Proceedings of the 55th International Convention of Society of Wood Science and Technology

August 27-31, 2012 - Beijing, CHINA

Preparation And Morphology Of Nanocrystalline

Cellulose From Bamboo Pulp

Zhi-Ming Liu, Cheng Xie

(Key Laboratory of Bio-based Material Science and Technology of Ministry of

Education, College of Material Science and Engineering, Northeast Forestry

University, Harbin 150040, P. R. China)

ABSTRACT

The nanocrystalline cellulose (NCC) from bamboo pulp was prepared with two kinds of
preparation conditions. Condition 1 is by using 55% of sulfuric acid mass fraction, 50℃ of
reaction temperature and 4 h of hydrolysis time. Condition 2 is 55% of sulfuric acid mass
fraction, 55℃ of reaction temperature and 3h of hydrolysis time. The morphology of NCC of
bamboo pulp was characterized with Environmental Scanning Electron Microscope (SEM)
and Transmission Electron Microscope (TEM), respectively. For the surface morphology of
NCC from bamboo pulp, there is no significant difference between Condition 1 and
Condition 2 by SEM. The surface morphology of rod-like NCC of bamboo pulp under
preparation condition 1 forms a mesh under TEM.

Keywords: nanocrystalline cellulose, bamboo pulp, preparation; morphology

INTRODUCTION

Acid hydrolysis method is one of methods for nanocellulose preparation (Ye, 2007; Song et al.
2011; Satyamurthy et al. 2011; Bondeson et al. 2006). Nanocellulose can be prepared with
different raw materials (Chen et al. 2012; Voronova et al. 2012; Peng et al. 2012; Lu et al.
2012; Dai, 2011;Liu et al. 2011). Green composites are prepared from sustainable
nanocellulose with biodegradability of nanocellulose (Abdul khalil et al. 2012; Zhen et al.
2008; Yuan et al. 2010; Fan et al. 2010). Some researchers analyzed the morphology of
nanocellulose (Liu et al. 2011; Tang et al. 2010; Krishnamachari et al. 2011). Bamboo pulp is
a kind of raw materials for nanocellulose preparation. Nanocrystalline cellulose from bamboo
pulp is prepared with sulfuric acid hydrolysis method and its morphology is analyzed by
scanning electron microscope (SEM) and transmission electron microscope (TEM),
respectively, for providing the basic data of green composites.

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 Proceedings of the 55th International Convention of Society of Wood Science and Technology
August 27-31, 2012 - Beijing, CHINA

MATERIALS AND METHODS

Materials
Bamboo pulp, Guizhou Chitianhua Co., Ltd.; Sulfuric Acid (AR), Tianjin Kermel Chemical
Reagent Development Center. Samples of bamboo pulp are listed in Fig. 1.

Fig. 1 Samples of bamboo pulp

Instruments
FZ102 Micro-plant shredders, 101-2A Drying oven, Tianjin Taisite Instrument Co., Ltd.;
scientz-ΙΙD Ultrasonic cell crusher, Ningbo Xinzhi Biotechnology Co., Ltd.; FD-1A-50
Freeze-drying machine, Beijing Boyikang Experimental Instrument Co., Ltd.; H-7650
Transmission electron microscopy, Japan Hitachi Instrument Co., Ltd.
Determination of composition of bamboo pulp

Moisture content, ash content, SiO2 in the ash content, lignin content , cellulose content of
bamboo pulp were determined (Gao,2008; Nie,2008; Liu et al. 2011; Chen et al.1994; Xiao et
al. 2009).

Preparation of nanocrystalline cellulose

2 g of bamboo pulp was placed into 100 mL reactor with mass fraction 55% sulfuric acid.
Nanocrystalline cellulose (NCC) from bamboo pulp was prepared with two kinds of
preparation conditions. Condition 1 is by using 55% of sulfuric acid mass fraction, 50℃ of
reaction temperature and 4 h of hydrolysis time. Condition 2 is 55% of sulfuric acid mass
fraction, 55℃ of reaction temperature and 3 h of hydrolysis time. The suspended solution
was obtained respectively and centrifuged several times with NaHCO3 neutralizing until the
suspended solution is neutral, and then was placed in the ultrasonic cell disruption
instruments for 10 min disruption, nanocrystalline cellulose colloid was obtained and
freeze-dried.

