Page 146 - 《精细化工》2020年第6期
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第 37 卷第 6 期                             精   细   化   工                                  Vol.37, No.6
             202 0 年 6 月                             FINE CHEMICALS                                 June    2020


              催化与分离提纯技术
                         SnO 负载硅钨酸催化制备月桂酸单甘酯
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                       缪艳丽 ,徐   超 ,丁雨茜 ,梅星雨 ,韩晓祥 ,唐秀娟
                 (1.  浙江工商大学  食品与生物工程学院  浙江  杭州    310018;2.  浙江工商大学  环境科学与工程学院  浙江
                 杭州    310018)
                 摘要:以金属氧化物、硅钨酸为原料,采用浸渍法合成了系列金属氧化物负载硅钨酸催化剂。通过 FTIR、XRD、
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                 TGA-DTG、BET 及固态 P MAS NMR 表征技术对催化剂的结构、热稳定性、表面形貌及酸性进行了表征与测
                 试。考察了该系列催化剂在月桂酸单甘酯(GML)制备中的催化性能。结果表明,20HSiW/SnO 2 〔即 20%
                 H 4 SiW 12 O 40 /SnO 2 ,20%表示硅钨酸的含量(以 H 4 SiW 12 O 40 和 SnO 2 总质量为基准,下同),缩写为 20HSiW/SnO 2 ,
                 下同〕催化剂显示出较好的催化性能,这归因于较强的 Brønsted 酸性及硅钨酸(Brønsted)与载体(Lewis)间
                 的酸性协同效应。以 20HSiW/SnO 2 为催化剂,在 n(甘油)∶n(月桂酸)=5∶1、20HSiW/SnO 2 催化剂用量为月桂酸
                 质量的 7%、反应时间 3 h、反应温度 423 K 条件下,月桂酸转化率为 91.4%,GML 产率为 78.9%;20HSiW/SnO 2
                 催化剂显示出较好的重复使用性能,经 5 次循环利用后,GML 的产率为 73.6%;动力学研究表明,20HSiW/SnO 2
                 催化制备 GML 反应活化能为 33.02 kJ/mol。
                 关键词:金属氧化物;硅钨酸;催化剂;酯化反应;GML;动力学;催化技术
                 中图分类号:O614.4;O643.32      文献标识码:A      文章编号:1003-5214 (2020) 06-1212-09



                              Preparation of monoglyceride laurate catalyzed by
                                      silicotungstic acid supported on SnO 2


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                     MIAO Yanli , XU Chao , DING Yuxi , MEI Xingyu , HAN Xiaoxiang , TANG Xiujuan
                 (1. School of Food and Biotechnology, Zhejiang Gongshang University, Hangzhou 310018, Zhejiang, China; 2. School
                 of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310018, Zhejiang, China)
                 Abstract:  A  series  of  catalysts  were  synthesized  by  impregnation  method  from  metal  oxide  and
                 silicotungstic  acid.  The  structure,  thermal  stability,  surface  morphology  and  acidity  of  the  catalysts
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                 were  characterized  and  tested  by  FTIR,  XRD,  TGA-DTG,  BET  and  solid-state  P  MAS  NMR.  The
                 catalytic  performances  of  the  catalysts  for  the  preparation  of  monoglyceride  laurate  (GML)  were
                 investigated. The results showed that 20HSiW/SnO 2  〔That is, 20%H 4SiW 12O 40/SnO 2, and 20% represents
                 the content of silicotungstic acid (based on the total mass of H 4SiW 12O 40 and SnO 2, the same below)〕
                 catalyst exhibited better catalytic performance, which was attributed to strong  Brønsted  acidity  and  the
                 acid synergistic effect between silicotungstic acid (Brønsted acid) and support (Lewis acid). Under the
                 optimal conditions of n(glycerol)∶n(lauric acid)=5∶1, dosage of 20HSiW/SnO 2 catalyst 7% (based on
                 the mass of lauric acid), reaction time 3 h and reaction temperature 423 K, the conversion of lauric acid
                 was 91.4%, and the yield of GML was 78.9%, respectively. The yield of GML could still reach 73.6%
                 after 20HSiW/SnO 2 catalyst was reused 5 times, indicating that the catalyst had excellent reusability.
                 Kinetic studies confirmed that the activation energy of GML prepared by 20HSiW/SnO 2 catalyst was
                 33.02 kJ/mol.
                 Key  words:  metal  oxide;  silicotungstic  acid;  catalyst;  esterification;  monoglyceride  laurate;  kinetics;
                 catalysis technology

                 收稿日期:2019-12-20;  定用日期:2020-03-20; DOI: 10.13550/j.jxhg.20191184
                 基金项目:国家重点研发计划(2018YFD0400600);国家级大学生创新创业训练计划项目(GJ201910002)
                 作者简介:缪艳丽(1999—),女,本科生,E-mail:1848870713@qq.com。联系人:韩晓祥(1974—),男,副研究员,硕士生导师,
                 E-mail:hxx74@126.com。
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