is highly self-compatible what means that it requires crop rotation. Similar to other lignocellulosic fibers, hemp is biodegradable and environmentally friendly (Mutjé et al., 2007). This, together with its high strength and durability and low density, explains the increase in the use of hemp fibers in the manufacture of composite materials (Carver, 1941; Hayo and van der Werf, 2004). The most common material obtained from hemp is its fibers, espe- cially the coarse ones which are extremely strong and durable. As the most valuable fibers are located in the phloem, they must often be separated from the xylem material (“hemp core”), which is con- sidered a waste in the hemp industry (Sedan et al., 2008; Troëdec et al., 2011). Corresponding author at: Chemical Engineering Department, Chemistry Faculty, Complutense University of Madrid, Avda. Complutense s/n, Madrid 28040, Spain. Tel.: +34 91 394 42 45. E-mail address: [email protected] (M.C. Monte). The use of cellulose fibers as reinforcing agents in composite building materials offers many advantages over glass fibers, such as the possibility to manufacture products with low density and good biodegradability (Joshi et al., 2004; Li et al., 2006; Mwaikambo and Ansell, 2003). However, cellulose fibers also have some disad- vantages, for instance, they present low modulus of elasticity, high moisture absorption, they decompose in alkaline environments and are susceptible to biological attack, and they have variable mechanical and physical properties (Swamy, 1990). Some of these disadvantages could be overcome using fibers from hemp core with a higher durability than the traditional cellulose fibers from pine and with a specific tensile strength of 0.750 GPa, and specific mod- ulus of elasticity of 60 GPa. These properties make hemp fibers a candidate material with potential as reinforcement fiber (Li et al., 2004). Many authors have studied the use of hemp fibers as reinforce- ment for building materials based on cement (Dalmay et al., 2010; Placet, 2009; Sedan et al., 2008; Troëdec et al., 2011). However, the use of hemp core fibers for this purpose has not been yet reported. This research aims to contribute to fill this lack of knowledge. In general, cell wall polymers and their matrices determine the mechanical and physical properties of natural fibers. In view of this, a number of researchers have reported the chemical composition of natural cellulose fibers and some of them have recommended improving the natural cellulose fiber properties by modifying the cell wall polymers (Golbabaie, 2006; Wielage et al., 2003; Young, 1997). Furthermore, the incorporation of cellulose fibers in a poly- mer or mineral matrix can involve an interface incompatibility 0926-6690/$ see front matter © 2012 Elsevier B.V. All rights reserved. doi:10.1016/j.indcrop.2012.02.017

Use of Cellulose Fiber From Hemp Core

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  • Industrial Crops and Products 39 (2012) 89 96

    Contents lists available at SciVerse ScienceDirect

    Industrial Crops and Products

    journa l h o me page: www.elsev ier .com

    Use of cellulose bers from hemp core in ber-ceoccul ro

    R. Jarabo utja Chemical Eng id 280b Faculdade de xias Nc Grup LEPAMA

    a r t i c l

    Article history:Received 21 NReceived in reAccepted 14 F

    Keywords:Fiber-cementPulping conditHemp coreAgricultural wFlocculation

    feasihroul and

    of thired fetentiertieof theighe

    1. Introduction

    The use of agricultural wastes as reinforcement of compositematerials is one of the most important targets in todays materialsresearch (Aet al., 2009)wastes fromcellulose b

    Industriathose of temintensive orequires crois biodegradThis, togethexplains thecomposite mThe most cocially the cothe most vabe separatesidered a wet al., 2011)

    CorresponComplutense Tel.: +34 91 39

    E-mail add

    The use of cellulose bers as reinforcing agents in compositebuilding materials offers many advantages over glass bers, suchas the possibility to manufacture products with low density andgood biodegradability (Joshi et al., 2004; Li et al., 2006; Mwaikambo

    0926-6690/$ doi:10.1016/j.hankari et al., 2011; Ashori and Nourbakhsh, 2010; Rabi. The present research is concerned with the use of the

    the industrial hemp, Cannabis Sativa L., to obtain usefulers to manufacture ber-cement products for roong.l hemp is one of the crops having a highest yield amongperate zones, being at the same time one of and less

    nes. It is highly self-compatible what means that itp rotation. Similar to other lignocellulosic bers, hempable and environmentally friendly (Mutj et al., 2007).er with its high strength and durability and low density,

    increase in the use of hemp bers in the manufacture ofaterials (Carver, 1941; Hayo and van der Werf, 2004).

    mmon material obtained from hemp is its bers, espe-arse ones which are extremely strong and durable. Asluable bers are located in the phloem, they must oftend from the xylem material (hemp core), which is con-aste in the hemp industry (Sedan et al., 2008; Trodec.

    ding author at: Chemical Engineering Department, Chemistry Faculty,University of Madrid, Avda. Complutense s/n, Madrid 28040, Spain.4 42 45.ress: [email protected] (M.C. Monte).

    and Ansell, 2003). However, cellulose bers also have some disad-vantages, for instance, they present low modulus of elasticity, highmoisture absorption, they decompose in alkaline environmentsand are susceptible to biological attack, and they have variablemechanical and physical properties (Swamy, 1990). Some of thesedisadvantages could be overcome using bers from hemp core witha higher durability than the traditional cellulose bers from pineand with a specic tensile strength of 0.750 GPa, and specic mod-ulus of elasticity of 60 GPa. These properties make hemp bers acandidate material with potential as reinforcement ber (Li et al.,2004).

