纤维素酯基固—固相变材料的制备与性能研究
发布时间：2018-09-01 17:16
【摘要】：纤维素作为一种绿色环保的可再生资源,无毒无害、来源丰富、可生物降解、廉价、生物相容性好。但因为分子内和分子间的氢键作用,纤维素的分解温度低于熔融温度,不能实现熔融加工,且不溶于常用有机溶剂。本论文首先以微晶纤维素为原料,在1-烯丙基-3-甲基咪唑氯盐([Amim]Cl)离子液体或1-乙基-3-甲基咪唑醋酸盐([Emim]Ac)/N,N-二甲基乙酰胺(DMAc)体系中溶解纤维素并接枝苯甲酰氯(BC),运用了傅里叶变换红外(FTIR)、核磁共振氢谱(1H-NMR)、差示扫描量热法(DSC)、热重分析(TG)、热台显微镜(POM)以及溶解性等测试仪器和表征方法,探究了在一定反应时间内不同含量的BC、不同反应温度下制备的纤维素苯甲酸酯(CB)的性能。以CB为反应单体,以二乙二醇正十六烷基醚(E2C16)为功能物质制备纤维素苯甲酸酯-g-二乙二醇正十六烷基醚(CB-g-E2C16)固-固相变材料。探究了不同反应温度(70℃-110℃)、不同投料比(E2C16:AGU=2:1-8:1 mol%)等反应参数对产物结构与性能的影响。当CB(DS=0.12)的取代度较低时,CB不具有热塑性,随着取代度增加,CB开始出现玻璃化转变温度(143.2℃-182.1℃);并且DS越大,玻璃化转变温度越低。相比较于微晶纤维素,取代度较低的CB(DS=0.13-1.05)的热稳定性有所下降,取代度较高(DS=2.80)时,CB的热力学稳定性比纤维素高。所制备的CB(DS=0.13-2.98)均能溶解于DMSO和DMF等极性溶剂,具有较高取代度的CB(DS=2.80-2.98)可溶解于DMSO和DMF等极性溶剂的同时也能溶解于丙酮;在热台显微镜下,取代度达到一定值的CB(DS=1.05)具有熔融的迹象。DS为0.68-1.24的CB-g-E2C16固-固相变材料具有7 J/g-24 J/g的相变焓,热稳定性优良,起始分解温度为280℃-300℃,峰值分解温度为320℃-340℃,且均能溶解于DMSO和DMF等极性溶剂。在热台显微镜下,70℃-110℃的反应温度下制备的CB-g-E2C16共聚物在30℃-250℃没有熔融,表现为固-固相变。
[Abstract]:As a kind of green renewable resource, cellulose is non-toxic and harmless, rich in sources, biodegradable, cheap, and has good biocompatibility. However, due to the intermolecular and intramolecular hydrogen bonding, the decomposition temperature of cellulose is lower than the melting temperature, which can not realize melting processing and is insoluble in common organic solvents. In this paper, microcrystalline cellulose was used as raw material. The Fourier transform infrared (FT-IR) (FTIR), spectroscopy was used to dissolve cellulose and graft benzoyl chloride (BC), into 1-allyl-3-methylimidazolium chloride ([Amim] Cl) ionic liquid or 1-ethyl-3-methylimidazolium acetate ([Emim] Ac) / (DMAc) system. (1H-NMR), differential scanning calorimetry (DSC), thermogravimetric analysis, (TG), thermogravimetric analysis, (POM), solubility and other testing instruments and characterization methods, The properties of cellulose benzoate (CB) prepared at different reaction temperature with different content of BC, in a certain reaction time were investigated. Cellulose benzoate -g- diethylene glycol cetyl ether (CB-g-E2C16) was prepared by using CB as reaction monomer and diethylene glycol cetyl ether (E2C16) as functional substance. The effects of different reaction temperature (70 鈩，
本文编号：2217852
[Abstract]:As a kind of green renewable resource, cellulose is non-toxic and harmless, rich in sources, biodegradable, cheap, and has good biocompatibility. However, due to the intermolecular and intramolecular hydrogen bonding, the decomposition temperature of cellulose is lower than the melting temperature, which can not realize melting processing and is insoluble in common organic solvents. In this paper, microcrystalline cellulose was used as raw material. The Fourier transform infrared (FT-IR) (FTIR), spectroscopy was used to dissolve cellulose and graft benzoyl chloride (BC), into 1-allyl-3-methylimidazolium chloride ([Amim] Cl) ionic liquid or 1-ethyl-3-methylimidazolium acetate ([Emim] Ac) / (DMAc) system. (1H-NMR), differential scanning calorimetry (DSC), thermogravimetric analysis, (TG), thermogravimetric analysis, (POM), solubility and other testing instruments and characterization methods, The properties of cellulose benzoate (CB) prepared at different reaction temperature with different content of BC, in a certain reaction time were investigated. Cellulose benzoate -g- diethylene glycol cetyl ether (CB-g-E2C16) was prepared by using CB as reaction monomer and diethylene glycol cetyl ether (E2C16) as functional substance. The effects of different reaction temperature (70 鈩，
本文编号：2217852
本文链接：https://www.wllwen.com/kejilunwen/cailiaohuaxuelunwen/2217852.html
