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1 Journal of Korea TAPPI Vol. 48. No. 2, 2016, 46-55p ISSN (Print): Printed in Korea 오일팜 EFB(Empty fruit bunch) 를이용한 MCC 제조및제제적용성평가 김동성 성용주 김철환 1 김세빈 2 접수일 (2016 년 3 월 25 일 ), 수정일 (2016 년 4 월 6 일 ), 채택일 (2016 년 4 월 8 일 ) Preparation and Evaluation of Tabletting properties of Microcrystalline Cellulose from Oil Palm Empty Fruit Bunch Dong Sung Kim, Yong Joo Sung, Chul-Hwan Kim 1 and Se-Bin Kim 2 Received March 25, 2016; Received in revised form April 6, 2016; Accepted April 8, 2016 ABSTRACT The microcrystalline cellulose (MCC) was prepared from oil palm biomass, empty fruit bunch (EFB) for increasing the usability of EFB. The morphological, physical and chemical properties of MCC made from EFB were evaluated by comparing with those of the commercial MCC obtained from AVICEL. The EFB-MCC had the wider distribution in particle size and there were many small particles around 10 μm. There were no significant differences in the cellulose crytallinity and the chemical composition between EFB-MCC and AVICEL-MCC. The properties of tablet samples made by the common direct compression process were evaluated depending on the types of MCC and the compression pressure during tablet making process. The tablet made of EFB MCC showed the higher compressed structure, which resulted in the less disintegration by the water soaking treatment than those made of Avicel-MCC. The results of this study showed that the EFB-MCC could be utilized as one of the commercial MCC. Keywords: White waste paper, fluorescent whitening agent, fluorescence index, surfactant, disintegration 충남대학교농업생명과학대학환경소재공학과 (Dept. of Biobased Materials, College of Agriculture and Life Science, Chungnam Natl. Univ. Daejeon 34134, Republic of Korea) 1 경상대학교환경재료과학과 /IALS(Dept. of Env. Materials Sci./IALS, Gyeongsang National University, Jnju, 52828, Korea) 2 충남대학교농업생명과학대학산림환경자원학과 (Dept. of Environment & Forest Resources, College of Agriculture and Life Science,Chungnam Natl. Univ., Daejeon 34134, Republic of Korea) 교신저자 (Corresponding Author): yosung17@cnu.ac.kr 46 펄프 종이기술 48(2) 2016
2 김동성 성용주 김철환 김세빈 1. 서론 화석연료를대체하는바이오매스기반에너지와소재는지구환경의보전에대한전세계적인관심의증대와함께더욱중요한이슈가되고있다. 대표적인바이오매스자원인목재의경우산림의보존과수요에비해제한적인조림등 1) 으로목재자원의공급이제한되면서새로운대체자원확보가시급한실정이다. 이를위해초본류를포함한농산부산물, 유기성폐기물등다양한바이오매스의활용가능성이평가되어왔는데특히, 발생량과경제성면에서많은장점을가지는오일팜바이오매스는많은관심의대상이되고있다. 오일팜은팜오일의생산을위해주로인도네시아와말레이시아등의열대지방에서집중적으로재배되고있다. 특히인도네시아의경우 8.9백만 ha( 한국국토면적 9.9 백만 ha) 로넓은재배면적을가지고있는데, 팜오일열매수확량은 2010년 2억 2천만톤, 2013년 2억 7천만톤으로매년생산량이꾸준히증대되고있으며 2), 인도네시아 23.5 백만톤 (2011년기준 ) 3), 말레이시아 11.9 백만톤의팜오일이매년생산되고있다. 