Preparation and characterization of polyurethane /charcoal foam composite Taranitha Taranitharan ran Thiruselvan*, Thiruselvan*, Dr. Dr. Firuz Firuz Zainuddin* Zainuddin* * Polymer Engineering, Engineering, School of Material Engineering, Engineering, Universiti Malaysia Malaysia Perlis (UniMAP), (UniMAP), Kompleks Pusat Pengajian eja!i ", #aman Muhi$$ah, %"&%% eja!i, Arau, Perlis, Malaysia'
Abstract
In this research, polyurethane rigid foam with charcoal ller were prepared and characterized. The purpose is to use coconut shell charcoal ller which was grinded to otain powder form to e used as partic particula ulate te ller ller in polyur polyureth ethane ane foam foam to produ produce ce a compos composite ite with with its mechan mechanica icall streng strength th to e identied y several testings. !roperties of the composite foam were compared with the control !" foam with with four four percen percentag tage e consid consider ered ed #$%, #$%, &%, &%, '% and (%). (%). Two atch atch were were produ produced ced with with dier dierent ent procedures where the rst atch the ller were mi+ed with polyol rst them DI while for the second atch is where the ller were mi+ed with DI then polyol. -ompression test was e+ecuted to compare the modulus and the compressive strength of the lled foam. Density test were also carried out to determine the eect of ller loading on the !" foam. The density does not vary much when more ller is added due to the characteristic structure of the charcoal ller. orphology of the foam surface that undergone the compression test were proed using canning /lectron icroscopy. The images otained shows shows the the ruptur ruptured ed closed closed cells cells and the diere dierence nce in averag average e cell cell size size upon upon ller ller loadin loading. g. The spectroscopy ehavior of the charcoal composite !" foam was analyzed using the Fourier Transform Infrared #FTI0) spectroscopy. spectroscopy. The chemical structure and functional groups were inspected from the pea1 analysis of the sample tested. Key!ors Polyurethane foam* Preparation* +haracteriation* +harcoal* +oconut shell* +omposite +omposite
1. Introduction Introduction any any ye2r3 ye2r3 2go, 2go, pl23t4 pl23t4c c 4ndu 4ndu3tr 3tr4e3 4e3 were were u34ng u34ng d4fferent 14nd3 of fo2m compo34t4on3 to produce 2 v2r4ety of pl23t4c product3 3uch 23 polyethylene 2nd e+p2 e+p2nd nded ed poly poly3t 3tyr yren ene e unt4 unt4ll they they d43c d43cov over ered ed polyureth2ne 2nd th2t 4t could e 2ltered 4n m2ny d4fferent w2y3. !olyureth2ne ased fo2m3 h2ve een commerc42lly u3ed 4n d4ver3e v2r4ety of application 3u3e5uently from 67&83. /ven now we can notice that polyurethane foam plays an important role in industri industrial al sectors. sectors. ostly ostly these these rigid rigid polyure polyurethan thane e foam foam is used used as therm thermal al insu insulat lating ing mater material ials s for for constr construc uctio tion n purp purpose ose and for for sole sole insula insulatio tion n in refriger refrigerators ators and freezers freezers 96:. !olyuret !olyureth2ne h2ne3 3 2re con34der con34dered ed 23 e3ter3 e3ter3 or 2m4de 2m4de e3ter3 e3ter3 of c2ron4c c2ron4c 2c4d 2c4d.. They They 2re 2re 3ynt 3ynthe he34 34ze zed d y the the re2c re2ct4 t4on on of poly olyfun funct4o ct4on n2l hydro+ ro+yl comp ompoun ound3 w4th polyfunct4on2l 43ocy2n2te3. ;n gener2l, c2t2ly3t, 3urf2ct2nt, 2nd low4ng 2gent 2re 2l3o employed employed to varies varies the morphology morphology 2nd proper propert4e t4e3 3 of the foam foam cell cell 3truc 3tructur ture3. e3. In some some cases, these additives were already mi+ed with the polyol and diisocyanates. o3t viale d443ocy2n2te3 2nd 2nd poly polyol ol3 3 2re 2re deve develo lope ped d from from the the r2p4 r2p4dl dly y d4m4n43h d4m4n43h4ng 4ng n2tur2l n2tur2l re3ource re3ource3 3 petroleu petroleum m 9$:. For now, the sustitu sustitution tion is only een discover discovered ed for polyol polyol to e produced produced from renew2 renew2le le re3ource re3ource3 3 3uch 3uch 23 f2t3, f2t3, o4l3 o4l3 2nd 3t2rch 3t2rch