淀粉烷基糖苷的制备及其理化性质

Synthesis and Physicochemical Property of Starch-based Alkyl Polyglycoside

通过L9(34)正交试验法优化了以玉米淀粉和马铃薯淀粉为原料用转糖苷化法制备淀粉烷基糖苷(Alkyl polyglycoside,APG)的制备工艺,得到制备淀粉APG的最适宜条件为:以m次亚磷酸钠∶mEDTA∶m对甲苯磺酸=2∶1∶(6～9)配比组成的复合物为催化剂、糖苷化温度为120～125℃、m淀粉∶m催化剂=1∶0.015～0.016、m玉米淀粉∶m乙二醇∶m十二醇=6∶1∶0.75、m马铃薯淀粉∶m乙二醇∶m十二醇=4∶1∶0.25;减压蒸馏脱醇的条件是:压力0.1 MPa,温度130℃/135℃(低碳醇)1、50℃/165℃(高碳醇),携带剂应预热至120℃且待反应体系温度达到120℃时加入为宜。在此工艺条件下总糖苷得率≥135%,且APG产品与标准品的红外光谱图(Infrared spectroscopyI,R)一致;性能试验测得APG的表面张力29.25 mN.m-1,临界胶束浓度(Critical micelle concentration,CMC)0.80%,亲水亲油平衡值(Hydrophile-lipophile balance,HLB)15.43,pH 11～12,泡沫性好。各项性能和品质指标基本优于市售APG,且各项技术指标均符合GB/T 19464—2004的要求。

The L9 （3^4） orthogonal experimental method was adopted to optimize the synthesis technique that the alkyl polyglycoside （APG） was synthesized by trans - glycosidation of potato or corn starch, so that the optimum con- ditions for synthesis of starch APG were obtained as follows： catalyst of the compound composed by the mix ratio of mSoaium hypophosphite： mEDTA： mparatoluenfonic acid =2： 1：（6 -9）, glycosidation temperature 120 - 125 ℃, mstarch： mcatalyst = 1： 0. 015 - 0. 016, m tarch： methylene glycol： mdodecanol = 6 ： 1 ： 0.75 or mpotato starch ： methylene glycol ： mdod 1 = 4 ： 1 ： 0. 25. The conditions for vacuum distillation and dealchoholization were as follows： pressure： 0.1 Mpa; temperature： 130 ℃/ 135 ℃ （low -carbon alcohol） or 150 ℃/165 ℃ （high -carbon alcohol） ; carried agents should be preheated to 120 ℃ and added after the temperature of reaction system rose up to 120 ℃. Under the said technical conditions, the yield of total glycoside was≥ 135%, and APG products and standard products had the same infrared spectroscopy （IR）. In the process of performance test, it was determined that APG surface tension was σ = 29.25 mN· m^ - 1, the critical micelle concentration （CMC） was 0.80%, the hydrophile - lipophile balance （HLB） was 15.43, pH was 11 - 12 and the spumescence was in good condition. So, various performance and quality indices were basically superior to APG sold in the market and all technical indices met the requirements of GB/T 19464--2004.