研磨强化无溶剂法合成蔗糖脂肪酸酯  

Grind-strengthened Solvent-free Synthesis of Sucrose Fatty Acid Esters

作　　者：李媛 陈佳志 麦裕良 陈晓填 高敏杰 LI Yuan;CHEN Jia-zhi;MAI Yu-liang;CHEN Xiao-tian;GAO Min-jie(Guangdong Provincial Key Laboratory of Industrial Surfactant,Guangdong Research Institute of Petrochemical and Fine Chemical Engineering,Guangzhou 510665,Guangdong,China)

机构地区：[1]广东省工业表面活性剂重点实验室广东省石油与精细化工研究院,广东广州510665

出　　处：《精细化工》2019年第1期118-123,共6页Fine Chemicals

基　　金：广东省科学院实施创新驱动发展能力建设专项(2017GDASCX-0855;2017GDASCX-0705);国家自然科学基金(21703042);广州市科学研究计划重点项目(201804020004)~~

摘　　要：以蔗糖和脂肪酸甲酯为反应原料,无溶剂条件下采用研磨强化的方法合成了蔗糖脂肪酸酯(即蔗糖酯),考察了研磨时间、乳化剂用量、反应时间、反应压力以及催化剂用量对蔗糖酯收率及脂肪酸甲酯转化率的影响,产品经水洗、醇提精制后,用FTIR和HPLC-ELSD对其进行了表征和分析。结果表明:研磨处理能将反应分散物粒径(D50)降至约5μm,有效地增强了蔗糖与脂肪酸甲酯的无溶剂酯交换反应。得到的最优反应条件为:研磨时间为60min,硬脂酸钾乳化剂质量分数为10%(占体系总质量,下同),K2CO3质量分数为2.0%,反应时间6 h,反应压力0.5 kPa,在该条件下脂肪酸甲酯转化率为91.2%,蔗糖酯收率为61.6%。精制后产品中蔗糖酯质量分数为81.9%,且其游离糖质量分数为0.6%,酸值为3.0mgKOH/g,水分(质量分数)为0.2%和灰分(质量分数)为0.5%,均达到FAO/WHO标准。A grind-strengthened strategy was developed for the solvent-free synthesis of sucrose fatty acid esters(SE).The effects of grinding time,emulsifier,reaction time,reaction pressure and catalyst dosage on the yields and production distributions of SE and the conversion of fatty acid methyl ester were investigated.After the generated SE was purified by using water washing and alcohol extraction,the obtained product was characterized by Fourier transform infrared spectroscopy(FTIR) and high performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD).The results showed that the grinding pretreatment could reduce the particle size of reaction dispersion(D50) to 5 μm and effectively enhanced the solvent-free transesterification reaction of sucrose esters.Under the optimized conditions,a fatty acid methyl ester conversion of 91.2% and a SE yield of 61.6% were achieved,in which the grinding time was 60 min,the mass fraction of potassium stearate was 10%(based on the total mass of the system,the same below),the mass fraction of potassium carbonate was 2.0%,the reaction pressure was 0.5 kPa,and the reaction time was 6 h.After purification,the mass fraction of SE reached up to 81.9%,and its free sugar content was 0.6%(mass fraction),acid value was 3.0 mg KOH/g,water content was 0.2%(mass fraction),ash content was 0.5%(mass fraction).All these indicators completely accorded with the Food and Agriculture Organization/World Health Organization(FAO/WHO) standard.

关 键 词：蔗糖脂肪酸酯 机械化学 无溶剂法合成 酯交换 碱催化 日化原料 

分 类 号：TQ225.1[化学工程—有机化工]