RESULTS AND DISCUSSION

Composition of bamboo pulp

Composition of bamboo pulp is listed in table 1.

Table 1 Composition of bamboo pulp

Moisture Ash SiO2 in the ash Lignin Cellulose
content/% content/% content /% content/% content/%
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5.15 4.25 0.11 5.43 88.96

SEM morphology analysis of bamboo pulp nanocrystalline cellulose

SEM morphology of bamboo pulp nanocrystalline cellulose is listed in Fig. 2.

SEM of condition 1 SEM of condition

2
Fig. 2 SEM of bamboo pulp nanocrystalline cellulose

For the surface morphology of nanocrystalline cellulose from bamboo pulp, there is no
significant difference between Condition 1 and Condition 2 by SEM.
TEM morphology analysis of bamboo pulp nanocrystalline cellulose

TEM morphology of bamboo pulp nanocrystalline cellulose is listed in Fig. 3.

TEM of Condition 1
Fig. 3 TEM of bamboo pulp nanocrystalline cellulose

The surface morphology of rod-like nanocrystalline cellulose of bamboo pulp under

preparation condition 1 forms a mesh under TEM.

Bamboo pulp nanocrystalline cellulose is prepared with 55% of sulfuric acid concentration,
22-min ultrasonic time, 49.5℃of reaction temperature and 3.25 h of reaction time, TEM
morphology of bamboo pulp nanocrystalline cellulose with ultrasonic-assisted acid
hydrolysis method is listed in Fig. 4.

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August 27-31, 2012 - Beijing, CHINA

Fig. 4 TEM of bamboo pulp nanocrystalline cellulose with ultrasonic-assisted acid hydrolysis
method

The surface morphology of rod-like nanocrystalline cellulose of bamboo pulp with

ultrasonic-assisted acid hydrolysis method forms a mesh under TEM.

CONCLUSIONS

For the surface morphology of NCC from bamboo pulp, there is no significant difference
between Condition 1 and Condition 2 by SEM. The surface morphology of rod-like NCC of
bamboo pulp under preparation condition 1 and ultrasonic-assisted acid hydrolysis method
forms a mesh under TEM.

ACKNOWLEDGEMENTS

The authors are grateful for Project 31070633 supported by National Natural Science
Foundation of China, supported by “the Fundamental Research Funds for the Central
Universities” (DL11EB01), Human Resources and Social Security Department of China
Returned Overseas Students Science and Technology Merit-Based Funding
Project(07041311401) for financial support.

REFERENCES

ABDUL KHALIL H.P.S.; BHAT, A.H.; IREANA YUSRA A.F. Green composites from
sustainable cellulose nanofibrils: a review[J]. Carbohydrate Polymers, 2012, 87: 963-979.

BONDESON, D.; MATHEW, A.; OKSMAN, K. Optimization of the isolation of nanocrystals

from microcrystalline cellulose by acid hydrolysis[J]. Cellulose, 2006, 13: 171-180.

CHEN, H.L.; GAO, T.M.; ZHENG, L.; et al. 2012. Preparation of nano-crystalline cellulose
from pineapple leaf fiber. Chinese Journal of Tropical Crops, 33(1): 153-156. (in Chinese)

Paper PS-30 4 of 6
 Proceedings of the 55th International Convention of Society of Wood Science and Technology
August 27-31, 2012 - Beijing, CHINA

CHEN,Q.Z.; ZHU,Q.; ZHANG,G.L. 1994. GB/T 2677.8-1994. Beijing: Standards Press of

China:1-3.(in Chinese)

