Page 145 - 《精细化工》2023年第5期
P. 145

第 40 卷第 5 期                             精   细   化   工                                  Vol.40, No.5
             20 23 年 5 月                             FINE CHEMICALS                                 May  2023


              催化与分离提纯技术
                              聚对苯乙烯磺酸微球的绿色制备及


                                            催化合成生物柴油



                                                                       2
                                             2
                                                          2
                                                                                   2
                                                                                                2*
                                1
                       张春燕 ,苏佳俊 ,尹   惠 ,姚晨曦 ,肖   俊 ,罗建新
                 (1. 湖南工学院  化学与环境工程学院,湖南  衡阳  421002;2.  湖南工学院  材料科学与工程学院,湖南
                 衡阳  421002)
                 摘要:以水为介质、苯乙烯(St)为基体单体、二乙烯苯(DVB)为交联单体、对苯乙烯磺酸钠(NaSS)为功
                 能单体、甲基丙烯酸(MAA)为水溶性单体、过硫酸钾(KPS)为引发剂,采用无皂乳液聚合法制备了聚对苯
                 乙烯磺酸微球(PSS)。利用 FTIR、XPS、SEM、TGA 和 DSC 对其进行了表征,并对其粒径、Zeta 电位、比表
                 面积、酸密度进行了考察,探讨了 NaSS、DVB 和 KPS 用量对 PSS 结构、性能的影响。当 H 2 O 为 90 mL、St
                 为 76.9 mmol、MAA 为 9.3 mmol、NaSS 为 0.7 mmol、DVB 为 7.7 mmol、KPS 为 0.7 mmol 时,制备的 PSS-3
                 粒径均匀且酸密度较高。然后,将 PSS-3 作为固体酸催化剂,用于催化油酸/甲醇酯化合成生物柴油(油酸甲酯)。
                 结果表明,当甲醇/油酸的物质的量比为 10∶1、PSS-3 用量为油酸质量的 2%、反应温度为 80  ℃、反应时间为
                 6 h 时,油酸的转化率可达 86.4%。PSS-3 作为固体酸催化剂具有较好的重复使用性能,循环使用 4 次后油酸转
                 化率没有明显下降。
                 关键词:无皂乳液聚合;聚对苯乙烯磺酸微球;生物柴油;油酸;催化技术
                 中图分类号:TQ630      文献标识码:A      文章编号:1003-5214 (2023) 05-1065-08



                     Green preparation of poly(p-phenylene sulfonic acid) microspheres
                                      and its catalytic synthesis of biodiesel


                                       1
                                                                                                 2*
                                                                                   2
                                                                        2
                                                  2
                                                           2
                       ZHANG Chunyan , SU Jiajun , YIN Hui , YAO Chenxi , XIAO Jun , LUO Jianxin
                 (1. School of Chemical and Environment Engineering, Hunan Institute of Technology, Hengyang 421002, Hunan, China;
                 2. School of Materials Science and Engineering, Hunan Institute of Technology, Hengyang 421002, Hunan, China)
                 Abstract: Poly(p-phenylene sulfonic acid) microspheres (PSS) were prepared by soap-free emulsion
                 polymerization using  water  as medium, styrene  (St) as matrix monomer,  divinylbenzene  (DVB) as
                 cross-linking monomer,  sodium  p-phenylene sulfonate (NaSS) as functional monomer, methacrylic acid
                 (MAA) as water-soluble monomer, and potassium persulfate (KPS) as initiator. The obtained microspheres
                 were then characterized by FTIR, XPS, SEM, TGA and DSC, followed by investigation on their particle
                 size, Zeta potential, specific surface area and acid density as well as the influence of NaSS, DVB and KPS
                 dosages on the structure and properties of the microspheres. When H 2O was 90 mL, St was 76.9 mmol,
                 MAA was 9.3 mmol, NaSS was 0.7 mmol, DVB was 7.7 mmol, and KPS was 0.7 mmol, the prepared
                 PSS-3 has a uniform particle size and high acid density. The catalytic performance of PSS-3 in catalyzing
                 the esterification of oleic acid/methanol for biodiesel synthesis was further analyzed. The results showed
                 that the conversion rate of oleic acid could reach 86.4% when the molar ratio of methanol to oleic acid was
                 10∶1, PSS-3 dosage was 2% of the mass of oleic acid, reaction temperature was 80  ℃, and reaction time
                 was 6 h. As a solid acid catalyst, PSS-3exhibited good reusability with the conversion of oleic acid showed


                 收稿日期:2022-08-25;  定用日期:2022-12-08; DOI: 10.13550/j.jxhg.20220795
                 基金项目:国家自然科学基金(21802039);湖湘青年科技创新人才项目(2020RC3055);国家级大学生创新创业训练计划项目
                 (202211528024);湖南省大学生创新创业训练计划项目(湘教通[2022]174 号);衡阳市科技计划项目(202150063362)
                 作者简介:张春燕(1984—),女,博士,副教授,E-mail:chinachunyan@126.com。联系人:罗建新(1983—),男,博士,教授,E-mail:
                 luojianxin392@163.com。
   140   141   142   143   144   145   146   147   148   149   150