干法制木薯淀粉磷酸酯及其反应机理研究
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摘要
淀粉磷酸酯是原淀粉与磷酸盐发生酯化反应而生成的一种淀粉衍生物,现在应用的大多数是结合磷量较低的淀粉磷酸酯,产品附加值较低。在新闻纸与食品这两个领域中,使用的淀粉磷酸酯都要求具有较高结合磷含量,而且需求量较大,开发出适用于这两个领域的高结合磷的淀粉磷酸酯,将进一步拓宽淀粉磷酯酯的应用前景。
     本文分别用三聚磷酸钠和磷酸二氢钠为酯化剂,考察干法制备木薯淀粉磷酸单酯的反应条件,研究了反应温度、反应时间、pH值、酯化剂用量和催化剂用量对产物取代度和反应效率的影响规律。在本实验选择的实验条件范围内,以三聚磷酸钠为酯化剂的适宜的反应条件为:反应温度130~150℃,反应时间1.5~2h,pH值5左右,三聚磷酸钠用量7%~9%,尿素用量4%~5%,取代度和反应效率可高达0.075、61.60%以上;以磷酸二氢钠为酯化剂的适宜的反应条件分别为:反应温度150~160℃,反应时间2~2.5h,pH值为5.8,磷酸二氢钠用量为9%,尿素用量为6%。在这些条件下,取代度最
    
    广西大学硕士学位论文
    干法制备木薯淀粉磷酸醋及结构性质研究
    高可达0.093,此时反应效率为68.73%。
     同时,在单因素实验的基础上,以取代度为指标,选取反应温
    度、反应时间、pH值、酉旨化剂用量和尿素用量为因素,进行五因素
    六水平均匀设计实验,并对实验数据进行统计分析,建立数学回归
    模型。
     对产物的流变特性进行研究,得出各个反应条件下的流变模型。
    用红外光谱对醋化反应产物进行结构分析,说明变性处理后的淀粉
    并未破坏原淀粉的基本结构,酉旨化反应只是在原来的淀粉分子链上
    增加了新的基团。
Starch phosphate ester is one kind of starch derivative produced from esterification of starch and phosphate. Starch phosphate ester which is being applied usually has lower combined phosphorus content, or lower degree of substitution and lower accessional value. Now it is applied in the fields of newspaper and food industry with high demands and required to have a higher combined phosphorus content. So the studies on synthesis of starch phosphate ester and its reaction mechanism would become more and more important and widen their perspective application.
    In this paper, reactive conditions of preparation of cassave starch phosphate ester using STP and NaH2PO4 as esterify reagent were studied. The influence factors including reaction temperature, reaction time, the value pH, the amount of esterify reagent and the amount of urea were also studied. The results show that the optimum reaction conditions using STP to prepare starch phosphate ester under the dry process are that the reaction temperature is 130~150C, reaction time 1.5~2h, pH 5, amount of STP 7%~9%, and amount of urea 4%~5%, respectively. Under the optimal conditions, the DS is 0.075 and the RE is 61.60%. The optimum reaction conditions using NaH2PO4 to prepare starch phosphate ester under the dry process are that the reaction temperature is 150~160C, reaction time 2~2.5h, pH 5.8, amount of NaH2PO4 9%, and amount of urea 6%, respectively. Under the optimal conditions, the DS is 0.093 and the RE is 68.73%.
    On the base of single factor experiment, even design experiment was designed under five factors and six levels, the factors including reaction temperature, reaction time, the value pH, amount of esterify reagent and the amount of urea, then analyzing the data and setting up the maths model.
    
    
    
    
    Rheological property of products was studied, the rheological model of different reactive conditions established. FTIR of starch phosphate ester showed that the basic structure of the modified starch wasn't destroyed, and the new groups were added to the origin starch molecule.
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