应用响应面分析法优化“一锅法”制备乙酰化纳米纤维素

Optimization of preparation process for acetylated nanocrystalline cellulose via one-pot reaction with response surface methodology

以竹人纤浆为原料,4-二甲氨基吡啶（DMAP）为催化剂,采用机械力化学法制备纳米纤维素并同时进行乙酰化,探索一锅法制备乙酰化纳米纤维素（A-NCC）的较佳工艺,并应用响应面分析法对影响乙酰化纳米纤维素得率的4个主要因素进行优化.得到优化的较佳工艺条件为：球磨时间2h、反应温度120℃、超声时间3h、反应时间5h,此时A-NCC的得率为42.76%.滴定法测得的A-NCC取代度在0.125-0.214之间,通过XRD和FTIR分析表明,机械力化学法制备得到的产物含特征官能团羰基,且结晶度较高.

To optimize the manufacture procedure for nanocrystalline cellulose （ NCC） that preparation and modification can be carried out simultaneously,bamboo pulp was milled into nanocellulose,and followed by being acetylated in mechanochemical method with 4-dimethylaminepyride （DMAP） as catalyst Four main factors,including milling time,reaction temperature and time,and ultrasonic, were investigated via response surface methodology. Results showed that with milling time,reaction temperature, ultrasonic-time and reaction time being 2 h,120℃,3 h and 5 h, respectively, A - N C C yield optimized at 4 2 . 7 6 %,with substitution degree of bamboo pulp ranging from 0.125 to 0.214. Further-nore,X-ray diffraction and Fourier transform infrared spectroscopy analysis confimied that A-NCC manufactured in this approach contained characteristic functional groups of carbonyl and demonstrated high crystallinity.