오일팜의재배와팜오일생산을통해오일팜중빈오일팜열매송이 (EFB, Empty fruit bunch), 오일팜씨박 (PKS, Palm kernel shell), 오일팜잎 (OPF, Oil palm frond), 오일팜트렁크 (OPT, Oil palm trunk) 등다양한폐기성바이오매스가대량으로발생된다. 특히, 팜오일생산과정을통해지속적으로발생되는 EFB(Empty fruit bunch) 는인도네시아와말레이시아각각 25.9, 19.8 백만톤이발생한다고알려져있으며 5), 현재특별한활용용도없이버려지거나연료로활용되는데, 섬유활용 6), 플라스틱복합체 7), 보드 8) 및활성탄소제조 9) 등의다양한연구가진행되고있으나, 대부분저급한용도로활용되고있어고부가가치화활용방안에대한관심이높아지고있다. EFB는셀룰로오스 44.2%, 헤미셀룰로오스 33.5 %, 리그닌이 20.4 % 로로구성되어있는데 10), EFB 구성성분중가장큰구성을차지하는셀룰로오스는바이오매스의주요성분으로, 최근고부가가치화를위한다양한연구개발이집중되고있는데, 특히식의약소재등의주요원료로활용되는 MCC(Microcrystalline cellulose, 미세결정셀룰로오스 ) 제조에대한관심이증대되고있다. 글루코스의 β-d-1,4 글루코시드결합을이루고있는구조로구성된 MCC 11) 는, 순도가높고불순물이거의없 고, 높은결정화도 ( 약 55 ~ 80%) 를가지며 12), 친환경적이고인체에무해한이점을활용하여증점제, 수분보유제, 제제제조등의목적으로화장품, 식품, 제약산업등에 1960년대이후널리사용되고있는주요소재로써 12,13), 주로목재를가수분해하여추출하거나, 면섬유를무기산용매로용해하여 MCC를제조및사용되어지고있다. MCC는추출소재의종류혹은가수분해의조건에따라셀룰로오스의결정화도, 비표면적, 공극구조, 입자크기및분자량등의차이가발생됨을보고된바있으며 13-15), 주로산가수분해를이용하여 MCC를제조하는데 16), 최근다양한비목질바이오매스소재의 MCC의제조를통한고부가가치화활용을위해쥬트 17), 밀과볏집 18,19), 부레옥잠 20), 코코넛껍질 21), 사탕수수찌꺼기 22), 모시 23), 콩껍질 24), EFB를이용하여 MCC를추출하는등다양한바이오매스소재의 MCC 추출에관한연구가보고되었으며 25,26), MCC의고도활용을위해 MCC를추출공정의개선연구 27), MCC의다양한활용을위한 nanowhisker 제조 28), 인산합성을통한활용 26) 등다양한연구가진행되고있다. 특히 MCC는다른소재에비해의약용제제제조가용이하여제제의주요소재로사용되고있으며 29), 다양한소재를활용한제제의제조특성및대체소재에다양한연구가진행되고있다 30,31). 본연구에서는 EFB의고도활용을위한방안으로고순도셀룰로오스소재인 EFB 기반 MCC의제조및활용특성을알아보았다. 특히, EFB 유래 MCC의특성과이를활용하여제제 (tablets) 를제조하여기존상업적으로사용되고있는 Avicel-MCC(PH 101) 과제품적용특성을비교평가해보았다. 이러한실험들을통해향후 EFB를기반으로한고부가가치셀룰로오스소재개발을위한기반자료를제공하고자하였다. 2. 재료및실험방법 2.1. 공시재료 본연구에서는인도네시아에서공수받은 EFB(Empty fruit bunch) 를적용하여실험을실시하였다. EFB는제조및채취공정시다량의불순물이표면에붙게되는데, 이를제거하고 MCC(Micrycrystalline cellulose) 제조시원료에대한영향을최소화하기위해세척후건조하여사용하였다. 제조된 EFB-MCC(Empty fruit bunch J. of Korea TAPPI Vol.48 No.2 Apr
3 오일팜 EFB(Empty fruit bunch) 를이용한 MCC 제조및제제적용성평가 Microcrystalline cellulose) 의비교평가를위해상업적으로사용되고있는 Avicel-MCC(PH 101) 을이용하였다. 2.2 오일팜 EFB 펄핑 오일팜 EFB MCC의제조를위한펄핑방법으로는소다펄핑 (Soda Pulping) 을적용하였는데, 소다펄핑의경우분리된리그닌이 Sulphur-free의특성을가지고있기때문에 32), 페놀릭레진 33), 동물사료 34), 분산제 35) 등으로이용이가능한장점을가지고있다. 본실험에서는 170, NaOH 20%, 액비 1: 6, 2 시간의조건으로소다펄핑을실시하였고 (Table 1), 소다펄핑을실시후흑액을제거한섬유분에서, 40 mesh와 200 mesh 분급을실시하여본셀룰로오스추출을위해 40~200 mesh 사이의분급분을사용하였다. 분급을실시한섬유분에잔류흑액성분이남아있지않도록충분히세척을실시하였다. Table 1. Pulping conditions for EFB pulp Methods Concentration Temp ( ) Time (min) Liquor ratio Soda : 셀룰로오스추출 홀로셀룰로오스추출 펄핑공정에서수득한 EFB 섬유를이용하여홀로셀룰로오스추출을실시하였다. 셀룰로오스추출을위하여 TAPPI Method 중홀로셀룰로오스추출방법을참고하여 (TAPPI standard method T203 cm-99) 1000 ml 삼각플라스크 (Erlenmeyer flask) 에펄프섬유 10 g, 증류수 (distilled water) 600 ml, 아세트산 (acetic acid) 0.8 ml, NaClO 2(sodium chlorite) 4 g을넣은후 water bath에서 70 의온도조건에서 1시간동안반응을진행시켰다. 그후삼각플라스크에따로세척및수득공정없이, 추가적으로아세트산 0.8 ml, NaClO 2 4 g을넣은후다시 1 시간동안 70 의온도조건에서반응을진행시켰으며, 이공정을 2번더반복하여, 총 4시간동안반응을진행시켰다. 