活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯

doi:10.3969/j.issn.1000-2006.2015.02.021

国家林草科技领军期刊
中国精品科技期刊
中国高校百佳科技期刊
江苏省新闻出版政府奖期刊奖
RCCSE林学权威期刊（A+）
CSCD核心期刊
Scopus数据库收录期刊
中文核心期刊
SCD核心期刊

作者加群：102861116

微信公众号：南京林业大学学报

高级检索

南京林业大学学报（自然科学版） ›› 2015, Vol. 58 ›› Issue (02): 121-126.doi: 10.3969/j.issn.1000-2006.2015.02.021

活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯

陈燕青,邹斌,董琳,吕昌,陈健敏,朱新宝^*

南京林业大学化学工程学院,江苏南京 210037

出版日期:2015-03-31 发布日期:2015-03-31
基金资助:
收稿日期:2014-03-28 修回日期:2014-09-20
第一作者:陈燕青,硕士生。*通信作者:朱新宝,教授。E-mail: zhuxinbao@njfu.com.cn。
引文格式:陈燕青,邹斌,董琳,等. 活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯[J]. 南京林业大学学报:自然科学版,2015,39(2):121-126.

Synthesis of diethylene glycol dibenzoate catalyzed by butyl titanate supported on activated carbon

CHEN Yanqing, ZOU Bin, DONG Lin, LYU Chang, CHEN Jianmin, ZHU Xinbao^*

College of Chemical Engineering, Nanjing Forest University, Nanjing 210037, China

Online:2015-03-31 Published:2015-03-31

摘要/Abstract

摘要： 以活性炭负载钛酸四丁酯为催化剂,正丁醚为带水剂,采用直接酯化法合成二乙二醇二苯甲酸酯(DEDB); 运用低温氮气吸附脱附(BET)与电子顺磁共振波谱(ESR)分析对催化剂进行表征,采用IR和¹H-NMR进行反应产物的表征; 探讨原料比、带水剂用量、反应温度等因素对酯化率的影响。确定了活性炭固载钛酸四丁酯催化二乙二醇(DEG)和苯甲酸(BA)酯化的适宜工艺条件为:原料量比n(DEG):n(BA)=1:2,带水剂占苯甲酸质量分数为20%,催化剂占苯甲酸质量分数为1.5%,反应温度200 ℃,反应时间6 h。催化剂可循环使用3次,具有较好的稳定性。

Abstract: Diethylene glycol dibenzoate(DEDB)was synthesized by catalyzing with n-butyl titanate supported on activated carbon and using n-butyl ether as the water carrier. These catalysts were characterized by BET and ESR.Effects of the ratio of substrates, amount of water carrier, and reaction temperature on esterification were examined,and the suitable esterification conditions was determined as follows:n(DEG)/n(BA)=0.5, 20%(wt)of water carrier and 1.5%(wt)of catalyst based on BA, 200 ℃ of reaction temperature and 6 h of reaction time. Meanwhile, the catalyst could be reused for 3 times, and showed good stability. The structure of product was characterized by IR and ¹H-NMR.

中图分类号:

TQ225.2

陈燕青,邹斌,董琳,等. 活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯[J]. 南京林业大学学报（自然科学版）, 2015, 58(02): 121-126.

CHEN Yanqing, ZOU Bin, DONG Lin, LYU Chang, CHEN Jianmin, ZHU Xinbao. Synthesis of diethylene glycol dibenzoate catalyzed by butyl titanate supported on activated carbon[J].Journal of Nanjing Forestry University (Natural Science Edition), 2015, 58(02): 121-126.DOI: 10.3969/j.issn.1000-2006.2015.02.021.

