该文以丰都红心柚的中果皮为原料,采用硫酸水解法制备柚皮纳米纤维素(nano-crystal cellulose, NCC)。以H2SO4浓度、反应温度、反应时间对得率的影响进行单因素试验和响应面优化分析,并对制备出的纳米纤维素结构进行扫描电镜、红外光谱和X-射线衍射等分析。在H2SO4质量分数为62%、反应温度为50℃、反应时间为78 min的条件下制备出的NCC得率最高,为63.27%。通过扫描电镜观察得知柚皮NCC呈类球状结构均匀分布,粒径在100~200 nm;由红外光谱和X射线衍射鉴定出样品为纤维素Ⅰ型结构,结晶度达到53.75%。相较于柚皮微晶纤维素(microcrystalline cellulose,MCC),制备出的NCC具有更规则的结构、更大的比表面积和更高的结晶度,使柚皮纤维素具有了更高的应用价值。
In order to develop the processing and pomelo peel utilization, and to increase the added value, nano-crystal cellulose (NCC) of pomelo peel was prepared by hydrolysis of sulfuric acid from the mesocarp of Fengdu red heart pomelo. The effects of sulfuric acid concentration, reaction temperature and reaction time on the yield were investigated by single factor experiment. On the basis of this, the response surface method was used to determine the optimal process parameters, and the prepared nano-cellulose structure was analyzed by scanning electron microscopy, infrared spectroscopy and X-ray diffraction. The results showed that the optimal conditions for the preparation of pomelo nano-cellulose were sulfuric acid mass fraction of 62%, reaction temperature of 50°C, reaction time of 78 min, contributing to the highest NCC yield of 63.27%. Scanning electron microscopy indicated that the NCC of the pomelo mesocarp showed a spheroidal structure with particle size between 100 nm and 200 nm, and the size distribution was uniform. The sample was identified by infrared spectroscopy as cellulose 2 structure with the crystallinity index of 53.75%. Compared with the microcrystalline cellulose (MCC), NCC has a more regular structure, a larger specific surface area and a higher crystallinity, which ensures a high application value of pomelo peel.
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