그후아스필레이터를이용하여 glass filter(1g3) 에반응이진행된 EFB 펄프섬유를추출하였으며, 산이잔류하지않도록충분히증류수로세척한후아세톤으로한번더세척을실시하였으며, 105 에서건조를실시하였다 알파셀룰로오스추출홀로셀룰로오스추출후건조된시료를이용하여알파셀룰로오스추출을실시하였다. NaOH 17.5% 의용액에 EFB 홀로셀룰로오스를첨가한후약 30 분간침지를실시하였다. 침지된시료를 glass filter(1g3) 를이용하여추출을실시하였다. 추출한후알칼리용액이남아있지않도록충분히세척하였다 MCC 추출건조된알파셀룰로오스를 2M HCL의용액에액비 1:10 의비율로삼각플라스크에첨가한후환류냉각기를이용, 30분동안가열한후 Glass filter(1g3) 를이용하여필터링을실시하였다. 필터링된 MCC를잔여산성분이남아있지않도록충분히세척한후 40 에서건조하였다. 그후건조된 EFB-MCC를막자사발을이용하여최대한고르게분산시킨후사용하였다. 2.4 MCC의물리적특성평가 SEM 분석 EFB-MCC와 AVICEL-MCC의비교평가및제제를제조한후표면및단면의형태를분석하기위하여전자주사현미경 (Field emission scaning electron microscope, EF SEM, Philps XL30 ESEM TMP) 을사용하여평가하였다 입도분석 EFB-MCC와 AVICEL-MCC의입자크기를파악하기위하여입도분석기를이용한입도분포를측정하였다. 입도분석기는 Sympatec GmbH(Germany) 사의레이저회절입도분석기 (HELOS (H1433) & RODOS) 로, 측정범위는 0.1μm ~ 3500μm 까지가능한기기를사용하였다 백색도측정백색도는 KS M ISO 에의거하여 Spectrophotometer(Technidyne, Color touch 2) 를이용하여 EFB-MCC와 AVICEL-MCC의비교평가를실시하였다. 리그닌등의잔류불순물의함량에따라백색도의차이가나타나기때문에이를활용하여셀룰로오스순도대체평가를실시하였다. 48 펄프 종이기술 48(2) 2016
4 김동성 성용주 김철환 김세빈 2.5 화학적특성평가 결정화도분석결정화도를평가및측정을하기위하여 X-ray 회절, IR, FT-IR, Ramen, NMR 분광법등 36) 의방법들중 X-ray 회절방법을이용하였다. EFB-MCC와 Avicel-MCC를 X선회절분석기 (X-ray Diffractometer, Bruker AXS(Germany)/D8 ADVANCE) 를이용하여분석을실시하였으며, 다양한 X-ray 방법중널리쓰이고있는 Segal 법을이용하여 EFB-MCC와 AVICEL-MCC 의결정화도평가를실시하였다 37). 110 plane 과 200 plane 사이에서최소값을나타내는값 (I am) 과최대값을나타내는값 (I 200) 을 Eq.1를이용하여나타내었다. 1 χ CR : Crystallinity index of a specimen, I 200 : max intensity in 200 plane peak, I am : min intensity between the 200 plane and 110 plane peaks FT-IR 분석 EFB-MCC와 AVICEL-MCC의화학적관능기를비교평가하기위하여적외선분광분석장치 (Fourier transform infrared spectroscopy, FT-IR) 을이용하여분석을실시하였다. 각각의시료를전반사측정 (attenuated total reflectance, ATR) 분석시나타나는 peak point 를이용하여분석하였다. 2.6 MCC 제제제조 AVICEL-MCC와 EFB로제조한 MCC로제제를제조하여특성의비교평가를실시하였다. 제제의제조시결정화도, 수분함량, 분말크기등에따른압축특성변화가보고된바있는데 36), 각각의 MCC의수분함량을약 7.5±0.5 % 로조절하여, Single punch press( 가로 :19.10 mm, 세로 : 9.90 mm) 를이용, 전건기준 0.3 g의시료를 10, 20, 30, 40 kg/cm 2 의압력으로약 1분간압착하여제제를제조하였다. 제조된제제를이용하여제조특성평가를실시하였다. 2.7 제제제조특성평가 압축특성평가제조된 tablet을버니어켈리버스 (Vernier Calipers, mitutoyo) 를이용하여원료의종류및압력에따라동일양으로제조된제제의최종두께측정을통해각 MCC 원료의압축특성평가를실시하였다. 두께는가장높은두께가나타나는지점을측정하여압력별 EFB-MCC와 AVICEL-MCC의압축성형조건에따른두께의차이를통해압축성을평가하였다 물풀림성평가제조조건에따른제제의특성변화에따라물속에서의물풀림성이달라지게되는데, 이는의약용제제의제조시고려해야할매우중요한특성으로알려져있다 38). 본실험에서는 MCC 원료의종류및압착압력에따른제제물풀림성평가를실시하였다. 삼각플라스크 (300 ml) 에증류수 50 ml를추가한후제조된제제를약 30초간침지시켰다. 30초간침지시킨삼각플라스크를 Shaker(Lab companion, SI-600R) 를이용하여회전수가 200 rpm에도달한후 1분동안 200 rpm으로회전시킨후삼각플라스크를 40 mesh에필터링하여물속에서풀리지않은제제잔여분의무게측정을통해물풀림성을평가하였다. 3. 결과및고찰 3.1 물리적특성평가 MCC의형태적특성평가 EFB-MCC의형태적특성을기존의 AVICEL-MCC와비교평가하였다. AVICEL-MCC의경우약 50 um 이상의크기를가진것으로알려져있는데, 제조된 EFB- MCC와비교하였을때, 시료의형태가다소긴형태를가지고있는것으로나타났고 EFB-MCC의경우상대적으로다양한형태와입자로구성되어있는것을확인할수있었다. J. of Korea TAPPI Vol.48 No.2 Apr