    Many authors have studied the use of hemp bers as reinforce-ment for building materials based on cement (Dalmay et al., 2010;Placet, 2009; Sedan et al., 2008; Trodec et al., 2011). However, theuse of hemp core bers for this purpose has not been yet reported.This research aims to contribute to ll this lack of knowledge.

    In general, cell wall polymers and their matrices determine themechanical and physical properties of natural bers. In view of this,a number of researchers have reported the chemical compositionof natural cellulose bers and some of them have recommendedimproving the natural cellulose ber properties by modifying thecell wall polymers (Golbabaie, 2006; Wielage et al., 2003; Young,1997). Furthermore, the incorporation of cellulose bers in a poly-mer or mineral matrix can involve an interface incompatibility

    see front matter 2012 Elsevier B.V. All rights reserved.indcrop.2012.02.017ation, retention, drainage and product pa, E. Fuentea, M.C. Montea,, H. Savastano Jr. b, P. Mineering Department, Complutense University of Madrid, Avda. Complutense s/n, MadrZootecnia e Engenharia de Alimentos, Universidade de So Paulo, Avenida Duque de CaP, Universitat de Girona, Avd. Llus Santal S/N, 17071 Girona, Spain

    e i n f o

    ovember 2011vised form 9 February 2012ebruary 2012

    ions

    astes

    a b s t r a c t

    The aim of this paper is to study thewaste, hemp core (Cannabis Sativa L.), tber-cement production. The physicadepend on the nature and morphologymust be kept between the limits requhow its use affects the occulation, rand the mechanical and physical prop

    The use of pulp obtained by means 180 C during 90 min resulted in the hthe studied hemp core pulps./ locate / indcrop

    ment production. Effect onperties

    c, C. Negroa

    40, Spainorte, 225, 13635-900 Pirassununga, SP, Brazil

    bility of using cellulose bers obtained from an agriculturalgh different new environmental friendly cooking processes for

    mechanical properties of the ber reinforced concrete, whiche bers, matrix properties and the interactions between them,or its application. Therefore, the morphology of the bers andon and drainage processes in the ber-cement manufacture,s of the ber-cement product have been studied.

    hemp core cooking in ethanolamine at 60% concentration atst solids retention and the best mechanical properties among

    2012 Elsevier B.V. All rights reserved.

  • 90 R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96

    Table 1Cooking conditions of hemp core using semi-chemical process.

    Pulps T (C) Time (min) NaOH (%) Yield (%)

    P1 P2

    Table 2Cooking condi

    Pulps

    P3P4

    between bchemical prthe chemic(e.g., electroeffect of thtions betweefciency wber (Negro

    The prosources detfore, it affecof this stagea semi-chemboth at diffthe cellulos

    First, a cocarried out on the berthe study ocement suseffect of usiproperties o

    2. Materia

    2.1. Materi

    The rawfrom the cuLEPAMAP g

    The hemlulose and to obtain hseparated, ocore bers. 10 mm (Mu

    Tables 1pulp by a secess emploand the yie

    The ethacial produc

    Organosrotator digetrol. The puliquor to soexperimentand pulping

    The pulpwith a solualyzer of thin a hydrap

    Table 3Composition of the ber-cement suspensions studied.

    Raw materials Dry weight (%)

    se 5% II cemsilica

    withd, cru

    conus stcore ned

    sincmanuortlar thee sizo 50rosilf micsphemou

    ocsionc polek p06 g/ed intrati

    com sumed, bM1 ws preulp wed asouglly uironm

    eredeted to

    ethod

    Dens beomet

    radi (10

    ore tC forapplyred:180 90 25 49.1140 30 15 68.8

    tions of hemp core using organosolv (chemical) process.