from from agricu agricultu lture. re. < numer of re3e2rcher3 h2ve depicted the u3age of renew2le r2w m2ter42l3 to concoct !" foams. =ome of them them h2ve 2ve scr scrutin tinized ized the the poten tential tials s of convert4ng veget2le o4l3 4nto polyol3 for ma1ing !" fo2m3. >>>>>>>>>> >>>>>>>>>> * -orresponding author. Tel.? @'86' &&AA8BA E-mail E-mail aress aress? taranitharanCgmail.com #Thiruselvan.T) In the l2te 67(83, the 2l2y342n !2lm 4l Eo2rd #!E) already commenced in manufacturing manufacturing polyol from from epo+ epo+4d 4d4z 4zed ed p2lm p2lm o4l o4l 9, 9, &:. &:. Ther There e is some some research that already een using polyol decended from ref4ned le2ched deodor4zed #0ED) p2lm o4l to ma1e r4g4d !" fo2m. The den34ty of the ot24ned !" fo2m3 prov4ded prov4ded is 2ppro+4 2ppro+4m2tel m2tely y $88 1gGm 1gGm w4th compre334ve 3trength gre2ter th2n 6 !2. !2lm o4lH 23ed polyol3 polyol3 c2n e wrought wrought for produc4 produc4ng ng r4g4d r4g4d 2nd 3em4Hr4g4d fo2m3 to e utilized 23 w2ll, ce4l4ngH p2nel3 2nd 4n3ul2tor3. The progressive progressive rife u3age of polymer ased 4n3ul2 4n3ul2tor tor3 3 4n veh4cl veh4cle e tr2n3m tr2n3m433 4334on 4on 3y3tem 3y3tem3 3 2nd d43tr4u d43tr4utor3 tor3 h23 fronted fronted to 2n ongo4ng ongo4ng pursuit for 5u2l4ty 5u2l4ty 2nd low co3t3 co3t3 insulato insulators. rs. Th43 pursuit pursuit h23, consecut consecutivel ively, y, re3ulted re3ulted 4n amended amended perform2 perform2nce nce 2nd co3t profits, rought 2out y the u3e of new compo compo34t 34te e 2nd polym polymer4 er4c c re34n re34n3. 3. pora poradic dical ally, ly,
however, although 3ome propert4e3 were enhanced, there is some lo33 of prime perform2nce. Therefore, to under3t2nd the eh2v4or of these improvement and losses caused y additives added such as f4ller3 #c2ron l2c1, ch2rco2l, 34l4c2 2nd m4c2) to p2lm o4lH der4ved der4ved polyuret polyureth2ne h2ne re34n3 several several tests such as therm thermal al,, mechan mechanica icall and morph morpholo ology gy test test were were done. The outcomes of the3e te3t3 undoutedly undoutedly validated th2t th43 type of re34ns 2nd 4t3 compo34te3 c2n e u3ed to augment or m24nt24n the traits of the pure re34n3 2nd affi+ing 3ome e+tr2 features to the r4g4d polyureth2ne fo2m manufactured. Ee34de3, the m2or m2or 4ngred4 4ngred4ent ent to m21e the polyuret polyureth2ne h2ne fo2m h2ve een 3l4ghtly reduced 23 the f4ller pl2y 4t3 p2rt to f4ll up the m2tr4+ of polyureth2ne to reduce the co3t 2nd u32ge of petroleum 23ed re34n3 9B:. Tod2y, h4gh r2te3 of ur2n4z2t4on encountered 4n cert24n reg4on, 23 well 23 2n 4ncre234ng 2w2rene33 2ou 2outt 3u3t 3u3t24 24n2 n24 4l4 l4ty ty,, wh4c wh4ch h me2n me2n3 3 th2t th2t the the chem4c2l chem4c2l3 3 u3ed 4n 4ndu3tr 4ndu3tr4e3 4e3 move3 move3 more tow2rd env4ronment2l fr4endly 2nd to 32ve the deplet4on of petroleum 23ed chem4c2l. Th43 goe3 32me to the product4on product4on of polyureth2ne polyureth2ne r4g4d fo2m th2t 43 dr4v4ng the future future dem2nd dem2nd for 4oH23e 4oH23ed d 43ocy2n 43ocy2n2te3 2te3 2nd polyol3. J3 methylene d4phenyl d443ocy2n2te #D;), doe3 doe3 not not h2ve h2ve 2n effe effect ct4v 4ve e 3u3 3u3t4 t4tu tute te from from commerc4 commerc42l4z 2l4zed ed 4oH23e 4oH23ed d 43ocy2n2 43ocy2n2te3, te3, the ne+t mo3t 4mport2nt m2ter42l 4n r4g4d polyureth2ne fo2m product4on, polyol wh4ch were 2le to e commerc4 commerc42lly 2lly produced produced u34ng p2lm p2lm o4l to 4n4t42l4 4n4t42l4ze ze the 3u3t24n24l4ty 2nd help 4n reduc4ng the deplet4on of petroleum product. F4ller 43 m24nly 2dded to polyureth2ne fo2m to g4ve e+tr2 e+tr2 propert4 propert4e3 e3 for the 2ppl4c2 2ppl4c2t4on t4on purpo3e purpo3e 2nd the3e propert4e3 43 v2lued 23 mo3t f4ller3 2re che2p. -h2rco2l -h2rco2l powder powder f4ller f4ller 43 2l3o very che2p form of c2ron f4ller 2nd the ch2rco2l powder product4on 4n term3 of reu34ng the coconut 3hell 23 2 ch2rco2l 43 very product4ve. =4nce the powdered coconut 3hell ch2rco2l f4lled r4g4d !" compo34te fo2m h23 not een repo eported rted e+t e+ten3 en34ve 4vely 4n the the l4te 4ter2tu 2ture, re, 2n under3t2nd4ng of the compre334on