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机构地区:[1]华南理工大学化学与化工学院,广东广州510640
出 处:《精细化工》2009年第9期844-849,共6页Fine Chemicals
基 金:国家自然科学基金(20646003);广东省自然科学基金(07300767)~~
摘 要:以w(H2SO4)=64%的硫酸为催化剂,加入m(CuSO4)/m(纤维素)=0~3%的硫酸铜作助催化剂,水解脱脂棉,考察了制备纳米纤维素晶须(NCW)反应中反应温度、反应时间及硫酸铜加入量对纳米纤维素晶须产率、颗粒横截面直径、颗粒长度、颗粒长度与横截面直径之比和扫描电镜形貌的影响。结果表明,反应温度50℃、反应时间120min、催化剂投入量以m(CuSO4)∶m(纤维素)=1∶100为最佳工艺条件,纳米纤维素晶须对于脱脂棉的产率达58%左右,粒子的长径比为20~50,在原子力显微镜下观测到产品所成膜最高峰为27.95nm。加入了硫酸铜之后,缩短了反应时间,提高了反应效率和产率,减小了产物的颗粒直径,改善了纳米纤维素晶须的形状,因此,硫酸铜可以作为助催化剂有效地改善制备出的纳米纤维素晶须的形貌和尺寸分布。Nano-cellulose whiskers(NCW) were prepared from the absorbent cotton with 64% (by mass fraction) sulfuric acid used as catalyst and copper sulfate as cocatalyst. The effects of reaction time and temperature, the coeatalyst to cellulose ratio on the yield, the cross sectional diameter and length of NCW, the ratio of length and diameter of NCW, and the morphology of NCW by Scanning Electron Microscope were investigated. Experimental results showed that the optimal reaction temperature and time are 50 ℃ and 120 minutes respectively;and the optimal cocatalyst to cellulose ratio is m( CuSO4 ) :re(cellulose) = 1:100. The yield of NCW with the absorbent cotton is about 58%. The length to diameter ratio of whiskers ranges from 20 to 50, while the peak height of NCW film observed by Atomic Force Microscope is 27.95 nm. NCW with the better modified morphology and smaller size can be produced in a shorter time when an appropriate amount of copper sulfate was used, in case that the yield of NCW and the reaction efficient increased. It is proved that copper sulfate can be used as a cocatalyst to modify the morphology and size distribution of NCW.
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