CN201611110377
CN106582831A
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摘要:本发明公开了一种SBA?15固载聚合酸性离子液体催化剂,先将活化的SBA?15介孔分子筛与TEVS溶于无水甲苯中,氮气保护下回流;分离的固体洗涤后,用甲苯抽提,干燥后制得SBA?15?vinyl;将1?乙烯基咪唑用乙酸乙酯溶解,将1, 3?丙磺酸内酯滴加进该溶液,得到白色固体沉淀;将其溶于水中,滴加等摩尔量H2SO4,反应获得IL;将得到的IL加入到无水乙醇中,将SBA?15?vinyl加入,再加入AIBN作为引发剂,加热回流,进行SBA?15介孔分子筛表面聚合反应;反应结束后,产物过滤分离,并用丙酮和乙醇洗涤,40℃、真空干燥,得到SBA?15固载聚合酸性离子液体催化剂成品。本发明制备的催化剂结构稳定性高、热稳定性好、酸性强且便于回收。 |
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Abstract: The invention discloses an SBA-15-suported polymeric acidic ionic liquid catalyst. An activated SBA-15 mesoporous molecular sieve and TEVS are firstly dissolved in anhydrous toluene and subjected to reflux under the protection of nitrogen; SBA-15-vinyl is prepared after separated solids are washed, extracted with toluene and dried; 1-vinyl imidazole is dissolved with ethyl acetate, 1,3-propane sultone is dropwise added to the solution, and white solid precipitate is obtained; the precipitate is dissolved in water, H2SO4 with the molar weight equal to that of the precipitate is dropwise added, and IL is obtained through the reaction; the obtained IL is added to absolute ethyl alcohol, SBA-15-vinyl is added, AIBN is added to be used as an initiator, heating reflux is performed, and SBA-15 mesoporous molecular sieve surface polymerization reaction is performed; after the reaction ends, a product is filtered, separated, washed with acetone and ethyl alcohol and subjected to vacuum drying at 40 DEG C, and a finished SBA-15-suported polymeric acidic ionic liquid catalyst product is obtained. The prepared catalyst is high in structural stability, good in thermal stability, strong in acidity and convenient to recover. | |
申请人: 河南工业大学 | |
Applicant: UNIV HENAN TECHNOLOGY | |
地址: 450001 河南省郑州市高新技********(隐藏) | |
发明(设计)人: 谢文磊 张弛 王宏雁 | |
Inventor: XIE WENLEI; ZHANG CHI; WANG HONGYAN | |
主分类号: B01J31/06(2006.01)I | |
分类号: B01J31/06(2006.01)I | |
2019-03-08 | 授权 |
2017-05-24 | 实质审查的生效 IPC(主分类):B01J 31/06申请日:20161206 |
2017-04-26 | 公开 |
主权项 | 一种SBA‑15固载聚合酸性离子液体催化剂,其特征在于:制备方法包括下述步骤:第一步,SBA‑15介孔分子筛的乙烯基功能化修饰将经高温活化的SBA‑15介孔分子筛与1‑乙烯基三乙氧基硅烷溶于无水甲苯中,充分混合,在氮气保护下加热回流反应24h;反应结束后,将体系冷却至室温,对产物进行过滤分离,固体用无水甲苯洗涤;然后将产物置于索氏提取器中,用甲苯抽提4h,除去未反应的硅烷;操作结束后,将产物过滤分离并置于60℃下真空干燥10h,可得到乙烯基功能化修饰的SBA‑15介孔分子筛;第二步,乙烯基酸性离子液体的合成将1‑乙烯基咪唑用乙酸乙酯溶解,在0℃和搅拌条件下将丙磺酸内酯缓慢滴加进该溶液,滴加完成后继续搅拌1h,再将混合溶液置于25℃下搅拌反应24h;抽滤,干燥,得到离子液体中间体盐;然后,将该中间体盐溶于水中,在搅拌下缓慢滴加等摩尔量的H2SO4,然后在50℃下搅拌反应12h,可获得酸性离子液体[SO3H‑(CH2)3‑IM‑vinyl] [HSO4];第三步,制备SBA‑15固载聚合酸性离子液体催化剂将第二步得到的[SO3H‑(CH2)3‑IM‑vinyl][HSO4] 酸性离子液体加入无水乙醇中,充分混合后,将第一步制得的乙烯基修饰SBA‑15介孔分子筛加入,再加入偶氮二异丁腈作为引发剂,加热回流反应20h,进行SBA‑15介孔分子筛表面的聚合反应;反应结束后,对产物进行过滤分离,并用丙酮和乙醇进行洗涤,再在40℃和真空条件下干燥8 h后,可得到SBA‑15固载聚合酸性离子液体催化剂成品。 | ||||||||||||||||||
公开号 | 106582831A | ||||||||||||||||||
公开日 | 2017-04-26 | ||||||||||||||||||
专利代理机构 | 郑州异开专利事务所(普通合伙) 41114 | ||||||||||||||||||
代理人 | 王霞 | ||||||||||||||||||
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类型 | 阶段 | 文献号 | 公开日期 | 涉及权利要求项 | 相关页数 |
Y | SEA | CN103506156A | 20140115 | 1-4 | 说明书第[0011]-[0018]段 |
A | SEA | CN103611568A | 20140305 | 1-4 | 全文 |
A | SEA | CN104193621A | 20141210 | 1-4 | 全文 |
Y | SEA | CN105107547A | 20151202 | 1-4 | 说明书第[0007]-[0011]段 |
A | SEA | CN105642344A | 20160608 | 1-4 | 全文 |
A | SEA | CN105688993A | 20160622 | 1-4 | 全文 |
类型 | 阶段 | 期刊文摘名称 | 作者 | 标题 | 涉及权利要求项 | 相关页数 |
A | SEA | 《Food Chemistry》 | Wenlei Xie et al. | Propylsulfonic and arenesulfonic functionalized SBA-15 silica as an efficient and reusable catalyst for the acidolysis of soybean oil with medium-chain fatty acids | 1-4 | 74-82 |
WENLEI XIE ET AL.: "Propylsulfonic and arenesulfonic functionalized SBA-15 silica as an efficient and reusable catalyst for the acidolysis of soybean oil with medium-chain fatty acids", 《FOOD CHEMISTRY》 | ||||||
类型 | 阶段 | 书名 | 作者 | 标题 | 涉及权利要求项 | 相关页数 |