DAI,D.S. 2011. Fabrication, characterization and application of nanocellulose from hemp

fibres. Fuzhou: Fujian Agriculture and Forestry University, 1-120. (in Chinese)

GAO, J. 2008. GB/T 462-2008. Beijing: Standards Press of China:1-7. .(in Chinese)

GUO, N.W.; HE, J.X.; CUI, S.Z. 2012. Preparation of bamboo cellulose nanowhiskers.
Journal of Cellulose Science and Technology, 20(1): 58-61.(in Chinese)

KRISHNAMACHARI, P.; HASHAIKEH, R.; TINER, M. Modified cellulose morphologies

and its composites; SEM and TEM analysis[J]. Micron, 2011, 42: 751-761.

LIU, Z.M.; XIE, C.; FANG, G.Z.; et al. 2011. Morphology analysis of nano-microcrystalline
cellulose from eucalyptus pulp and cotton nanocrystalline cellulose. Biomass Chemical
Engineering, 45(2): 5-8. (in Chinese)

LIU, Z.M.; XIE, C.; FANG, G.Z.; et al. 2011. Preparation optimization and morphology
analysis of nanocrystalline cellulose from reed pulp. Chemistry and Industry of Forest
Products, 31(6): 87-90. (in Chinese)

LU,H.J.;WEN, H.L.; LIU, X. 2012. Study on preparation of nanocrystal cellulose by

ultrasonic-assisted acid. Journal of the Chinese Cereals and Oils Association, 27(4):
96-100.(in Chinese)

NIE, J.H. 2008. GB/T 742-2008. Beijing: Standards Press of China:1-6.(in Chinese)
PENG, Y.C.; GARDNER, D.J.; HAN, Y. Drying cellulose nanofibrils: in search of a suitable
method[J]. Cellulose, 2012, 19: 91-102.

SATYAMURTHY, P.; JAIN, P.; BALASUBRAMANYA, R.H.; et al. 2011. Preparation and
characterization of cellulose nanowhiskers from cotton fibres by controlled microbial
hydrolysis[J]. Carbohydrate Polymers, 83: 122-129.

SONG, X.Z.; WU, Q.L.; FU, F.; et al. 2011. Research progress of nanocrystalline cellulose
prepared from crops and agricultural residues. Transactions of the Chinese Society for
Agricultural Machinery, 42(11): 106-112. (in Chinese)

TANG, L.R.; HUANG, Biao; DAI, D.S.; et al. 2010. Optimum process conditions of
nanocellulose crystal and morphology characterization. Journal of Fujian College of Forestry,
30(1): 88-91. (in Chinese)

Paper PS-30 5 of 6
 Proceedings of the 55th International Convention of Society of Wood Science and Technology
August 27-31, 2012 - Beijing, CHINA

VORONOVA, M.I.; ZAKHAROV, A.G.; KUZNETSOV, O.Y.; et al. The effect of drying
technique of nanocellulose dispersions on properties of dried materials[J]. Materials letters,
2012, 68: 164-167.

XIAO,Q.; WAN, J.Q.; WANG, Y. 2009. CP/MAS 13CNMR spectroscopy study of the
ultrastructure of wood pulp fiber. Acta Chimica Sinica, 67(22): 2629-2634. (in Chinese)

YE, D.Y. 2007. Preparation of nanocellulose. Progress in Chemistry, 19(10): 1568-1575. (in
Chinese)

YUAN, Y.; FAN, Z.Q.; SHEN, Q. 2010. Recent development in nanocellulose research and
applicationⅠ. Polymer Bulletin, (2): 75-79. (in Chinese)

FAN, Z.Q.; YUAN, Y.; SHEN, Q. 2010. Recent development in nanocellulose research and
applicationⅡ. Polymer Bulletin, (3): 40-60. (in Chinese)

ZHEN, W.J.; SHAN, Z.H. 2008. Application of nanocellulose in green composites. Modern
Chemical Industry, 28(6): 85-88. (in Chinese)

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