5 오일팜 EFB(Empty fruit bunch) 를이용한 MCC 제조및제제적용성평가 포에서는 EFB-MCC의크기가 AVICEL-MCC에비해다소커지는것으로볼때, EFB-MCC의경우상대적으로작은입자들이많이존재하고있는것으로판단되었다. <AVICEL-MCC> <AVICEL-MCC> <EFB MCC> <EFB MCC> Fig. 1. Scanning electron micrographs of AVI- CEL-MCC and EFB-MCC 입도분석 AVICEL-MCC와 EFB-MCC의입자크기의분포를확인하기위해입도분석을실시하였다. AVICEL-MCC 의경우입자크기의분포가균일한것과는달리 EFB- MCC의경우입자의분포가매우광범위하게분포하고있는것을 Fig.2를통해확인할수있었다. Table 2에서보여지는것과같이누적분포를통한입자크기의분포분석결과 X50 에서 AVICEL-MCC는 μm, EFB-MCC μm 으로나타났으며, 이후의누적분 Fig. 2. Particle size distribution of AVICEL-MCC and EFB-MCC 백색도평가 MCC의백색도가높을경우잔여리그닌의함량이적은것으로볼수있는데 39), EFB로제조된 MCC와 AVI- CEL-MCC와과의백색도평가를실시를통해외관특성및리그닌의잔여등에따른셀룰로오스의순도특성평가를실시하였다. 평가를실시한결과 AVICEL-MCC와 EFB-MCC가각각 80.05, 79.69로유사한수준의백색도를나타내는것을확인하였다. Table 3. ISO brightness of AVICEL-MCC and EFB-MCC ISO brightness Average Std Dev. High Low AVICEL -MCC EFB-MCC 화학적특성평가 MCC 결정구조평가셀룰로오스의구조는결정영역과비결정영역으로나누어지고이러한셀룰로오스결정화도는제제의제조시영향을미치는데, 결정화도가낮을경우결정화도가높은제제에비해강도적특성이낮게나타난다는보고가있다 40). XRD를이용하여각시료의결정구조를측정한후 Segal식을이용하여 AVICEL-MCC와제조된 EFB- MCC의결정화도를 Eq.1 공식으로계산하였다. 본실험에서 AAVICEL-MCC 75.6 %, EFB-MCC 75.1 % 의결정화도를나타내어선행연구와유사한결정화도를가지는것을확인하였으며 27,41), 이러한결과를바탕으로결정화도는제제제조특성에주요한차이를가져오지않을것으로판단하였다. Table 2. Cumulative distribution of AVICEL-MCC and EFB-MCC Cumulative distribution X 10 X 16 X 50 X 84 X 90 X 99 AVICEL-MCC (μm) EFB-MCC (μm) 펄프 종이기술 48(2) 2016
6 김동성 성용주 김철환 김세빈 Table 4. Crystallinity of AVICEL-MCC and EFB -MCC Crystallinity Min Max Crystallinity(%) AVICEL -MCC EFB-MCC MCC 의관능기평가 FT-IR을이용하여 EFB-MCC와 AVICEL-MCC의화학관능기평가를실시하였다. 스펙트럼에서 1(669 cm -1 ) 은 C-H의 bending 피크, 2(896 cm -1 ) 은방향족알켄의 C-H bending 피크 42), 3,4는 ( cm -1 ) 피크는 C-O-C 신축진동피크 43), 5,6(1320~1425 cm -1 ) 은 OH 면내변동피크 26), 1425는아로마틱링그룹의수소결합의상호작용에대한피크이며 44), 6(1645 cm -1 ) 은물의흡수물분자의상호작용에따른셀룰로오스와물사이의강한상호작용으로인하여나타나는피크 43,45), 7(2900 cm -1 ) 은 CH 2 그룹의신축피크 45), 8(3350 cm -1 ) 은 OH 신축진동피크 43,46) 나타낸다. AVICEL-MCC와 EFB- MCC의 FTIR 스펙트럼이유사한것으로보아화학적관능기의특성차이는거의없는것으로확인하였다. 으로확인되었는데이는 EFB-MCC의넓은입자크기분포로 AVICEL-MCC에비해상대적으로제제제조시팩킹특성이우수하게나타나는것으로판단되었다. 이러한영향으로실제 Fig 5에서나타나는것과같이제제표면에서도상대적으로균일하고매끈한표면을가지게되는것으로나타났다. 제제의단면의비교시에서는특별한차이점이나타나지않았다. Fig. 4. Change in thickness of tablets depending on press pressure of AVICEL-MCC and EFB-MCC. <AVICEL-MCC> <EFB MCC> (a) Surface structure(10 kg/cm 2 ) Fig. 3. FT-IR spectra of AVICEL-MCC and EFB-MCC. 3.3 제제제조특성평가 제제압축성평가 AVICEL-MCC와 EFB-MCC를각각이용하여제조한제제의압력별두께측정평가를실시하여압축성을평가하였다. 또한제조후제제의형태적특성을전자현미경을통해평가하였다. EFB-MCC의동일압력조건에서 AVICEL-MCC에비해밀도가높은제제가형성되는것 <AVICEL-MCC> <EFB MCC> (b) Cross section structure(10 kg/cm 2 ) Fig. 5. Scanning electron micrographs of the tablets made of AVICEL-MCC and EFB-MCC 물풀림성평가 제조된제제가물속에서자연해리되는특성을물풀림성으로비교평가하였다. AVICEL-MCC와 EFB-MCC 모두에서제제제조시압착압력이증가함에따라물에풀 J. of Korea TAPPI Vol.48 No.2 Apr
