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固体有机酸催化剂的制备及催化性能 |
徐永强1,2,白丽丽3,王海燕4,商红岩1,2,刘晨光1,2
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(1.中国石油大学(华东)理学院,山东青岛266580;2.中国石油大学(华东)重质油国家重点实验室,山东青岛 266580;3.新疆寰球工程公司, 新疆克拉玛依 833699;4.中国石油大学(华东)计算机科学与技术学院,山东青岛266580)
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摘要: |
硅胶经酸化预处理,增加表面羟基含量,在碱环境下与环氧氯丙烷反应,表面键合环氧丙烷基团,与NaHSO3或硫酸反应,制备得到钠型有机酸催化剂或氢型有机酸催化剂,采用化学滴定、元素分析、固体H-NMR等手段对实验进行分析表征。结果表明:采用甲基磺酸预处理载体硅胶,30~40 ℃下与环氧氯丙烷反应6 h,60 ℃下磺化时间8 h,制得的固体酸酸量达到2.04 mmol/g;固体有机酸催化剂用于生物柴油(脂肪酸甲酯)的合成,循环使用6次,产品收率仍超过80%;固体有机酸催化剂催化酯化活性高,稳定性好。 |
关键词: 硅胶 环氧氯丙烷 有机酸催化剂 生物柴油 酯化 |
DOI:10.3969/j.issn.1673-5005.2020.01.020 |
分类号::O 643.36 |
文献标识码:A |
基金项目:国家自然科学基金面上课题项目(21376267) |
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Preparation of solid organic sulfonic acids catalyst and its catalytic performance |
XU Yongqiang1,2, BAI Lili3, WANG Haiyan4, SHANG Hongyan1,2, LIU Chenguang1,2
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(1.College of Science in China University of Petroleum(East China), Qingdao 266580, China;2.State Key Laboratory of Heavy Oil Processing in China University of Petroleum(East China), Qingdao 266580, China;3.Xinjiang Global Engineering Company,Karamay 833699, China;4.College of Computer Science and Technology in China University of Petroleum(East China), Qingdao 266580, China)
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Abstract: |
The silicagel was activated to increase the content of hydroxyl on the surface by acidification, which further reacted with epichlorohydrin in the alkali environment. Then the surface was bonded to epoxy propane group to react with the NaHSO3 or H2SO4, through which the Na-type or H-type organic sulfonic acid catalyst was prepared. The samples were characterized and analyzed by chemical titration, elemental analysis and solid H-NMR. The results show that the acid amount of the obtained solid organic acid catalyst is up to 2.04 mmol/g when the carrier silica gel is pretreated with methanesulfonic acid, reacted with epichlorohydrin for 6 h at 30-40 ℃, and sulfonated for 8 h at 60 ℃. The catalyst is used in the synthesis of biodiesel (fatty acid methyl ester).After the catalyst is recycled for 6 times, the product yield is still over 80%, which proves that the solid organic acid catalyst has high catalytic activity and good catalytic stability. |
Key words: silica gel epichlorohydrin organic acid catalyst biodiesel esterification |