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.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
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)
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
cassava starch
ethanol solvent
crosslinked octenyl succinic anhydride cassava starch ester
non-crystallization
relative crystaUinity