参考文献

[1] 王正平,张含平.新型增塑剂二甘醇二苯甲酸酯的合成[J].应用科技,2004,18(9): 52-54.Wang Z P,Zhang H P.Synthesis of a new plasticizer diethylene glycol dibenzoate[J]. Applied Science and Technology,2004,18(9): 52-54.
[2] 聂颖.无毒增塑剂环氧大豆油的开发和利用[J].精细化工原料及中间体,2008,17(1):12-14.Nie Y.The development and utilization of non-toxic plasticizer epoxidized soybean oil[J]. Fine Chemical Industrial Raw Materials & Intermediates,2008,17(1):12-14.
[3] Biedermann-Brem S,Biedermann M P, Fenninger S.Plasticizers in PVC toys and childcare products: what succeeds the phthalates market survey[J].Chromatographia,2008,68(4):227-234.
[4] 高永辉,黄凤英,黎佩琼.一缩二乙二醇二苯甲酸酯的合成[J].佛山科学技术学院学报:自然科学版,2000,17(4):43-46.Gao Y H,Huang F Y,Li P Q.Synthesis of diethylene glycol dibenzoate[J]. Journal of Foshan University:Natural Science Edition, 2000,17(4): 43-46.
[5] 张劭诚,韩宝莲.苯甲酸酯类增塑剂在聚氨酯中应用[J].现代塑料加工应用,2001,13(3): 55-57.Zhang Z C,Han B L.Plasticizer of benzic ether and its application in polyurethane[J].Modern Plastics Processing and Application,2001,13(3): 55-57.
[6] 王强.一缩二乙二醇二苯甲酸酯的合成[J].化学与生物工程,2008,25(2):57-59.Wang Q. Synthesis of diethylene glycol dibenzoatc[J].Chemical & Biological Engineering, 2008,25(2):57-59.
[7] 张庆勋,金振兴,刘连利,等.固载杂多酸催化剂 PW12/SiO₂ 复相催化合成二苯甲酸二甘醇酯[J].现代化工,1996(5):26-28.Zhang Q X,Jin Z X,Liu L L,et al. Heterogeneous catalytic synthesizing diethylene glycol dibenzonate terphthalate by supported heteropoly acid catalyst PW12/SiO₂[J]. Modern Chemical Industry,1996(5):26-28.
[8] 蒋维.磷钨酸铝催化合成二甘醇二苯甲酸酯[J].化学世界,2001,18(2):75-77.Jiang W.Synthesis of diethylene glycol dibenzoate catalyzed by aluminium phosphotungstate[J].Chemical World,2001,18(2):75-77.
[9] 单晓梅,杜铭华,朱书全,等.活性炭表面改性及吸附极性气体[J].煤炭转化,2003,26(1):33-36.Shan X M,Du M H,Zhu S Q,et al.A survey of activated carbon surface chemical modification and its application in adsorption of polar molecules[J].Coal Conversion, 2003,26(1):33-36.
[10] 郭明翠.脂肪族二元酸烷氧基乙酯增塑剂的合成工艺研究[D].南京:南京林业大学,2010.Guo M C.Kinetics for catalytic synthesis of aliphatic dicarboxylic acid alkoxy ethyl ester[D].Nanjing: Nanjing Forest University,2010
[11] 石万聪,盛承祥.增塑剂[M].北京:化学工业出版社,1989:32-33.Shi W C,Sheng C X. Plasticizers[M].Beijing:Chemical Industry Press,1989:32-33.
[12] 宋桂贤,吴雄岗.一缩二乙二醇二苯甲酸酯的合成研究[J].河北化工, 2008,31(8):13-14. Song G X,Wu X G.Synthesis of diethylene glycol dibenzoate[J].Hebei Chemical Industry,2008,31(8):13-14.
[13] Marcilla A,Garcia S,Garcia-Quesada J C. Study of the migration of PVC plasticizers[J]. J Anal Appl Pyrolysis,2004,71(2):457-463.
[14] 李丹阳.酯化反应中的催化剂[J]. 丹东师专学报,1999,21(1):43-44.
[15] Gimeno R A, Marce R M, Borrull F. Determination of plasticizers by high-performance liquid chromatography and atmospheric pressure chemical ionization mass spectrometry in water and sediment samples[J].Chromatographia,2003,58(2):37-41.
[16] Zhu Z H, Radovic L R, Lu G Q.Effects of acid treatments of carbon on N₂O and NO reduction by carbon-supported copper catalysts [J]. Carbon, 2000,38(3): 451-464.

活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯

Synthesis of diethylene glycol dibenzoate catalyzed by butyl titanate supported on activated carbon

PDF

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 0

编辑推荐

Metrics

本文评价

作者

读者

审稿