    T (C) Time (min) Ethanolamine (%) Yield (%)

    180 90 60 28.2155 30 40 53.6

    ers and matrix, which may be overcome through theetreatment of bers, with the aim of modifying eitheral nature of the ber surface or the surface propertiesstatic charge, conformation of adsorbed polymers). The

    is treatment is probably a modication of the interac-en the mineral matrix and bers, which increases theith which stress is transferred from the matrix to the

    et al., 2005; Ouajai and Shanks, 2005).cess through which bers are obtained from naturalermines the properties of the bers surface and, there-ts the interface matrixber surface. To study the effect

    on the nal product two different treatments, namelyical pulping process and a chemical pulping process,

    erent cooking conditions have been applied to obtaine bers from the hemp core.mprehensive study of the morphology of the bers was

    (Jarabo et al., 2012); then, the effect of using these bers-cement manufacture process was determined throughf the occulation, retention and drainage of the ber-pensions prepared with the different bers. Finally, theng the obtained bers on the physical and mechanicalf ber-cement probes was determined.

    ls and methods

    als

    material used for this study was the hemp core, wastelture of C. Sativa L. grown in Spain and supplied by theroup.p ber is constituted by 43% cellulose, 16% hemicel-

    8% lignin. Hemp straw is a sub-product in the processemp strands from stalk of the plant. This stalk can ber decorticated, into two main components: bers and

    The initial length of these core bers lies between 5 andtj et al., 2007; Barber et al., 2011).

    and 2 show the cooking conditions used to obtain hempmi-chemical process and a chemical (organosolv) pro-ying NaOH and ethanolamine as solvents, respectively,ld obtained in each case.nolamine PA-ACS solution was supplied as a commer-t by Panreac.

    CelluloASTMMicro

    screenpresse

    Thepreviohemp

    Reerencein the

    A Pused foparticl2 m t

    Mictype ophous small a

    ThesuspenanioniHatsch7.4 1dissolvconcen

    Theries ispreparthem: M2 waKraft pwas us

    Althnormato envbers win the ascribe

    2.2. M

    2.2.1. The

    tipycnatomicing 1 A

    Befat 60

    times measuolv pulping were performed in a 25-L stainless steelster with a heat exchanger system and pressure con-lping conditions were maintained constant as follows:lid ratio: 6:1 and digester pressure 57 bars. Selectedal conditions were: solvent concentration, temperature

    time.ing with NaOH was carried out in the same digester buttion of NaOH having 1.4 g/L of anthraquinone as a cat-e chemical reaction. The cooked pulps were deberedulper and screened through a Somerville vibratory at

    Vp (cm3) =

    Density (g

    where Vp iholder (16.the pressur(PSI), P2 is the W is theent 91%4%

    0.15 mm slot size; the screened pulp was washed,mbled and stored at 4 C.

    ditions chosen in these tables are the result best from audy carried out to optimize these cooking processes forbers (Barber et al., 2011).unbleached pine Kraft pulps (35 SR) were used as ref-e this pulp is commonly used to provide cellulose bersfacture of ber-cement through the Hatschek process.

    nd cement (type II/AV 42.5) containing 12% y ash was probes. It is a ne powder with a wide distribution of

    es, being the 80% of the particles in the interval from m.ica was also used to manufacture of the test probes. Therosilica employed was composed of ultra-thin amor-res of SiO2 with a particle size around 0.5 m containingnts of crystalline quartz (less than 0.5%) as impurities.culant employed to study the behavior of ber-cements and to prepare the ber-cement probes was anyacrylamide (APAM) commonly used in the industrialrocess (Negro et al., 2006) with a molecular weight ofmol and a charge density of 13.4%. The occulant was

    distilled water to prepare solutions of APAM with aon of 1.5 g/L.position of the prepared ber-reinforced cement slur-marized in Table 3. Five ber-cement slurries wereeing the source of cellulose the only difference betweenas prepared using pulp P1 as a source of cellulose bers,pared with P2, M3 with P3, M4 with P4 and the pineas used to prepare the ber-cement slurry MR, which

    a reference.h in air curing ber-cements synthetic bers (PVA) aresed due to their capacity to withstand degradation dueental conditions, in the present research, no synthetic

    used to prepare the probes so as to avoid interferencesrmination of the ber-cement properties that can be

    the use of cellulose bers.

    s

    ity of the bersr density was measured using a gas pycnometer (Mul-er). Helium was the gas employed because its smallus enables it to enter into crevices and pores approach-10 m).he measurement, the samples were dried in an oven

    24 h. The volume of each sample was determined veing Eqs. (1) and (2) to the pressure and volume values

    Vc Vr((

    P1P2

    ) 1

    )(1)

    /cm3) = WVp

    (2)

    s the sample volume, Vc is the volume of the sample

    163 cm3), Vr is the reference volume (8.068 cm3), P1 ise measurement after pressurizing the reference volumethe pressure measurement after including Vc (PSI) and

    dry weight of sample.

  • R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96 91

    2.2.2. Morphological characterization of bersThe morphological characterization of the bers was carried

    out using a ber and pulp morphological analyzer, Mor, V7.9.13.E(Techpap, France).

