Page 108 - 《精细化工》2020年第2期

第 38 卷第 2 期 精 细 化 工 Vol.38, No.2
202 1 年 2 月 FINE CHEMICALS Feb. 2021

功能材料
微晶纤维素的溶解及其阻燃性能

1
1*
来水利 ，张 昭 1,2 ，王 花
（1. 陕西科技大学 陕西省轻化工助剂重点实验室，陕西 西安 710021；2. 咸阳职业技术学院，陕西
咸阳 712000）

摘要：以氯代 1-氨甲酰甲基-3-乙烯基咪唑离子液体（[CmVIM]Cl）和四丁基氯化铵（TBAC）为溶剂，溶解微
晶纤维素（MCC），加入不同阻燃剂三聚氰胺磷酸酯（MP）、聚磷酸铵（APP）、纳米二氧化硅（SiO 2 ），制得了
阻燃纤维素复合材料。通过偏光显微镜观察 MCC 的溶解过程，并利用 FTIR、XRD、TGA 和 SEM 对再生 MCC
的结构、结晶度、热稳定性和形貌变化进行了表征。通过垂直燃烧、极限氧指数（LOI）和热重分析对纤维素复
合材料的阻燃性能进行了测试。结果表明，溶解温度为 90 ℃，TBAC 用量为[CmVIM]Cl 质量的 8%时，MCC
的溶解率达 6.3%，聚合度降至 505；与原 MCC 相比，再生 MCC 结晶度指数由 74.0%降至 46.4%，初始热分解
温度由 310 ℃降至 262 ℃，最大失重速率由 2.6%/min 降至 1.4%/min。MCC 表面由光滑平整的棒状结构转为凹
凸不平的不规则结构。当 MP、APP、SiO 2 质量分数分别为 5%、10%和 10%时，阻燃纤维素复合材料的极限氧
指数提升至 33.5%，垂直燃烧等级为Ⅴ-0。
关键词：离子液体；微晶纤维素；溶解率；结晶度；阻燃纤维素复合材料
中图分类号：TQ352；TB332 文献标识码：A 文章编号：1003-5214 (2021) 02-0310-07

Dissolution and flame retardancy of microcrystalline cellulose

1*
1
1,2
LAI Shuili , ZHANG Zhao , WANG Hua
（1. Shaanxi Key Laboratory of Chemical Additives for Industry, Shaanxi University of Science & Technology, Xi'an
710021, Shaanxi, China; 2. Xianyang Vocational & Technical College, Xianyang 712000, Shaanxi, China）

Abstract: Microcrystalline cellulose (MCC) was dissolved by chlorinated 1-carbamoylmethyl-3-vinyl
imidazole ionic liquid ([CmVIM]Cl) and tetrabutylammonium chloride (TBAC), and then different flame
retardants such as melamine phosphate (MP), ammonium polyphosphate (APP) and nano-silica (SiO 2) were
added to prepare flame retardant cellulose composites. The dissolution process of MCC was observed by
polarizing microscope. The structure, crystallinity, thermal stability and morphology change of regenerated
MCC were characterized by FTIR, XRD, TGA and SEM. The flame retardancy of cellulose composites was
tested by vertical combustion test, limiting oxygen index (LOI) and thermogravimetric analysis. The results
showed that the dissolution temperature was 90 ℃, TBAC was 8% of [CmVIM]Cl mass, the dissolution
rate of MCC was up to 6.3%, and the degree of polymerization was reduced to 505. Compared with those of
original MCC, the crystallinity index of regenerated MCC decreased from 74.0% to 46.4%, the initial
thermal decomposition temperature decreased from 310 ℃ to 262 ℃, and the maximum weight loss rate
decreased from 2.6%/min to 1.4%/min. The surface of MCC changed from smooth and flat rod structure to
uneven irregular structure. The LOI of the flame retardant cellulose composites containing 5%, 10% and
10% (mass fraction) of MP, APP and SiO 2 was up to 33.5%, and the vertical combustion level was Ⅴ-0.
Key words: ionic liquids; microcrystalline cellulose; dissolution rate; crystallinity; flame retardant cellulose
composite

收稿日期：2020-07-07; 定用日期：2020-09-28; DOI: 10.13550/j.jxhg.20200605
基金项目：陕西省科技攻关项目（2015SF266）
作者简介：来水利（1965—），男，教授，E-mail: lsl25206@163.com。联系人：王 花（1993—），女，硕士生，E-mail: wangh707@
163.com。