perform2nce of the powdered coconut 3hell ch2rco2l f4lled fo2m 43 re5u4red re5u4red 2nd covered covered 4n th43 3tudy. 3tudy. The 2dhe34on 2dhe34on etween the ch2rco2l p2rt4cul2te 2nd the polymer4c m2tr4+, re2gent3 u3ed 4n fo2m prep2r2t4on, 2nd the d43per34on of ch2rco2l f4ller 4n the fo2m 2re f2ctor3 controll4ng controll4ng fo2m mech2n4c2l perform2nce. perform2nce. The m24n purpose of th43 re3e2rch 43 to determine the the prope opert4 rt4e3 of the the ch2rco2 rco2ll f4lle 4lled d r4g4d 4g4d polyuret polyureth2ne h2ne fo2m from from the testings testings carried out. -harcoal -harcoal ller is process processed ed into re5uired re5uired size and used in dierent percentage for ller incooperation with with poly polyur uret etha hane ne to for form a comp compos osit ite e foam foam.. Dieren Dierentt mi+ing mi+ing method method were were introduc introduced ed and the propert4e3 of the ch2rco2l f4lled r4g4d polyureth2ne fo2m 2re determ4ned y den34ty te3t, compre334ve te3t, 3t, therm2l eh2v4or, morphology 2nd 3pectr 3pectro3c o3cop opy. y. Den34 Den34ty ty te3t te3t 43 done done manua manually lly y
2
weighing the mass and dividing its volume. Density test is done to determine the porosity of the foam. -ompre334ve te3t 43 done u34ng the ;n3tron m2ch4ne foll follow ow4n 4ng g the the #J=T #J=T D6'$ D6'$6) 6).. Th43 Th43 te3t te3t sche scheme me de3i de3ign gnat ates es 2 tech techni ni5u 5ue e for for asce ascert rtai aini ning ng the the comp compre re33 334v 4ve e prop proper ert4 t4e3 e3 of unyi unyiel eldi ding ng cell cellul ul2r 2r m2ter42l3, predominantly e+p2nded pl23t4c3, 23ed on te3t te3t m2ch4 m2ch4ne ne cro33 cro33he he2d 2d mot4o mot4on. n. orph orphol ology ogy 2n2ly343 43 o3erved y u34ng the =c2nn4ng /lectron 4cro3cop 4cro3copy y #=/) #=/) 2n2ly343 2n2ly343.. Four4er Four4er Tr2n3m43 Tr2n3m4334on 34on ;nfr2 0ed -h2r2cter4z2t4on #FT;0) 43 run to 2n2lyze the chem4c2l 2n2ly343 2nd to 4dent4fy the functional group on r4g4d polyureth2ne fo2m with ch2rco2l f4ller lo2ded composite. 2. Experimental "'.' Materials
formul2t formul2t4on 4on for control control 2nd !" w4th the ch2rco2l ch2rco2l powder. Tale Tale The formul2t4on formul2t4on of control control !" fo2m. 2ter42l3 !olyol ;3ocy2n2te -oconut 3hell -h2rco2l !owder
02t4o 6 6.6 H
Tale Tale & The formul2t4on formul2t4on of e+pected coconut 3hell ch2rco2l powder u3ed. 2ter42l3 02t4o !olyol 6 ;3ocy2n2te 6.6 -oconut 3hell -h2rco2l !owder $%, &% 2nd '% "'"' Sample Preparation
The m24n m2ter42l 4n produc4ng produc4ng the coconut 3hell ch2rco2l f4lled r4g4d polymer fo2m 43 polyol, D; 2nd coconut coconut 3hell ch2rco2l ch2rco2l powder. powder. The polyol u3ed 43 the 2314m4fo2m 77BEGB wh4ch 43 3uppl4ed from 2314m4 !olyol =dn. Ehd. 2314m4fo2m 77BEGB 43 2 polyet polyether her polyol polyol w4th w4th 2m4ne 2m4ne c2t2ly c2t2ly3t 3t #K8.(% #K8.(%)) wh4ch w4ll re2ct w4th 43ocy2n2te to form polyureth2ne. T2le 6 3how the phy34c2l 2nd the chem4c2l propert4e3 of the polyol. The d443ocy2n2te u3ed 4n th43 3tudy 43 2314m4n2te (8 2nd 3uppl4ed from 2314m4 !olyol =dn. Ehd. -hem4c2l compo34t4on of 2314m4n2te (8 43 23 follow3L !olymer4c D; #-23 Mo. 786'H(AH7) w4th concentr2t4on of BB% wh4le the other &B% 43 ethylene D4phenyld443ocy2n2te #-23 Mo. Mo. 686H 686H'( '(H( H(). ). T2l T2le e $ 3how 3how the the phy3 phy34c 4c2l 2l 2nd 2nd chem4c2l propert4e3 of d443ocy2n2te. Tale Tale 6 !hy34c2 !hy34c2ll 2nd chem4c2l chem4c2l propert4 propert4e3 e3 of 2314m4f 2314m4fo2m o2m 77BEGB 3uppl4ed from 2314m4 !olyol =dn. Ehd 9':. !hy34c2l Nellow O45u4d dor -h2r2cter43t4c Den34ty #$BP-) 4n 6.68 gGcm Q43co34ty #$BP-) $B8 R B8 cp3 =olu4l4ty 4n w2ter D433olve 4n w2ter Fl23hpo4nt Mot 2ppl4c2le Tale Tale $ !hy34c2l 2nd -hem4c2l !ropert4e3 of 2314m4n2te (8 3uppl4ed from 2314m4 !olyol =dn. Ehd. 9':. The coconut 3hell ch2rco2l u3ed 43 3uppl4ed y S2rr42 S2rr42nw2 nw2re re -h2rc -h2rco2l o2l Er45u Er45uett ette. e. The ch2rc ch2rco2l o2l wh4ch 43 4n the r45uette form 43 gr4nded 2nd 34eved y 2 3c4ent4f4c 34eve w4th 2ppro+4m2tely 'Hm4cron 34ze powder 34eved. The fo2m 43 prep2red 23ed on the mold volume. The mold 43 u3ed to prep2re the fo2m 4n rect2ngul2r fr2me w4th d4men34on3 of clo3ed rect2ngul2r mold 43 $B8mm + 678mm + ABmm. For cont contro roll !" fo2m fo2m the the we we4g 4ght ht r2t4 r2t4o o of poly polyol ol to 43ocy2n2te 43 l ? 6.6. The tot2l we4ght r2t4o of !" fo2m 43 $$8 g #2ccord4ng to d4men34on of rect2ngul2r mold). T2le 2nd T2le & 3how the