    This chaconsisting ocamera. Imbers, whicysis, whichwere analyparametersweighted incoarseness,

    Fines arepulps weretheir dimenlength valu75 m, neet al., 2012;

    The samby adding 1the suspensterization w

    2.2.3. FloccA comm

    (FBRM) M5employed tthe propertlength distrcentrationsa focal poinwindow, whcircular patthe focusinthe reecteoptical bethe intercepduration ofmovement.In this waypulses rececase). Each ticles in sureects thecal parametevolution, emeasured pand Schell,

    In the pimmersing pared withAfter 10 minAPAM was lution of thstirring inteformed (dereduced aga(Jarabo et a

    2.2.4. RetenThe equ

    was a vacuua barrier: thup to the ada mesh in th

    and it is connected to a vacuum pump and to a probe in whichthe ltrate is stored and weighted in real time. The nal volume ofltrate is measured. In a typical trial, 400 mL of ber-cement sus-pension, prepared with water saturated in Ca(OH)2, were stirred

    rpmcrea

    Afterringn waacedh thened o obtd cais of

    Prepar rerougals wsolidble 2

    wasas fowatestic y fore ba

    emoecimrepa

    mecinat

    Mechchane Emg con

    rupity (Mtionspan

    thely recsing site f

    (MPa

    Pa)

    (kPa)

    /m2)

    LMAXf the

    majotivelyeec

    absoint coum s

    mece coracterization is based on an image analysis system,f a diode that emits unpolarized light and a micro-

    aging is performed until the equipment counts 5000h is the optimum value for subsequent statistical anal-

    is performed using a computer software. The imageszed using a specic program to determine different

    of the bers and pulps: bers, arithmetic length, length length, average length weighted in area, average width,

    number of microbrills and nes length. generated mainly during the beating stage when the

    debered. There are differentiated from the bers bysions. The equipment was programed to consider beres between 100 and 10,000 m, width between 5 ands length below 100 m and width below 5 m (Jarabo

    Moral et al., 2010).ples for morphological characterization were prepared

    g of dry bers to 600 mL of water and homogenizingion in a laboratory disintegrator ENJO-692. The charac-as done in duplicates.

    ulation of ber-cement suspensionercial focused beam reectance measurement probe00L, manufactured by Mettler Toledo, USA, waso monitor the occulation process and to determineies of the ocs. The FBRM device measures the chordibution on real time over a wide interval of solid con-. A laser beam is generated by a diode and focused ont in the plane next to the external surface of the probeich is inside the suspension. The focal point describes a

    h at a constant speed of 2000 m/s due to the rotation ofg lens. When a particle intercepts the focal point path,d light reaches the detector through the probe and ther. The detector receives light pulses. A chord length ofting particle is determined as the product of the time

    the light pulse by the linear speed of the focal point Thousands of particles can be measured each second., a chord length distribution is obtained from the lightived during the measurement time (set in 5 s in thisdistribution is a function of the size and shape of par-spension. The evolution of the chord size distribution

    aggregation or dispersion of particles. Many statisti-ers can be calculated from the distribution to follow its.g., the mean chord size and the total number of countser second (Blanco et al., 2002; Hubbe, 2007; Kerekes1992; Negro et al., 2007).resent study, the occulation trials were carried outthe probe in a 400 mL ber-cement suspension, pre-

    water saturated in Ca(OH)2, and stirred at 800 rpm., stirring intensity was reduced to 400 rpm. 100 ppm of

    added 5 min later, to induce occulation, and the evo-e ocs was studied at 400 rpm for 4 min. After that, thensity was increased to 800 rpm to break down the ocsocculation) for 2 min and, nally, stirring intensity wasin to 400 rpm to induce the reocculation of the systeml., 2010).

    tion and drainage of ber-cement suspensionipment used for measuring the retention and drainagem drainage tester (VDT). It has two jars separated bye upper jar keeps the ber-cement suspensions stirreddition of the occulant dosage. The second jar containse bottom to carry out the dewatering of the suspension

    at 600was deadded.the stipensiowas plthrougof draiorder ttion ananalys

    2.2.5. Fibe

    tory thmateriwith a evacuagauge)cake wof the in a plathis wafrom thwere rtest spwere ption ofdeterm

    2.2.6. Me

    machinbendinulus ofelasticcalcula

    A sused indigitalprocescompo

    MOR

    LOP (M

    MOE

    SE (kJ

    wherepoint ois the respecis the d

    Thethe pomaxim

    Theafter th during 6 min in the upper jar. Then, stirring intensitysed to 300 rpm and, 5 min later 100 ppm of APAM werer 15 s of contact time between occulant and mixture,

    was stopped, the barrier was removed and the sus-s drained to the second jar in which an 18 mesh wire. The suspension was drained under vacuum (0.2 atm)

    lter and a computerized balance recorded the masswater over time. The drainage curve was analyzed inain the drainage rate for the different occulants. Reten-ke humidity were determined gravimetrically after thethe formed cake (Fuente et al., 2010).

