共沉淀法制备木质素/纳米纤维素杂化颗粒及其形貌调控  

Preparation of lignin/nanocellulose hybrid particles by co-precipitation method

作　　者：李豪 郭娆 田雪 樊亚博 王成毓[1] 宦思琪 LI Hao;GUO Rao;TIAN Xue;FAN Yabo;WANG Chengyu;HUAN Siqi(College of Materials Science and Engineering,Northeast Forestry University,Harbin 150040,China)

机构地区：[1]东北林业大学材料科学与工程学院,哈尔滨150040

出　　处：《林业工程学报》2024年第5期107-114,共8页Journal of Forestry Engineering

基　　金：国家自然科学基金(32301513)。

摘　　要：纤维素和木质素是自然界中储量最丰富的可再生资源,受天然木材中纤维素和木质素的共生互缠绕结构启发,以林木生物质微纳米基元重组多维新材料为目的,研究并探索木质素/纤维素杂化颗粒的制备及应用,是提高和拓展林木生物质高值化利用的有效手段之一。本研究基于溶解-沉降的方法,分别采用四氢呋喃和无水乙醇溶解硫酸盐木质素,再向其溶液中瞬时加入纤维素纳米纤维(CNF)悬浮液,使木质素溶液迅速产生相分离;在实现木质素微纳米球(LNS)制备的同时,混合纳米纤维素,一步法制备稳定且均匀分散的LNS/CNF杂化颗粒;探讨了不同溶剂、不同质量分数CNF悬浮液以及不同滴加速率对所得LNS/CNF杂化颗粒悬浮液稳定性、颗粒微观形貌、尺寸、表面张力以及成膜特性的影响。实验结果表明:硫酸盐木质素在不同溶剂中的溶解行为差异及CNF悬浮液的质量分数和滴加速率,都会影响其杂化颗粒的稳定性、形貌和尺寸,使用四氢呋喃处理所得LNS/CNF杂化颗粒的尺寸形貌更为均一;反应的最佳CNF质量分数为0.5%,所得LNS/CNF杂化颗粒的尺寸大小最为均匀;通过控制滴加速度,能有效调控所得颗粒的尺寸,实现LNS的可控制备,在CNF质量分数一定的情况下,滴加速度越快,所制备的LNS/CNF纳米杂化颗粒和所得薄膜的性能也越好。As natural energy sources,cellulose and lignin are the most abundant renewable resources in nature.Inspired by the symbiotic and entangled structure of cellulose and lignin in natural wood,the research and exploration of lignin/cellulose hybrid particles aim at recombining multi-dimensional new materials based on the micro-nano elements of forest biomass,which is one of the effective means to enhance and expand the high-value utilization of forest biomass.Based on the dissolution-precipitation method,this study used two solvents,tetrahydrofuran,and anhydrous ethanol,to dissolve lignin sulfonate separately.Cellulose nanofiber(CNF)suspension was then instantly added to the solution,causing phase separation in the lignin solution,and achieving rapid preparation of lignin micro-nanospheres(LNS),while mixing with nano cellulose to prepare stable and uniformly dispersed LNS/CNF hybrid particles in one step.The effects of different solvents,different CNF concentration suspensions and different drop rates on the stability,particle morphology,size,surface tension and film formation properties of LNS/CNF hybrid particle suspensions were discussed.The characterization of LNS/CNF hybrid particles and the obtained films included following procedures:the size and microstructure of LNS and CNF were observed by atomic force microscopy(AFM),20 samples were selected from the AFM diagram of LNS and CNF,respectively,and their sizes were measured and analyzed manually.The LNS/CNF suspension prepared with tetrahydrofuran(CNF mass ratio was 0.5%)was diluted to 1/10000,and the solution of uranyl acetate was added for staining.After the ultrasound treatment,the suspension was added to carbon net for drying,and then characterized by the transmission electron microscopy(TEM).Scanning electron microscopy(SEM)was used to observe and verify the microstructure of LNS/CNF hybrid particles and the obtained films.The surface tension of LNS/CNF hybrid particle suspensions prepared by different methods was measured by an optical contact angle measu

关 键 词：木质素 纤维素 相分离 杂化颗粒 薄膜 

分 类 号：TQ35[化学工程] TB332[一般工业技术—材料科学与工程]