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第 36 卷第 1 期                             精   细   化   工                                  Vol.36, No.1
             201 9 年 1 月                             FINE CHEMICALS                                 Jan.  2019


              医药与日化原料
                            研磨强化无溶剂法合成蔗糖脂肪酸酯



                                                     *
                                 李   媛,陈佳志 ,麦裕良,陈晓填,高敏杰
                       (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)


                 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(D 50 )降至约 5  μm,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 60 min,硬脂酸钾乳化剂质量分数为 10%(占体系总质量,下同),K 2 CO 3 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 3.0 mg KOH/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。
                 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
                 中图分类号:TQ225.1      文献标识码:A      文章编号:1003-5214 (2019) 01-0118-06



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


                                                 *
                             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)


                 Abstract: 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 (D 50) 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.
                 Key words: sucrose fatty acid ester; mechanochemistry; solvent-free synthesis; transesterification; alkali
                 catalysis; cosmetic materials
                 Foundation items: Guangdong Academy of Sciences (GDAS) Special Project of Science and Technology
                 Development (2017GDASCX-0855, 2017GDASCX-0705); National Natural Science Foundation of China

                 收稿日期:2018-04-10;  定用日期:2018-08-10; DOI: 10.13550/j.jxhg.20180257
                 基金项目: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)
                 作者简介:李   媛(1991—),女,硕士。联系人:陈佳志(1987—),男,博士,电话:020-37276448,E-mail:chenjiazhi@gdcri.com。
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