    ration of ber-cement probesinforced cement probes were prepared in the labora-h a slurry vacuum de-watering technique. The matrixere added and dispersed in Ca(OH)2 saturated waters concentration of 20%. The slurry was transferred to an00 mm 200 mm casting box and a vacuum (60 kPa

    exerted until excess water was removed and a solidrmed. The pad was pressed at 3.2 MPa, so that the restr was removed. After pressing, the plates were sealedbag at room temperature. Three pads were prepared in

    each formulation. After 2 days; the pads were removedgs and placed in water. Twenty-six days later, the padsved from the water and four 200 mm 50 mm exuralens were diamond wet-sawn from each pad. Eight padsred to provide sufcient specimens for the determina-hanical properties and four pads were prepared for theion of physicals properties.

    anical properties of ber-cement probesical tests were performed in the universal testingic DL-30,000 equipped with 1 kN load cell. A four pointguration was employed in the determination of mod-

    ture (MOR), limit of proportionality (LOP), modulus ofOE) and specic energy (SE) of the specimens following

    specied in Eqs. (3)(6).of 100 mm and a deection rate of 0.5 mm/min were

    bending test (Savastano et al., 2000). Test data wereorded and reduced using automatic data collection andfacilities. Eight exural specimens were tested for eachormulation.

    ) =(

    LMAXb h2

    ) (Sdown Sup) (3)

    =(

    LLOPb h2

    ) (Sdown Sup) (4)

    = tg(

    LMAX

    ) (Sdown Sup)

    3

    b h3 (5)

    = Absorbed energyb h (6)

    is the maximum stress, LLOP is the stress at the upper linear portion of the stressstrain curve, (Sdown Sup)r span, b and h are the specimen width and thickness,, tg is the initial slope of the stressstrain curve and tion of the composite.rbed energy is the area under the stressstrain curve torresponding to a reduction in carrying capacity to thetress (Tonoli et al., 2010).hanical properties of the probes were measured 28 daysnstruction of the sheet.

  • 92 R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96

    Table 4Morphological characterization of pulps.

    Process Semi-chemical Organosolv Kraft

    Pulps P1 P2 P3 P4 PR

    FibersFibers (106/g 45.2 28.5 10.8Arithmetic l 345 352 456Length weig 459 497 1129Average leng 472 526 1344Average wid 24.0 27.3 25.5Coarseness ( 0.06 0.10 0.18Microbrills 1.68 1.48 1.62

    FinesFines numbe 8947 15,474 49,192Fines length 19.5 25.1 40.3

    2.2.7. PhysiWater a

    were obtainprocedures

    Four spe

    3. Results

    3.1. Morph

    The resubers and pprocess arefor compari

    It is notifrom the heTherefore, tthan that omatrix.

    P1 and Plength weigwhich lowecan be due tpulps P1 antion during

    Regardinsolv), the oand with lo

    NaOH usamorphousthe surfacethe coarsencoarseness Organosolvcelluloses abe used to oorganosolv surface is h

    The percPR and higthe interactimprove th

    It has bequick and 2011).

    3.2. Floccul

    Fig. 1 shand ocs in

    r 600 s of stirring at 400 rpm, the value of the mean chordas constant. 900 s after starting the trial, the addition of oc-

    to the suspension caused a fast increase in the mean chorde to the aggregation of particles to form larger ocs. A max-value of this parameter was reached at 10 or 15 s and thened decreasing with different rate depending on the stabilityength of the ocs in such hydrodynamic conditions (evolu-

    ocs). When the stirring was increased to 800 rpm, part ofaining ocs was broken, thus decreasing the mean chord

    eoc by tcreaan beachent frion ocs fover, hord

    suspand er theose

    resuare mg read theded

    4) 32.0 61.2 ength (m) 356 389hted in length (m) 539 574 th weighted in area (m2) 583 617 th (m) 19.2 29.0 mg/m) 0.08 0.40

    (%) 1.38 1.66

    r 13,149 30,470 (%) 25.4 32.7

    cal properties of ber-cement suspensionbsorption, bulk density and porosity values at 28 daysed from the tested exural specimens following the

    specied in ASTM C 948-81 (ASTM C 948-81).cimens were used to determine these properties.

    ological characterization of pulps

    lts of the morphological characterization of hemp coreulps obtained by both semi-chemical and organosolv

    shown in Table 4. Kraft pine pulp was also characterizedson.ceable that the length of the bers and nes obtainedmp core is much shorter than that of the pine bers.he number the bers per gram on hemp pulps are highern pine pulp. This could improve their dispersion in the

    3, presented lower values of bers arithmetic length,hted in length, average width and coarseness alongr nes length than those for the pulps P2 and P4. Thiso the more aggressive cooking conditions used to obtaind P3, which increase the probability of bers degrada-

    the process.g the effect of the process (semi-chemical or organo-

    rganosolv pulps (P3 and P4) had slightly shorter berswer coarseness than the semi-chemical pulps.ed in semi-chemical process is well-known to remove

    materials, such as hemicelluloses and pectins, from of hemp bers (Trodec et al., 2009); this reducesess of the bers, which is lower for P1. However, theof the organosolv bers is even lower than that of P1.

    process consists of dissolving lignin, extractives, hemi-nd pectin in ethanolamine but in such way that they canbtain valuable chemical products. The efciency of theprocess in removing these compounds from the berigh even when soft cooking conditions is applied.