7 오일팜 EFB(Empty fruit bunch) 를이용한 MCC 제조및제제적용성평가 리지않고남아있는제제의양이증가함을보였으며, 10 kg/cm 2 으로제조한제제를제외하고는 EFB-MCC가상대적으로물속에서덜해리되는것으로나타났다. 이러한현상은 EFB-MCC의형태적특성에서작은크기의입자들이 AVICEL-MCC 보다많이존재하기때문인것으로판단되었다. 이러한특성으로낮은압력으로압착하여제조되는경우입자사이즈가균일하지못하기때문에 AVICEL-MCC에비하여풀어짐성이높아지나, 20 kg/ cm 2 의압력이상으로압착하여제조되는경우상대적으로높은강도의제제가제조됨에따라물풀림성이감소하는것으로판단되었다. 과결정화도는매우유사한것을수있었다. 3) 원료에따른제제제조특성평가를위해압축성, 물풀림성특성을평가한결과, EFB-MCC가 AVI- CEL-MCC에비해압축성이더높은것을확인할수있었으며, EFB-MCC가 20kg/cm 2 압력이상에서제조시 AVICEL-MCC에비해제제강도가우수하여상대적으로물풀림성이낮게나타나는것을알수있었다. 이러한결과를통해입자크기의분포를조절함으로써제제의강도적특성의개선효과를가져올수있을것으로판단되었다. EFB-MCC의적용성을평가한본연구의결과를기반으로하여효율적제조방안과적용성개선방안연구등추가적인관련연구가진행된다면 EFB의고부가가치활용방안을확보할수있을것으로생각된다. 사사 Fig. 6. Changes in water disintegration depending on the tablet making pressure of AVI- CEL-MCC and EFB-MCC. 본연구는산림청 산림과학기술개발사업 ( 과제번호 : S111215L070110) 의지원에의하여이루어진것입니다. Literature Cited 4. 결론 본논문에서는동남아시아를중심으로매년많은양으로발생되는폐기성바이오매스인오일팜 EFB의고도활용방안을모색해보고자 EFB로부터고순도셀룰로오스소재인 MCC를제조하여그특성을평가하여보았다. 특히, 제약산업의소재로적용가능성을평가하기위하여다양한공정조건에서고밀도제제를제조하여제제의품질특성변화를기존의 AVICEL-MCC와비교평가하였고그결과는다음과같다. 1) EFB-MCC와 AVICEL-MCC와의물리적특성을평가한결과, EFB-MCC가 AVICEL-MCC에비해입자크기분포가넓게분포하였고, 상대적으로작은크기의입자분포가높은것을확인할수있었다. 2) XRD, FT-IR을이용한결정화도및화학관능기평가결과 AVICEL-MCC와 EFB-MCC와의화학적조성 1. Kim, D. S., Sung, Y. J., Kim, C. H., and Kim, S. B., Effects of pre-treatments on the oil plam EFB fibers, Journal of Korea TAPPI, 44(6):36-42 (2012). 2. Kim, D. S., Sung, Y. J., Kim, C. H., and Kim, S. B., Changes in the water absorption properties of pulp mold manufactured with oil palm EFB by surface treatments, Journal of Korea TAPPI, 47(1):75-83 (2016). 3. Bardant, T. B., Abimanyu, H., and Adriana, N., Effect of pretreatment technology on enzyme susceptibility in high substrate loading enzymatic hydrolysis of palm oil EFB and water hyacinth, International Journal of Environment and Bioenergy, 3(3): (2012). 4. Abdul Khalil, H.P.S., Nur Firdaus, M. Y., Jawaid, M., Anis, M., Ridzuan R., and Mo- 52 펄프 종이기술 48(2) 2016
8 김동성 성용주 김철환 김세빈 hamed, A. R., Development and material preperties of new hybrid medium density fibreboard from empty fruit bunch and rubberwood, Materials and Design, 31: (2010). 5. Tan, L., Wnag, M., Li, X., Li, H., Zhao, J., Qu, Y., Choo, Y. M., and Loh, S. K., Fractionation of oil palm empty fruit bunch by bisulfite pretreatment for the production of bioethanol and high value products, Bioresource Technology, 200: (2016). 6. Jiménez, L., Serrano, L., Rodríguez, A., and Sánchez, R., Soda-anthraquinone pulping of palm oil empty fruit bunches and beating of the resulting pulp, Bioresource and Technology, 100: (2009). 