The charcoal charcoal in its original form cannot e used as a ller due to its size and need to e processed to ac5uir ac5uire e the the right right size size which which is small smaller er than than ' microns. There were few processes done to get the small small particul particulate ate form form of charcoal charcoal ller from from the chun chun1 1 of coco coconu nutt shel shelll char charco coal als s whic which h we were re origi original nally ly in ri5 ri5uet uette te form. form. Thus, Thus, it is grin grinded ded,, sieved sieved and and oven oven dried dried efor efore e used used as ller ller.. The gr4nd4ng proce33 43 done y u34ng 2 0TH& 4n42ture Ur4nd Ur4nder er wh4ch wh4ch u3e3 u3e3 the pr4nc pr4nc4pl 4ple e of h2mmer h2mmer 2nd coll43 coll434on 4on etwe etween en gr4nd gr4nd4n 4ng g ch2me ch2merr 2nd 2nd 2gge 2gged d cru3h4n cru3h4ng g l4ner, l4ner, 2nd 2du3t the output output f4nene33 f4nene33 y d4ffe d4fferen rentt pore pore 34ze 34ze of repl2c repl2ce2 e2le le f4lter f4lter 3creen 3creen,, 3u4t2le for 3m2ll 3c2le product4on product4on of every m2ter42l. V4th gr4nder 3p4nn4ng 2t &B8 0! the f4nene33 of the gr4nded 43 r2ng4ng from Bmm to 'mm. -h2rco2l r45uette 43 cru3hed 2nd f4lled 4n the gr4nder. The gr4nd4ng proce33 43 done repe2tedly for to 2c5u4re 2 f4ner p2rt4cul2te form. The 34ev4ng proce33 proce33 43 done done to ot24n the e+pected e+pected 34ze of the coconut 3hell ch2rco2l powder. =c4ent4f4c 34eve w4th fl2t me3h 34ze of 'Hm4cron, wh4ch 43 2l3o the de34red 34ze for the p2rt4cul2te f4ller is used to sieve the grinded charcoal powder. =4ev4ng 43 done 2nd the powder 43 collected 4n 2 cle2n cont24ner. The open 34ev4ng 2nd env4ronment hum4d4ty m4ght h2ve c2u3ed the ch2rco2l powder to e 3l4ghtly hum4d 2nd 3t4c1 together thu3 the 34eved ch2rco2l powder 43 !hy34c2l dor Den34ty #$BP-) Q43co34ty #$BP-) =olu4l4ty 4n w2ter
Erown l45u4d -h2r2cter43t4c 6.$$ W 6.$B gGcm 6B8 W $B8 cp3 Mot 3ol 3olule 4n w2 w2ter 2nd 2nd re2ct3 w4th 4t 4mme 4mmed4 d42t 2tel ely y dr4ed r4ed 4n oven oven 2t (8o- for for 2o 2out overn4ght efore u3ed for re2ct4on. The oven dry4ng proce33 repe2t3 every t4me u3t efore the f4ller 43 2dded 4nto the proce33 l2ter on to 2vo4d hum4d4ty.
4+4ng proce33 w4ll e done 4n two w2y3 th2t 43 m4+4ng m4+4ng of f4ller f4ller 4n polyol polyol 2nd d443ocy2 d443ocy2n2te n2te3. 3. !olyol !olyol 2nd ch2rco2l powder 2re m4+ed together u34ng h4gh
3
3peed 3t4rrer 3t4rrer w4th w4th $888 rpm 4n $8 seconds. seconds. Jfter Jfter m4+4ng polyol w4th ch2rco2l powder the d443ocy2n2te 43 2dded 2nd m4+ed for $8 3econds at $888rpm unt4l the m4+ture 43 lended well together homogeneou3ly unt4 unt4ll the the m4+t m4+tur ure e rele rele23 23e e he2t he2t 4nd4 4nd4c2 c2t4 t4ng ng the the 4n4t42t4o 4n4t42t4on n of the chem4c2l chem4c2l re2ct4on. re2ct4on. Jnother Jnother 3et of m4+4ng 43 done w4th 2 3l4ght ch2nge 4n procedure whe where ch2rco 2rco2l 2l powde wder 43 f4r3 4r3t m4+ m4+ed w4th 4th d443 d443oc ocy2 y2n2 n2te te efo efore re 2dd4 2dd4ng ng 4n the the poly polyol ol.. The The m4+ture m4+ture w4ll e poured 4nto the clo3ed mold w4th d4me d4men3 n34o 4on n of $B8m $B8mm m + 678m 678mm m + ABmm ABmm.. Jfte Jfterr pour4 pour4ng ng the m4+ture m4+ture,, the mold h23 to clo3e clo3e f23t f23t efore the m4+ture 43 r434ng 2nd overflow. The mold w4th w4th polyure yureth th2 2ne fo2m fo2m 43 pl2ce l2ced d 4n room room temper2ture 2nd cured for 6 hour and post cured in oven at (88- with the mold for another 6 hour. Jfter cur4ng the 32mple 43 t21en out from the mold. The overall Xow chart is as shown in Figure 6 . "'/' +haracteriation of Samples
