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[1]康婧娟,汤吉海,张竹修,等.溶剂辅助制备K2O-NaA固体碱催化合成3-乙氧基丙酸乙酯[J].南京工业大学学报(自然科学版),2018,40(06):1-6.[doi:10.3969/j.issn.1671-7627.2018.06.001]
 KANG Jingjuan,TANG Jihai,ZHANG Zhuxiu,et al.A solvent-assisted approach to prepare K2O-NaA for synthesis of ethyl 3-ethoxypropionate[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2018,40(06):1-6.[doi:10.3969/j.issn.1671-7627.2018.06.001]
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溶剂辅助制备K2O-NaA固体碱催化合成3-乙氧基丙酸乙酯()
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《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
40
期数:
2018年06期
页码:
1-6
栏目:
出版日期:
2018-11-20

文章信息/Info

Title:
A solvent-assisted approach to prepare K2O-NaA for synthesis of ethyl 3-ethoxypropionate
文章编号:
1671-7627(2018)06-0001-06
作者:
康婧娟1汤吉海12张竹修1费兆阳1陈献1崔咪芬1乔旭12
1.南京工业大学 化工学院 材料化学工程国家重点实验室,江苏 南京 210009; 2.江苏先进生物与化学制造协同创新中心,江苏 南京 210009
Author(s):
KANG Jingjuan1TANG Jihai12ZHANG Zhuxiu1FEI Zhaoyang1CHEN Xian1CUI Mifen1QIAO Xu12
1.State Key Laboratory of Materials-Oriented Chemical Engineering,College of Chemical Engineering, Nanjing Tech University,Nanjing 210009,China; 2.Jiangsu National Synergetic Innovation Center for Advanced Materials(SICAM),Nanjing 210009,China
关键词:
固体碱 K2O-NaA 重复使用性能 3-乙氧基丙酸乙酯
Keywords:
solid base K2O-NaA reusablity ethyl 3-ethoxypropionate
分类号:
TQ032.4
DOI:
10.3969/j.issn.1671-7627.2018.06.001
文献标志码:
A
摘要:
以KNO3为前驱体,NaA为载体,通过溶剂辅助分步焙烧法(SASC)制备固体碱催化剂K2O-NaA。研究有机溶剂的引入对前驱体KNO3分解的促进作用,采用热重-质谱连用仪(TG-MS)分析KNO3在高温下的分解性能。结果表明:SASC法制备过程中的有机溶剂在N2氛围中炭化生成具有还原性的C,C与未分解的KNO3反应,产生更多的碱性位,催化剂的碱强度和碱量明显增加。考察了K2O-NaA在乙醇和丙烯酸乙酯加成制备3-乙氧基丙酸乙酯(EEP)中的催化性能,当乙醇和丙烯酸乙酯的摩尔比为8:1,催化剂用量为丙烯酸乙酯质量的10%,反应温度为70 ℃,反应8 h,丙烯酸乙酯转化率为95.3%,3-乙氧基丙酸乙酯选择性为99.1%。催化剂重复使用4次后,丙烯酸乙酯的转化率依旧保持在90%以上,说明该催化剂的重复使用性能高。
Abstract:
Solid base catalysts based upon KNO3 as a precursor and NaA as a support were prepared by a solvent-assisted stepwise calcination approach(SASC).To investigate the positive effect of organic solvent on the decomposition of KNO3,thermal gravimetric mass spectrometer(TG-MS)was used to track the decomposition process of KNO3 on NaA.Results showed that during the SASC process,the organic solvent was converted to carbon which subsequently acted as the reductant for the fully decomposition of remaining KNO3.More basic sites were thereby generated compared to the direct calcination approach.Catalytic activity was evaluated via the addition reaction of ethyl acrylate and ethanol for the synthesis of ethyl 3-ethoxypropionate(EEP).95.3% ethyl acrylate was converted to EEP with 99.1% selectivity in 8 h at 70 ℃ by using 10% catalyst(n(ethanol)/n(ethyl acrylate)=8).The recyclability test exhibited that the conversion of ethyl acrylate maintained above 90% even after four catalytic cycles.