7. Chai, L. L., Zakaria, S., Chia, C.H., Nabihah, S., and Rasid, R., Physicomechanical preperties of PF composite board from EFB fibres suing liquefaction technique, Iranian Polymer Journal, 18(11): (2009). 8. Khalid, M., Ratnma, C. T., Chuah, T. G., Ali, S., and Choong, T.S.Y., Comparative study of polypropylene composites reinforced with oil palm empty fruit bunch fiber and oil palm derived cellulose, Materials and Design, 29(1): (2008). 9. Alam, M. Z., Ameem, E. S., Muyii, S. A., and Kabbashi, N. A., The factors affecting the performance of activated carbon prepared from oil palm empty fruit bunches for adsorption of phenol, Chemical Engineering Journal, 155(1-2): (2009). 10. Hamzah, F., Idris, A., and Shuan, T.K., Preliminary study on enzymatic hydrolysis of treated oil palm (Elaeis) empty fruit bunches fibre (EFB) by using combination of cellulase and β 1-4 glucosidase, Biomass and Bioenergy, 35: (2011). 11. Sung, Y. J., Lee, Y. J., Lee, J. W., Kim, S. B., Park, G. S., and Shin, S. J., Study of preparation and characterization of microcrystalline cellulose from Miscanthus sinensis, Journal of Korea TAPPI, 42(4):56-63 (2010). 12. Chuayjuljit, S., Su-uthai, S., and Charuchinda, S., Poly(vinyl chloride) film filled with microcrystalline cellulose prepared from cotton fabric waste : Properties and biodegradability study, Waste Management & Research, 28: (2010). 13. El-Sakhawy, M., and Hassan, M. L., Physical and mechanical properties of micro-crystalline cellulose prepared from agricultural residues, Carbohydrate Polymer, 67:1 10 (2007). 14. De Menezes, A. J., Siqueira, G., Curvelo, A. A. S., and Dufresne, A., Extrusion and characterization of functionalized cellulose whiskers reinforced polyethylene nanocomposites, Polymer, 50: (2009). 15. Li, R., Fei, J., Cai, Y., Li, Y., Feng, J., and Yao, J, Cellulose whiskers extracted from mulberry : a novel biomass production, Carbohydrate Polymers, 76:94 99 (2009). 16. Battista, O.A., Hydrolysis and crystallization of cellulose, Industrial and Engineering Chemistry, 42(3): (1950). 17. Fahma, F., Iwamoto, S., Hori, N., Iwata, T., and Takemura, A., Isolation, prepa-ration, and characterization of nanofibers from oil palm empty-fruit-bunch (OPEFB), Cellulose 17: (2010). 18. Jain, J. K., Dixit, V. K., and Varma, K. C., Preparation of microcrystalline cellulose from cereal straw and its evaluation as a tablet excipient, Indian Journal of Pharmaceutical Science, 45:83-85 (1983). 19. Chen, J. N., Yan, S. Q., and Ruan, J. Y., A Study on the preparation and properties of microcrystalline cellulose, Journal of Macromolecular Science, Pure and Applied Chemistry, A33: (1996). 20. Gaonkar, S. M., and Kulkarni, P. R., Improved method for the preparation of microcrystalline J. of Korea TAPPI Vol.48 No.2 Apr