Den34ty 43 the m233 per un4t volume of 3u3t2nce3, the 3ymol3 u3ed for den34ty 43 Y #Uree1 letter rho) 2nd 4t3 un4t 2re 1gGm . Vhere volume 43 2 me23ure of the 3p2ce occup4ed y 2 3ol4d 2nd 43 me23ured y mult4ply 2 length y length, 4f the length 43 4n meter the un4t of volume 43 cu4c meter #m ) 2nd m233 43 the 2mount of m2tter 4n 2 ody 2nd 4t3 me23ured 4n 14logr2m #1g). From the ul1 fo2m produced B cue 32mple w4th d4men34on of B8mm + B8mm + B8mm 43 cut cut 2nd 2nd te3t te3ted ed for for 4t3 4t3 den3 den34t 4ty y 2nd 2nd the the 2ver 2ver2g 2ge e den34ty w4ll e recorded for e2ch type of formul2t4on. "'/'"' +ompre112on #e1t
;n th43 re3e2rch, un42+42l compre334on w23 u3ed to te3t te3t 2nd 2nd ev2lu2 ev2lu2ted ted the 3tr24n 3tr24nHr2 Hr2te te effect effect3 3 of the compo34te compo34te m2ter42l3. m2ter42l3. The 2pp2r2tu 2pp2r2tu3 3 u3ed for th43 te3t4ng 43 the 32me 23 th2t u3ed 4n 2 ten34le te3t. The only mech2n4c2l mech2n4c2l te3t4ng u3ed for for th43 re3e2rch 43 the compre compre334 334on on te3t. te3t. -ompr -ompre33 e334on 4on te3t4n te3t4ng g w23 condu conducte cted d 2ccor 2ccord4n d4ng g to J=T J=T D6'$ D6'$6H6 6H68 8 u34ng u34ng 2 "n4ver "n4ver32l 32l Te3t4n Te3t4ng g 2ch4 2ch4ne ne #"T) #"T) ;n3tr ;n3tron on BB'8 BB'8 m2ch m2ch4n 4ne. e. The The 32mp 32mple le d4me d4men3 n34o 4on n 43 2 cue cue of B8mm+ B8mm+B8 B8mm+ mm+B8 B8 mm. The cro33 cro33he he2d 2d 3peed 3peed for comp compre re33 334o 4on n te3t te3t 43 68mm 68mmGm Gm4n 4n 2t $BR $BRo-. Jn 2ver2ge of f4ve 32mple3 43 reported. 4ourie 4ourierr
#ransfo ransform rm
5nfr 5nfrare are
Jfter the 3pec4men w23 deformed, =/ m2ch4ne model model [/OH[ [/OH[= =H'& H'&'8H '8HOJ OJ 433ued 433ued to e+2m4n e+2m4ne e the the 3urf2c 3urf2ce e morph morpholo ology. gy. The The 3pec4 3pec4men men w23 cut cut 4nto 4nto 3m2ll 34ze wh4ch 43 68 mm + 68 mm + 68mm to undergo =/. =/ h23 2n 2dv2nt2ge 4n 3uff4c4ently produce 2 cle2r enl2rgement of the 4m2ge to v4ew the cell 2nd 4t funct4on3 y 3c2nn4ng the 3pec4men w4th h4gh W energy e2m of electron3. &,&\H methylene !olyol @ -oconut shell charcoal d4phenyl d44socy2n2te d44socy2n2te @ -oconut shell i+ #$888 rpm in for $8 sec) i+ #$888 rpm in for $8 sec) &,&\H methylene !olyol d4phenyl
"'/'.' 0en12ty Me31urement
"'/'/' "'/'/' (4#56)
"'/'7' Morphology (8c3nn2ng Electron M2cro1copy)
Spect Spectro rosco scopy py
Fourie Fourierr Transfor ransform m Infrare Infrared d pectro pectroscop scopy y #FTI0) #FTI0) machine machine model model !er1in /lmer /lmer FTHI0 FTHI0 pectro pectrometer meter pec pectr trum um 0H6 0H6 was was used used to char charac acte teri rize ze the the chemical chemical structur structures es of the otained otained rigid rigid charcoal charcoal lled lled !" foam. foam. The !" char charcoa coall compo composit site e foam foam were scraped to otain the powder foam of the foam for aout 8.86 grams to 8.8 grams to e clamped in the FTI0 infrared hole. It is tested from a spectrum ranging from &888 to 'B8 cm H6.
i+ing process #$888 rpm for -asting into mould -uring at room temperature for 6 !ostcured in oven for another 6 hour at 0igid !olyurethane foam lled with coconut shell charcoal com osite 6. $. . &.
Density easurement -ompression test orphology #/) Fourier Transform Infrared spectroscopy #FTI0)
Fig. 6. The flow ch2rt of methodology. 3. Results and discussion /'.' +ompression strength
The variation of compressive compressive strength over charcoal ller loading is clearly shown in Fig. $. From the ar graph graph in Fig. $, the compressiv compressive e strengt strength h tends to increase as the percentage percentage of charcoal charcoal ller were added until certain percentage and it egins to decrease decrease from from the highest highest compres compressive sive strengt strength h value. value. Sowever, Sowever, the decrease decrease in value value still still shows shows etter compressive strength value compared to the unlled polyurethane foam. There is a dierence in value etween the set data of compressive strength etween the 6st atchL where the charcoal ller is mi+ed with polyol rst then DI and the $ nd atchL where the charcoal ller is mi+ed with DI rst then polyol to produce the composite foam.
4
8.A 8.' 8.B FIOO/0 I/D VITS !ONO TS/M 8.& DI "ompressi#e strength ($Pa! 8.