参考文献/References:

[1] 俞小鸥,王树敏,邓一建,等.3-乙氧基丙酸乙酯的制备方法:101423475B[P].2009-05-06.
[2] 罗鑫鹏,吴小强.一种合成3-乙氧基丙酸乙酯的制备方法:104016861A[P].2014-09-03.
[3] YOSHIO O,HIDESHI H.Solid base catalysis[M].高滋,乐英红,华伟明,译.上海:复旦大学出版社,2013.
[4] 郭登峰,赵会晶,赵文,等.凹凸棒负载KF催化合成乙二醇烯丙基醚[J].高校化学工程学报,2014,28(2):270.
[5] 田丹碧,韦长梅,史宛芗,等.KF/Al2O3在Michael加成反应中的应用及其机理[J].南京工业大学学报(自然科学版),2004,26(2):92.
[6] EVANGELISTA J P,GONDIM A D,SOUZA L D,et al.Alumina-supported potassium compounds as heterogeneous catalysts for biodiesel production:a review[J].Renewable & sustainable energy reviews,2016,59:887.
[7] XIE W L,CHEN J.Heterogeneous interesterification of triacylglycerols catalyzed by using potassium-doped alumina as a solid catalyst[J].Journal of agricultural & food chemistry,2014,62(43):10414.
[8] BENJAPORNKULAPHONG S,NGAMCHARUSSRIVICHAI C,BUNYAKIAT K.Al2O3-supported alkali and alkali earth metal oxides for transesterification of palm kernel oil and coconut oil[J].Chemical engineering journal,2009,145(3):468.
[9] ZHU L,LU F,LIU X D,et al.A new redox strategy for low-temperature formation of strong basicity on mesoporous silica[J].Chemical communications,2015,51(49):10058.
[10] WIELAND W S,DAVIS R J.Novel solid base catalysts for Michael additions synthesis,characterization and application[J].Journal of molecular catalysis a(chemical),1998,173:490.
[11] SUN L B,LIU X Q,ZHOU H C.Design and fabrication of mesoporous heterogeneous basic catalysts[J].Chemical society reviews,2015,44(15):5092.
[12] NOIROJ K,INTARAPONG P,LUENGNARUEMITCHAI A,et al.A comparative study of KOH/Al2O3 and KOH/NaY catalysts for biodiesel production via transesterification from palm oil[J].Renewable energy,2009,34(4):1145.
[13] XIE W L,HONG P,CHEN L G.Transesterification of soybean oil catalyzed by potassium loaded on alumina as a solid-base catalyst[J].Applied catalysis a general,2006,300(1):67.
[14] LIU X Y,SUN L B,LU F,et al.Low-temperature generation of strong basicity via an unprecedented guest-host redox interaction[J].Chemical communications,2013,49(73):8087.
[15] PISITPONG I,CHESTA J,APANEE L,et al.The transesterification of palm oil using KOH supported on bentonite in a continuous reactor[J].International journal of green energy,2013,11(9):987.
[16] KONG Y,SHEN X,CUI S,et al.Facile synthesis of amine hybrid aerogel with high adsorption efficiency and regenerability for air capture via solvothermal-assisted sol-gel process and supercritical drying[J].Green chemistry,2015,17(6):3436.

备注/Memo

备注/Memo:
收稿日期:2017-05-11
基金项目:国家自然科学基金(21676141,21606130); 江苏省“六大人才高峰”(2015-XCL-017)
作者简介:康婧娟(1992—),女,江苏南通人,硕士,主要研究方向为原子经济反应; 汤吉海(联系人),教授,E-mail:jhtang@njtech.edu.cn.
引用本文:康婧娟,汤吉海,张竹修,等.溶剂辅助制备K2O-NaA固体碱催化合成3-乙氧基丙酸乙酯[J].南京工业大学学报(自然科学版),2018,40(6):1-6..
更新日期/Last Update: 2018-11-30