9 오일팜 EFB(Empty fruit bunch) 를이용한 MCC 제조및제제적용성평가 cellulose from water hyacinth, Textile Dyer Printer, 20(26):19-22 (1987). 21. Gaonkar, S. M., and Kulkarni, P. R. Microcrystalline cellulose from coconut shells, Acta Polymerica, 40(4): (1989). 22. Shah, D. A., and Shah, Y. D., Trivedi, B. M. Production of microcrystalline cellulose from sugar cane bagasse on pilot plant and its evaluation as pharmaceutical adjund, Research and Industry, 38(3): (1993). 23. Castro, A. D., and Bueno, J. H., Associacoes de celluloses microfina e microcristalina Na compressao direta. Estudos preliminaries, Revista CIE Pollo Ncias Farmace Pollo Uticcas, 15: (1996). 24. Nelson, Y. U., Edgardo, A. G., and Ana, A. W., Microcrystalline cellulose from soybean husk: effects of solvent treatments on its properties as acetylsalicylic acid carrier, International Journal of Pharmaceutics, 206:85-96 (2000). 25. Wanrosli, W. D., Mohamad Haafiz, M. K., and Azman, S., Cellulose phosphate from oil palm biomass as potential biomaterials, Bioresource, 6: (2011). 26. Wanrosli, W. D., Rohaizu, R., and Ghazali, A., Synthesis and characterization of cellulose phosphate from oil palm empty fruit bunches microcrystalline cellulose, Carbohydrate Polymers, 84: (2011). 27. Ramli, R., Junadi N., Beg, M. D. H., and Yunus, R. M., Microcrystalline cellulose (MCC) from oil palm empty fruit bunch (EFB) fiber via simultaneous ultrasonic and alkali treatment, World Academy of Science, Engineering and Technology International Journal of Chemical, Nuclear, Materials and Metallurgical Engineering 9(1):8-11 (2015). 28. Haafiz, M. K. M., Hassan, A., Zakaria, Z., Inuwa, I. M., and Islam, M. S., Physicochemical characterization of cellulose nanowhiskers extracted from oil palm biomass microcrystalline cellulose, Materials Letters, 113:87-89 (2013). 29. Wang, D., Shang, S. B, Song, Z., and Lee, M. K., Evaluation of microcrystalline cellulose prepared from kenaf fibers, Journal of Industrial and Engineering Chemistry, 16: (2010). 30. Shangraw, R. F., and Demarest, D. A., A survey of current industrial practices in the formulation and manufacture of tablets and capsules, Pharm. Tech., 17(1):32-32 (1993). 31. Suvachittanont, S., and Ratanapan, P., Optimization of micro crystalline cellulose production from corn cob for pharmaceutical industry investment, J. Chem. Chem. Eng., 7: (2013). 