8.$ 8.6 FIOO/0 I/D VITS DI TS/M !ONO
8
Percentage of charcoal ller added (!
lower viscosity and can mi+ faster accordingly to the reaction to produce the foam and ease the process and there is also less chances of the charcoal ller to dispense. Thus, the ller is much well dispersed in this this poly polyur uret etha hane ne foam foam matr matri+ i+ and and show shows s the the enhance in strength. /'"' +ompression Moulus
Vhen Vhen the the modu modulu lus s of a foam foam incr increa ease se,, the the comp compre ress ssiv ive e stre streng ngth th must must also also tall tally y with with the the modulus 9A:. In the region of where the modulus is calculated in the raw data plotted y the Instron\s la automation software aestro, the foam is said to have the deformation of which the foam can still retu return rns s to its its orig origin inal al size size afte afterr the the stre stress ss is remov removed. ed. In other other word, word, it is unde underg rgoin oing g elasti elastic c deformation. Fig. shows that as in tally with the compressive strength the &% charcoal ller loaded foam shows the highest modulus value and it can e analyzed that it shows an increasing trend compared to the control foam which is from $% to '% of the lle llerr load loadin ing g alth althou ough gh ther there e is a slig slight ht fall fall in modulus value for the '% ller loaded foam. The presence presence of ller during the foam e+pansion e+pansion aect the chemical structure of the foam and this causes the foam to ecome rittle and have lower capaility to deform elastically. This is the reason why the '% ller loaded foam shows less modulus value than the &% ller lled foam. /+plaining &% lle llerr load loaded ed foam foam show shows s the the high highes estt valu value e in modulus ecause it is the est ratio of ller that can e distriuted uniformly in the polyurethane foam matri+ and this lowering the pin point of pressure which could cause fracture of the cell.
Fig. $? Qariation of compressive strength over charcoal ller loading. The variation shows shows that the compressive strength strength set data collected for the $nd atch is always higher than the 6st atch. This dierences is mainly due to the mi+in mi+ing g techn techni5 i5ue. ue. !olyol olyol is 1nown 1nown to have have a lower viscosity and molecular weight compared to the DI. Thus, when mi+ing the ller with polyol is much much easier easier and it can e disper dispersed sed easier easier and faster faster throu through ghout out the the polyol polyol.. Sowev Sowever, er, the the ne+t ne+t addition that is the DI have higher viscosity and need longer time to e homogeneously mi+ed with the ller polyol mi+ture. There arises a prolem as the reaction of polyurethane foam to start is very fast and this time restriction causes to reduce the time for mi+ing the polyol ller mi+ture and DI. This might cause the ller not to e well dispersed dispersed thro throug ugho hout ut the the poly polyur uret etha hane ne foam foam matr matri+ i+ and and reduced the value of the compressive strength. Meverthe Mevertheless less,, the $nd atch atch where where the ller ller is mi+ed with DI ta1es longer time to e homogeneously mi+ed and dispersed throughout the DI compared to the ller polyol mi+ing due to the viscosity and the surface tension of the DI. The advantage of doing this mi+ing techni5ue is that the ne+t ne+t added added compou compound nd which which is the polyo polyoll have have
The pressure pressure pin point will usually occur in the area where there is agglomeration of llers which causes uneven distriution of force or pressure to cause the cells in the foam to fracture and lowers the aility to reform its cell size after the force was removed. A ' B FIOO/0 I/D VITS !ONO TS/M DI & $odulus ($Pa!
$
FIOO/0 I/D6VITS DI TS/M !ONO 8
8
8.8$ 8.8& 8.8' 8.8(
Percentage of charcoa l ller added (!
5
Fig. ? Qariation of compression modulus over charcoal ller loading. /'/' 0ensity #est
Density test is done done y dividing dividing the mass of of the part partic icle les s in a mate materi rial al y the the over overal alll volu volume me occupied y it. The overall volume sum is including interHparticle interHparticle void\s volume, particle\s volume and the the inte intern rnal al volu volume me of the the pore pores s 9(:. 9(:. For foam foam produced in closed molds the density seems to tally with the compressive compressive strength value as ller loading amount varies. The density change can e oserved through the morphology of the cell itself. In Fig. &, the graph shows that the highest density value is shown y the foam loaded with &% of charcoal llers with the $nd atch showing slightly higher value than 6st atch. This is mainly due to the mi+ing method, where the visco viscosit sity y play play its role role as e+pla e+plain ined ed in third third paragraph in section .6. n the other hand, for the lowest lowest densi density ty is shown shown y the (% ller ller loaded loaded foam.
B8 &7 FIOO/0 I/D VITS DI FI0T TS/M !ONO &( #$nd Eatch)
Fig. &? Qariation of density over ller loading ased on two mi+ing method. Sowever, the decrease is not much as and varies a lot in raw data otained this is caused y the natural characteristic of the charcoal particles itself as they they have have mill millio ions ns of pore pores s to aso asor rs s air air molecules 968:. This is ecause during the charcoal ma1ing ma1ing process process the charcoal charcoal will e treated treated with o+yge +ygen n whic which h then then incr increa ease ses s its its adso adsor ren entt characteristics. Sence as this occluded air molecules increasesL the ul1 density tends to decrease. /'7' Morphology (SEM)
canning electron microscopy result were shown in the followi following ng Fig. Fig. B to Fig. ig. ( accor accordin ding g to the the percentage of ller added. The accelerated voltage used used was was 68 1Q. The The scan scanne ned d cros crossH sHse sect ctio iona nall surfaces surfaces are showing showing ruptured ruptured cells cells as the foam were were scanned scanned after after the compres compression sion testing were were done. It can e noticed that some unruptured cells are almost spherical in shape with many windows which shows that they are closed cells 966:. The size of the foaming cell decreases as the percentage of llers added increases 96$:. From the result of / itself there is a gradual change in cell size averagely from Fig. B to Fig. (. Sowever, to e precise the uniformity of the cell size is varied when ller added this is ecause the dispersion of llers in the matri+ during the foaming will will cause cause dier dierenc ence e in force force to get get the foamin foaming g done. Thus, causing it to e smaller as the more ller is added more force needed for foaming with the ller incorporated on the cells and vice versa. 96$:.