    Aftesize wculantsize duimum it startand strtion ofthe remsize (dshownwas de

    It cwas rediffereevolutthe oMoreomean cthe MRin M1 but aftthan th

    Theerties cookinfavorewas ad

    d s

    ize (

    m

    )

    50

    60

    70

    80entage of microbrills is similar in pulps P2, P3 andher than in the two other pulps. This could increaseion among the bers and the matrix and, consequently,e properties of the ber-cement.en demonstrated that a ber analyzer (MorFi) can gainreliable results (Bartl and Pico, 2009; Pico and Bartl,

    ation of ber-cement mixtures

    ows the evolution of the mean chord size of particles cement suspensions.

    800

    Mean

    ch

    or

    10

    20

    30

    40

    Fig. 1. Evolutireocculationculation). The reocculation ability of the system ishe increase in the mean chord size when the stirringsed to 400 rpm again.

    observed that the largest maximum mean chord sized in the MR suspension. This value, however, is not toom those reached in suspensions M2 and M4 and thef the mean chord size in these two cases indicates thatrmed were more stable than those formed from MR.after the deocculation and reocculation stages, the

    size in M2 and M4 remained larger than in the case ofension. The maximum mean chord size values reached

    M3 were lower than those reached in the other cases, evolution stage the values obtained were slightly lower

    in MR.lts indicate that the occulation process and oc prop-ore affected by the cooking conditions than by the

    gent used, and that the use of soft cooking conditions formation of larger and more stable ocs when APAMto the ber-cement pulp.

    MR

    M1

    M2

    M3

    M4

    00 rpm 40 0 rpm800 rpm

    locc

    ulat

    ion

    lutio

    n of

    floc

    s

    tion

    cula

    tionTime (s)

    1300120011001000900

    100 ppm

    APAM

    F

    Evo

    Def

    locc

    ula

    Reflo

    c

    on of the mean chord size during the occulation, deocculation and of the ber-cement suspensions.

  • R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96 93

    Table 5Retention and humidity of ber-cement suspensions.

    Fiber-cementsuspension

    Source of bers Retention (%) Humidity (%)

    M1 P1 66.5 1.87 46.8 2.05M2 P2 29.1 4.90 63.7 0.80M3 P3 64.7 1.57 50.5 0.90M4 P4 18.5 5.70 64.7 1.33MR Unbleached Kraft pine 57.3 2.30 57.9 1.20

    3.3. Retention and drainage of ber-cement suspensions

    Fig. 2 shows the drainage curves of the ber-cement suspensionsconsidered in this research.

    Drainage took place in two steps: rst, the suspension was l-trated and a cake was formed with a fast water removal, whichcorresponds to the rst part of the drainage curves (linear partwith a high slope); secondly, the cake was compressed and thick-ened and water removal rate decreases toward zero. During therst stage, only the water between ocs was removed, while partof the water inside the ocs was removed during the compressionstage. Most of the solids loss with the ltrate takes place duringthe rst stage while the second stage determines the nal humid-ity and the formation properties of the cake. Drainage time can beobtained asto zero.

    There arthe ber-ceone for MRintensity ofest values fcompressioweight of rthe case of

    Table 5 scake was foimum valuetogether wisolids, werestage in theremaining iscopicity extwo cases.

    These dition of partiand from th

    0

    Filtr

    ate

    (g

    )

    0

    100

    200

    300

    400

    500

    F

    0

    0.5

    1

    1.5

    2

    2.5

    3

    3.5

    4003002001000

    %

    Chord size (m)

    MR

    M1

    M2

    M3

    M4

    Fig. 3. Chord lengths distribution of the ber-cement suspensions after the additionof the APAM.