32. Gullichsen, J., and C. J. Fogelholm., Book 6: Chemical pulping. Helsinki [etc.]: Fapet Oy [etc.], Gosselink, R. J. A., Abächerli, A., Semke, H., Malherbe, R., Käuper, P., Nadif, A., and Van Dam, J. E. G., Analytical protocols for characterisation of sulphur-free lignin, Industrial Crops and Products, 19(3): (2004). 34. Baurhoo, B., C. A. Ruiz-Feria, and X. Zhao., Purified lignin: Nutritional and health impacts on farm animals A review, Animal Feed Science and Technology, 144(3): (2008). 35. Nadif, A., D. Hunkeler, and P. Käuper., Sulfur-free lignins from alkaline pulping tested in mortar for use as mortar additives, Bioresource Technology, 84(1):49-55 (2002). 36. Heo, Y. D., Sung, Y. J., Joung, Y. J., Kim, D. K., and Kim, T. Y., Changes in the properties of cotton cellulose by hydrogen peroxide bleaching, Journal of Korea TAPPI, 45(3):59-68 (2013). 37. Ahn, J. E., Youn, H. J., Joung, Y. J., and Kim, T. Y., Determination of crystallinity index of cellulose depending on sample preparation and analysis insturments, Journal of Korea TAPPI, 44(4):43-50 (2014). 54 펄프 종이기술 48(2) 2016
10 김동성 성용주 김철환 김세빈 38. Rawas-Qalaji, M. M., Simons, F. E. R., and Simons, K. J., Fast-disintegrating sublingual tablets: effect of epinephrine load on tablets characteristics, AAPS PharmSciTech, 7(2):E1- E7 (2006). 39. Lee, Y. J., and Sung, Y. J., Preparation purified cellulose from rice hull, Journal of Korea TAPPI, 44(3):79-85 (2013). 40. Nakai, Y., Fukuoka, E., Nakajima, S., and Hasegawa, J., Crystallinity and physical characteristics of microcrystalline cellulose, Powder Technol., 54: (1977). 41. Kumar, V., and Kothari, S. H., Effect of compressional force on the crystallinity of directly compressible cellulose excipients, International Journal of Pharmaceutics, 177: (1999). 42. Alemdar, A., and Sain, M., Isolation and characterization of nanofibers from agricultural residues - wheat straw and soy hulls, Bioresource Technology, 99: (2008). 43. Rosa SML, Rehman N, De Miranda MIG, Nachtigall SMB and Bica CLD, Carbohydrate Polymers, 82: (2012). 44. Kumar, V., Maria De La LRM, and Yang, D., Preparation, characterization, and tabletting properties of a new cellulose-based pharmaceutical aid, International Journal of Pharmaceutics, 235: (2002). 45. Jonoobi M, Harun J, Tahir PM, Shakeri A, Azry SS., and Makinejad MD., Physicochemical characterization of pulp and noanofibers from kenaf stem, Materials letters, 65(7): (2011). 46. Zhbankov, R. G., Infrared spectra of cellulose and its derivatives, New York : Consultants Bureau, Plenum Publishing Corporation, Springer(2013). J. of Korea TAPPI Vol.48 No.2 Apr
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