6
addition from $%, &%, '% to (% there is gradual change in average cell size accordingly from &B8 ^m, &88 ^m, (8 ^m to 88 ^m.
Fig. B? -ontrol !" foam without charcoal llers.
Then for there is a pea1 identied after the charcoal ller is incorporated with the !" foam. This region indicates the hydrogenHonded hydrogenHonded HS stretch as noted it may oscure other pea1s in this region. !articularly, the newly mar1ed pea1 in this region which which lays in the range range of $($8H $($8H$A $A(8 (8 show show the functional group, MH-S the methylamino methylamino radical. In general, there is no much dierence in pea1 from the results otained for the rst atch and the seco second nd atc atch h due due to the the same same aggr aggreg egat ate e of chemicals and materials used in process while the die diere renc nce e is ust ust focu focuse sed d on the the meth method od of processing processing which also proves proves that charcoal does not have any specic chemical reaction with polyol or DI and a good choice to e used as ller. Control $B6A.(& '$.B6
6.A(
$7B6.BA $(A(.A6
$6'(.'6 $8$(.BA
7$(.(8 6'8B.(6 67&.$6 68$.$&
ABB.$$
6A87.'&
2% Polyol 6B6A.AB '$.&& 8$.B6
$7(B.6 $ (8 7. $$ $(A7.8&
$ & A. B $8$A.8' $6A6.66
6$6'.76
68AB.AA
6'8'.$$ 6'8'.$$
78.(7 67.7$ 68$.(8
ABA.7
6A68.7&
%T
6B6(.BB
4%Polyol $7('.(
'6.(
Fig. '? !" foam lled with $% charcoal ller.
$77.88
6$6(.86
68A7.$A
$8$'.&$ $6'B.(6
$(8(.(6
78.'6
$(A7.67
6'8'.68 67&.8( 68$.'A
ABA.&
6A68.A& 68AA.B
8% Polyol
6B6A.(
'6.7'
$77.A&
$(8A.'6 $7(A.77 $(A7.8&
3600
3200
2800
2400
2000
68(8.&' 6$6A.6A
6'8&.(A 6'8&.(A 67&.$$ 68$.'
6A66.8$
4000.0
6$6A.$
6B6A.6
$B8.&7 $8$'.6( $6'&.$'
18 1 800 cm-1
1600
1400
ABA.AA
1200
1000
800
6 50.0
Fig. 7? FTI0 spectrum of -ontrol !" foam and 6 st atch charcoal ller mi+ed composite foam.
Control $B6A.(& '$.B6
$7B6.BA
$6'(.'6 $8$(.BA
6.A(
7$(.(8 6'8B.(6
$(A(.A6
67&.$6 68$.$&
Fig. A? !" foam lled with &% charcoal ller.
ABB.$$
6A87.'&
2% MDI 6B6A.AB '.&7
8.68
$(8'.76 $7(A.87 $(A(.(
$&7.8B $8$(.( $6'(.8(
6$6'.76
68AB.AA 7$(.&$
6'8B.'$ 67&.8$ 68$.B
AB'.7'
6A68.(&
%T
6B6A.8
4% MDI
'$.$$
6.7B 7B
$(A7.8' $7((.B$
6$6'.7B
68A7.'B 7$7.B&
$&'.(7
$(8(.(B
$86.(
$6A8.$A
6'8'.86 67&.6$ 68$.$
6A68.&'
6$6A.A(
8% MDI
AB'.A'
68(8.BA
6B6(.B6 '$.86
8.$B
$7(A.$( $ (8 (. 'B $(A7.6A
6$6A.'
6B6A.6
$ & A. &6 $8$A.$7 $6'A.'$
78.A$
6'8B.87 67&.6A 68$.(
68A7.AB
ABA.8$
6A87.7&
4000.0
Fig. (? !" foam lled with (% charcoal ller. /'9' 4ourier transform infrare spectroscopy (4#56) The FTI0 spectrum of the !" foams prepared from palm oilHased polyol is shown in Fig. 7 and Fig. 68 e+hiit the characteristic pea1s of urethane onds at wavenumers wavenumers ranging from 6& to $77 cmH6 #HMS stretc stretchi hing ng), ), 6A87 6A87 to 6A6$ 6A6$ cmH6 cmH6 #H- #H- stretc stretchin hing) g) 6B6A to 6B67 cmH6 #HMS ending) and 67 to 67B cmH6 #H-MS #H-MS asymmetr asymmetric ic stretch stretching) ing).. They also e+hi e+hiit it a chara characte cteri risti stic c pea1 pea1 of unre unreact acted ed M- groups which is collective in materials synthesized using spare isocyanate relative to polyol.
