非晶交联辛烯基琥珀酸淀粉酯的制备与结构表征  

Preparation and Structure Characterization of Non-crystal Crosslinked Octenyl Succinic Anhydride Starch

作　　者：陆来仙[1,2] 童张法[1] 石海信[2] 张友全[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]钦州学院化学化工学院,广西钦州535000

出　　处：《高校化学工程学报》2014年第6期1315-1321,共7页Journal of Chemical Engineering of Chinese Universities

基　　金：广西自然科学基金重点项目(2011GXNSFD018013);广西自然科学基金资助项目(2013GXNSFAA019023);广西教育厅科研项目(201106LX540)

摘　　要：以木薯淀粉为原料,三偏磷酸钠(STMP)和辛烯基琥珀酸酐(OSA)为变性剂,用乙醇溶剂法合成非晶交联辛烯基琥珀酸淀粉酯(N-COSAS)。以结合磷含量(CP)、取代度(DS)、黏度(η)为评价指标,探讨STMP用量(占淀粉干基的质量分数),交联时间、交联温度、交联p H值和酯化时间、酯化温度、酯化p H值等因素对CP或DS和η的影响。通过单因素和正交试验,得出制备低黏度N-COSAS的较佳工艺条件:在加入STMP 1.5%时,交联反应的时间、温度和p H值分别为4 h,45℃和10.0,酯化反应的时间、温度和p H值分别为3 h、35℃和8.5。扫描电镜观察显示N-COSAS颗粒表面有明显裂痕,表面被卷起;X射线衍射图谱显示,N-COSAS的相对结晶度为8.24%,晶型属于V型;红外光谱显示,N-COSAS在1570.06 cm–1处出现新的吸收峰,在929.69 cm–1处峰的强度增加,证明在淀粉分子中引入了辛烯基琥珀酸基团和交联键。Abstract： Non-crystal crosslinked octenyl succinie anhydride starch ester （N-COSAS） was prepared in ethanol solvent using cassava starch as a raw material, sodium trimetaphosphate （STMP） and octenyl succinic anhydride （OSA） as denaturants. The effects of the amount of STMP, cross-linking time, temperature and pH on the combined phosphorus （CP） and viscosity （11） and esterification temperature, time and pH on the degree of substitution （DS） and q of N-COSAS were studied respectively. The efficient process conditions for preparation of low viscosity N-COSAS were obtained based on single factor experiment and orthogonal experiment. When the amount of STMP added equals to 1.5% of the mass of starch, the cross-linking time, temperature and pH are 4 h, 45 ~C, and 10.0, respectively, and the esterification time, temperature and pH are 3 h, 35 ~C and 8.5, separately. Results from scanning electron microscopy （SEM） showed that the surface of N-COSAS is obviously cracked and rolled up. X-ray diffraction （XRD） suggests that relative crystallinity of N-COSAS is 8.24%, and a V-type crystalline structure is formed. The new absorption peak appeared in the Fourier transform infrared spectroscopy （FT-IR） is 1570.06 cm-1, proving that the groups of octenylsuccinate are introduced into the starch molecules. The absorption peak at 929.69 crn-1 is strengthened, confirming that cross-linking bond is formed.

关 键 词：木薯淀粉 乙醇溶剂法 交联辛烯基琥珀酸淀粉酯 非晶化 相对结晶度 

分 类 号：TS235.2[轻工技术与工程—粮食、油脂及植物蛋白工程] TS201.7[轻工技术与工程—食品科学与工程]