    Fig. 3 shpensions Mwere muchspaces amofast. This e

    d MRose form

    amoge ra

    choumeThe sutesse ineten

    the an w

    echa

    4 shorve otainum ee of Mhaviothe clid paan M

    M1 M2 M3 M4 MR the time required to reduce the drainage curve slope

    e notable differences between the drainage curves ofment suspensions containing hemp core bers and the. The initial drainage rate was notably affected by the

    cooking conditions of the pulp and it took the low-or M1 and M3 suspensions. There was no appreciablen stage in the drainage curves of M2 and M4. The nalecovered ltrate was also higher in these cases and inM1.hows that the solids retention was very low when thermed from suspensions M2 and M4, taking its max-

    in the case of suspensions M1 and M3. These values,th the drainage curves, indicate that most of the mineral

    lost with the water drained during the rst drainage case of M2 and M4 with only some of the mineral solidsn the cake and the majority of bers, whose high hygro-plains the high humidity of the cakes formed in these

    fferences can be explained from the chord size distribu-cles in suspension after the occulation process (Fig. 3)e oc properties.

    MR

    M1

    M2

    M3

    M4 anthan thken, despacesdrainasolids.

    Thewere nsions. contribdecreawhen rtent ofless th

    3.4. M

    Fig.The cuthat obmaximthe casical beunder and sorigid th

    4

    6

    8

    tre

    ss

    (M

    Pa

    )Time (s)

    14012010080604020

    M4

    ig. 2. Drainage curves of the ber-cement suspensions.

    0

    2

    0.00

    S

    Fig. 4. ows that the chord size distributions of occulated sus-2, M4 and MR were similar, and that the ocs formed

    larger than in the case of M1 and M3. Therefore, theng the ocs are also larger and water can drain veryxplains the high initial drainage rate observed by M2,. However, the ocs formed from MR are much weakerformed from M2 and M4 and, therefore, they were bro-ed and compressed by the vacuum forces causing theng the ocs to diminish, which implies a decrease in thete (compression stage) and a higher retention of mineral

    rd size distributions of M1 and M3 show that thererous small ocs and particles present in these suspen-paces among the ocs were, therefore, smaller, what

    to an increase in the retention of solids, but causes a the drainage rate. The humidity of the cake decreasestion increases, and this is due to the higher mineral con-cake (water absorbed by the mineral particles is muchater absorbed by the bers).

    nical and physical properties of the probes

    ws the stressstrain curves of the specimens at 28 days.btained with M3 resulted to be the most similar one toed with MR is, although it is worth noticing that thelongation before the failure of the probe was higher in3, while the maximum stress was lower. This mechan-

    r, high elongation and stress reached, and the large areaurves can be associated with a good array of the bersrticles into the composite. The other probes were more3 and MR, as shown by their low strain values.0.020.01

    Strain (mm/mm)

    Stressstrain curves of the composite reinforced with hemp.

  • 94 R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96

    0.00

    2.00

    4.00

    6.00

    8.00 a b

    c

    MO

    R (

    MP

    a)

    0

    000

    000

    12000

    16000

    a)

    0.00

    2.00

    4.00

    6.00

    8.00

    LO

    P (M

    Pa)

    .00

    .15

    .30

    .45

    Fig. 5. lus of

    Thereforthe best mepared with

    Fig. 5 shof rupture, energy of thtwo applied

    These gbers, M3 ylimit of prowere lowerworth poinwere reneand degradbers and mthan those onicant effenot contribas ller andsuspension

    Furthermprepared frobtained fotg.

    A largera better disbearing capber was ususe of pine uct and it mthe beatingimproved

    Despite ties, the phporosity of considered.bers from are probablmatrix.

    of tbilitdroxh hy

    of t watas sleasoGolbs wases.

    resuits o

    n Sta341-

    d

    MRM4M3M2M1

    4

    8

    MO

    E (M

    P

    MRM4M3M2M1

    0

    0

    0

    0

    Sp

    ecif

    ic E

    nerg

    y (

    KJ/m

    2)

    Effect of the hemp on the mechanical properties: (a) modulus of rupture, (b) modu

    e, the probes prepared from M3 may be the ones withchanical properties among the ber-cement probes pre-hemp core bers.ows the results of the mechanical properties: moduluslimit of proportionality, elastic modulus and specice probes of ber-cement made of hemp pulps with the

    processes.ures show that, among the mixtures with hemp coreielded the probes with the highest modulus of rupture,portionality and specic energy, although these values

    than the values obtained with the reference MR. It isting out that the bers used in the preparation of MRd bers. Rening increases the presence of microbrillse ber surface, which enhances the interaction amongatrix. Pine bers and nes lengths are notably greaterf hemp core bers and these parameters also have a sig-

    Oneis its athe hythrougchange

    TheM4 wmain rloses (procesproces

    Thethe limChileaNo. 21ct on the mechanical properties of the probes. Fines doute signicantly to ber-cement strength but act more, in most cases, inuence negatively the drainage of the

