双活性磺酸基蔗渣木聚糖邻苯二甲酸酯的合成与表征  

Synthesis and Characterization of Dual Active Sulfonic Groups Bagasse Xylan Phthalate

作　　者：李和平[1] 武冠亚 杨旭[1] 袁金伟[1] 孙彦[1] 邹英东 Li Heping;Wu Guanya;Yang Xu;Yuan Jinwei;Sun Yan;Zou Yingdong

机构地区：[1]桂林理工大学化学与生物工程学院,广西桂林541004

出　　处：《化学反应工程与工艺》2016年第2期144-151,共8页Chemical Reaction Engineering and Technology

基　　金：国家自然科学基金(21466010)

摘　　要：以蔗渣木聚糖为主要原料,经两步酯化反应合成磺酸基蔗渣木聚糖邻苯二甲酸酯,考察反应条件对合成反应的影响,并通过红外光谱(FT-IR)、X射线衍射(XRD)、热重分析(TG-DTG)和扫描电镜(SEM)对蔗渣木聚糖经双酯化改性前后的样品进行表征。结果表明,较优的反应条件为:第一步以邻苯二甲酸酐为羧酸酯化剂,三乙胺为催化剂,在三乙胺与N,N-二甲基甲酰胺体积比为1:16,蔗渣木聚糖单元和邻苯二甲酸酐物质的量之比为1:2时,于80℃下反应4 h,经催化羧酸酯化合成单活性蔗渣木聚糖邻苯二甲酸酯;第二步以氨基三磺酸钠为酯化剂,在碱性条件下,蔗渣木聚糖邻苯二甲酸酯与NaNO_2的质量比为1:2时,于50℃下反应4 h,合成了双活性磺酸基蔗渣木聚糖邻苯二甲酸酯。双酯化后的磺酸基蔗渣木聚糖邻苯二甲酸酯的热稳定性增强,其分子表面形貌更加紧密。The sulfonic groups bagasse xylan phthalate was synthesized by two steps of esterification usingbagasse xylan as the raw material. The effects of reaction conditions were investigated and the optimalconditions were obtained. The samples were characterized by infrared spectroscopy(FT-IR), X-raydiffraction (XRD), thermal gravimetric analysis (TG-DTG) and scanning electron microscopy (SEM) beforeand after double esterification of the bagasse xylan. The single active bagasse xylan phthalate wassynthesized in the first step by catalytic esterification with phthalic anhydride as carboxylic acidesterification agent and triethylamine as the catalyst with the volume ratio of triethylamine to DMF 1:16, themolar ratio of bagasse xylan unit to phthalic anhydride 1:2, the reaction temperature 80 ℃ and the reactiontime 4 h. The dual active sulfonic groups bagasse xylan phthalate was synthesized in the second step underalkaline conditions using sodium nitrilotriacetic sulfonate as the sulfonation agent with the mass ratio ofbagasse xylan to NaNO2 1:2, the reaction temperature 50 ℃ and reaction time 4 h. The characterization results showed that the thermal stability of sulfonic groups bagasse xylan phthalate was enhanced, and themolecular surface morphology of the dual esterified derivative showed more closely.

关 键 词：磺酸基蔗渣木聚糖邻苯二甲酸酯 合成 双活性衍生物 蔗渣木聚糖 

分 类 号：O621.25[理学—有机化学]