3600
3200
2800
2400
2000
1800 cm-1
1600
1400
1200
1000
800
65 6 50 .0
Fig. 7? FTI0 spectrum of -ontrol !" foam and 6 st atch charcoal ller mi+ed composite foam %. "onclusion
Vrapping up this research, the preparation of the charcoal charcoal lled polyur polyuretha ethane ne composite composite foam were were accomplished and the characterization were done y analyzin analyzing g the morpholo morphology gy and mechanic mechanical al testing testing data. 0esult otained were sorted to two set of data due due to the the twoHd twoHdi ier eren entt mi+i mi+ing ng meth method od used used.. -onclusion were drawn for compression test that the parti particu culat late e char charcoa coall ller ller has has the cred credi iili ility ty to enhance the strength of the foam. "pon addition of
7
the charcoa charcoall ller ller $% and and &% f ller ller conten contentt the strength and the modulus increases correspondingly and decreases upon further addition of ller of '% and (%. Sowever, the decrease is still considered etter than the result control !" foam. From here it is conc conclud luded ed that that the optim optimum um amoun amountt charc charcoal oal ller addition into the polyurethane foam matri+ lays in the range of $% to '%. Motaly the $ nd atch results show an average of etter results compared to the 6st atch. This is due to the viscosity or the te+ture of the DI that said to e soften upon the stirring at $888 rpm in the $ nd atch efore adding the ller and the polyol that e added is already less viscous compared to DI can e mi+ed homogenenously much faster which is ust aout $8 second. -ontrarywise, the 6st atch does not have this this advant advantag age e as the the visco viscous us DI DI will will e added added straight away which will need more time for mi+ing to get homogeneous, and this race the reaction time for foaming foaming.. The compressio compression n modulus modulus does tally with the compression strength and density on the whole. It can e noticed that the density does not avert much eventhough the set of data correspond the the modu modulu lus s and and stre streng ngth th eca ecaus use e of the the the the charcoal charcoal structur structure e and process processing ing nature nature to have pores to adsor air particle. /venthough measures were were ta1en ta1en y oven oven dryin drying g the ller every time efore incorporation were done there is still some deviation.
I would li1e to e+press e+press my deepest gratitude to my pro proec ectt supe superv rvis isor or Dr. Dr. Firuz iruz Zain Zainud uddi din n for for oppo opport rtun unit itie ies s she she had had gave gave me to lear learn n and and to complete the proect under her supervision. I also would li1e to than1 oth the master students under my supervisor uhaili and Sazmi for their guidance that really helped me in solving most of the prolem prolem on the study.
References
96:
9$: 9:
9&:
9B:
9': 9A: 9A:
9(: 9(: 97: 97: 968: 968:
966: 966:
96$: 96$:
`lempner, D., 2nd Fr43ch, `. -. 6776. S2ndo S2ndoo1 o1 of !olymer4 !olymer4c c Fo2m3 Fo2m3 2nd Fo2m Technology,\\ Technology,\\ +ford "n4ver34ty !re33, Mew Nor1, Nor1, M.N. -h42n, `.=. 2nd U2n, O.S. 677(. Development of 2 r4g4d !olyureth2ne Fo2m from p2lm o4l. [. Jppl. !olym. =c4. '(? B87. 2znee, T. ;., Mor4n, Z. `. =., o4, T. O., =2lm42h, J. 2nd U2n, O. S. $886. /ffect3 of Jdd4 Jdd4t4 t4ve ve3 3 on !2lm !2lmHE HE23 23ed ed !oly !olyur uret eth2 h2ne ne Fo2m3. [. 4l !2lm 0e3. 6? A. Mor4n, Z. `. =. =., o4 o4, T. O. 2nd 2nd =2l =2lm42h, J. $88& $88&.. /ffe /ffect ct of Tr4e Tr4eth th2n 2nol ol2m 2m4n 4ne e on the the !ropert4e3 of !2lmHE23ed Fle+4le !olyureth2ne Fo2m3. [. 4l !2lm 0e3. 6'? ''. Vu, O., O., Q2n Q2n Uem Uemert, [., [., b -2m2rgo, 0. /. #$86$). 0heology 3tudy 4n polyureth2ne r4g4d fo2m fo2m3 3. Sunt3m2 t3m2n n -or -orpor2t or2t44on $678 /+ecut4ve S4ll3 Elvd. Juurn S4ll3, ; &($' "=J. =chm4dt S.!., V4l3on `. The BB u3e3 of 4och2r, 4och2r, the E4och2r E4och2r [ourn2l [ourn2l $86&, Jr2z, Jr2z, =w4tzerl2nd. Oems Oemstr tra, a, !.[ !.[., ., et al., al., -ompr ompres essi sive ve Fai Failu lurre in Sigh odulus !olymeric Fires, in Integration of Funda undame ment ntal al !olym olymer er cie cienc nce e and and Technolog Technology y. 67((, pringer pringer Metherlands. Metherlands. !. B&BHB&7. -hri -hrist stia ian, n, T. T. 0ev 0evie iews ws,, eHt eHtud udy y Uuid Uuide e for? for? oi oill in the /nvironment? -ram686. Ueor Ueorg ge, V., V., #67 #67(A). The The ;-; ;-; !oly olyureth reth2 2ne3 Eoo1. !ulication V4ley b =on3, Mew Nor1. [ohn [ohn3o 3on, n, !. !. -. 4n Jdv2 Jdv2nc nce3 e3 4n !ol !olyu yure reth th2n 2ne e Technology, Technology, #/d. Eu43t, [. . 2nd Uudgeon, Uudgeon, S.), S.), [ohn [ohn V4ley V4ley 2nd =on3 =on3 ;nc., ;nc., Mew Mew Nor1, Nor1, 67'(. !. &. -hua -huay yul uli it, t, ., ., angp angpa1 a1de dee, e, T. T. and ara arava vari ri,, ., $88A. !rocessing and properties of palm oilHased oilHased rigid rigid polyur polyuretha ethane ne foam. foam. Metals Mater Miner , .:, pp.6AH$. Fan, an, S., Te1 Te1ee eei, i, <., <., upp uppes es,, U.[. U.[. and and Ssie Ssieh, h, F.S., .S., $86$ $86$.. !rope !roperti rties es of ioa ioased sed rigid rigid polyure polyurethan thane e foams foams reinfor reinforced ced with llers? llers? micro microsp spher heres es and and nanoc nanoclay lay. 5nternational ournal of Polymer Polymer Science Science, "%.".
8