    (Tonoli et al., 2009).ore, Fig. 5 shows that the elastic modulus of the probes

    om M4 were the highest, even higher than the valuesr the reference probes. This is due to the high value of

    number of bers per gram could be associated withtribution of bers in the matrix and thus fewer loadsability. However, this was not the case when hemp coreed. Despite on the lower number of bers per gram, theimproved the mechanical properties of the nal prod-ay be attributed to both the superior ber quality and

    process, which produces brillation and consequentlyber matrix bonding (Savastano et al., 2000).the large differences observed in mechanical proper-ysical properties (water absorption, bulk density andthe probes) are similar (Fig. 6) between the composites

    Therefore, they do not explain the effect of the use ofhemp core on the mechanical properties. These effectsy related to the interaction between the bers and the

    4. Discussi

    The effefor ber-cebers morpselves depeto the berat hard coosmall ocs ((Fig. 2) andlower stren(Table 5), pand the othThis indicaM1 and M3suspension

    Albeit aM3, the mewere betterthe bers mrelated to tpercentagefore, it affeMRM4M3M2M1

    MRM4M3M2M1

    elasticity, (c) limit of proportionality and (d) specic energy.

    he drawbacks of the use of cellulose in ber-cementy to absorb moisture from the environment. Due toyl and oxygen-containing groups, moisture is retaineddrogen bonding. This causes a swelling and dimensionalhe bers affecting the composites.er absorption of the probes prepared from M3 andightly lower than those from M1, M2 and MR. Then for moisture absorption is attributed to hemicellu-abaie, 2006), whose removal through the organosolvs more efcient than those for semi-chemical and Kraft

    lts obtained with hemp core and pine bers fall withinf physical and mechanical properties according to thendard (Norma chilena NCh186/1-2003) and the DecretoMEIC.on

    ct of using hemp core bers in the Hatschek processment suspensions and probes is closely related to thehology and to the occulation process, which them-nd on the cooking conditions. The addition of APAM-cement suspensions prepared with the pulps obtainedking conditions (M1 and M3) induced the formation ofFigs. 1 and 3), which slowed down the drainage process

    an enhancement of the compression stage due to thegth of the ocs. This increased the retention of solidsart of them by means of their interaction with the berer part through blocking the small voids among ocs.tes a better performance in mechanical properties of

    ber-cement probes comparing with the ber-cements M2 and M4; however, the drainage is affected.

    high retention solid was obtained for both M1 andchanical properties of the probes obtained from M3

    than those for M1. This can be explained consideringorphology. Although the main effect on the process ishe cooking conditions, the pulping process affects the

    of microbrills, the length, and the coarseness; there-cts the interaction between bers and matrix and the

  • R. Jarabo et al. / Industrial Crops and Products 39 (2012) 89 96 95

    0.00

    5.00

    10.00

    15.00

    20.00

    a

    b

    c

    Wa

    ter

    Ab

    so

    rpti

    on

    (%

    by

    ma

    ss

    )

    0.000

    0.400

    0.800

    1.200

    1.600

    Den

    sit

    y (

    g/c

    m3)

    0.00

    10.00

    20.00

    30.00

    40.00

    Perm

    eab

    le v

    oid

    vo

    lum

    e

    (% b

    y m

    as

    s)

    Fig. 6. Effect odensity and (c

    dispersion microbrillincrease thebetween thneous surfabetween thbe better fo

    In additimay explainby the incre

    At the levbers coueffects astension, c

    It is also pcellulose occur in t

    5. Conclus

    The novmaterials, pfriendly and

    of ber-cement through new environmentally friendly cookingprocesses.

    The cooking process and cooking conditions used to preparethe pulp from the hemp core determined the feasibility of the use

    pulp. Coo

    90 m for nicaler, anditemen

    wled

    auttion 07-6

    to active we Unill as

    Diasity ledg

    of GMRM 4M3M2M1

    MRM 4M3M2M1

    Bulk density Fibers density

    of the factureduringstudiedmechaHowevpulp cober-c

    Ackno

    TheInnovaCTM20Jarabolaboraand thedge aZaqueuUniveracknowversityMRM 4M3M2M1

    f the hemp on the physical properties: (a) water absorption, (b) bulk) permeable void volume.

    of bers in the matrix. The increase in the number ofs, and the slight decrease in the length and coarseness

    surface area, which is available for chemical bondinge bers and the matrix. This leads to a more homoge-ce made of cellulose, which will enhance the adhesione bers and the matrix making this ber-cement probermed.on, there are other mechanisms and phenomena that

    the higher modulus of rupture of M3 probes inducedase in the microbrills:

    el of the microbrils, the longitudinal tension in theld involve not only tensional stresses, but also torsion

    well. This torsion stress, which initially impedes theould subside or relax as a result of the repeated stress.robable that rearrangements and re-orientations of themicrobrils and/or changes in the crystalline fractionhe bers (Placet, 2009).

    ions

    elty of this paper lies in the use of agricultural wastearticularly, industrial hemp straw (C. Sativa L.), as eco-

    renewable source of cellulose bers in the manufacture

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    gments

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