[1]郭登峰,刘红,刘准,等.固体碱催化剂KF/Al2O3催化合成乙二醇丁醚[J].南京理工大学学报(自然科学版),2011,(01):122-126.
 GUO Deng-feng,LIU Hong,LIU Zhun,et al.Synthesis of Ethylene Glycol Monobutyl Ether with KF /Al2 O3 Solid Base Catalyst[J].Journal of Nanjing University of Science and Technology,2011,(01):122-126.
点击复制

固体碱催化剂KF/Al2O3催化合成乙二醇丁醚
分享到:

《南京理工大学学报》(自然科学版)[ISSN:1005-9830/CN:32-1397/N]

卷:
期数:
2011年01期
页码:
122-126
栏目:
出版日期:
2011-02-28

文章信息/Info

Title:
Synthesis of Ethylene Glycol Monobutyl Ether with KF /Al2 O3 Solid Base Catalyst
作者:
郭登峰1刘红1刘准2曹惠庆2赵文1石兆君1
1. 常州大学化学化工学院,江苏常州213164; 2. 江苏怡达化工有限公司,江苏江阴214441
Author(s):
GUO Deng-feng1LIU Hong1LIU Zhun2CHAO Hui-qing2ZHAO Wen1SHI Zao-jun1
1. School of Chemistry and Chemical Engineering,Changzhou University,Changzhou 213164; 2. Jiangsu Yida Chemical Co. Ltd. ,Jiangyin 214441
关键词:
固体碱催化剂 制备 乙二醇丁醚 表征 合成
Keywords:
solid base catalysts preparation ethylene glycol monobutyl ether characterization Synthesis
分类号:
O623. 42
摘要:
针对乙二醇丁醚合成中传统催化剂产物后处理工艺复杂、污染环境等缺点,采用浸渍法 制备KF /Al2O3 负载型固体碱催化剂,催化环氧乙烷( EO) 与丁醇反应合成乙二醇丁醚。考察了 催化剂前驱体/载体比例、焙烧温度对催化性能的影响。结果表明氟化钾( KF) 负载量为30%, 焙烧温度为600℃时,催化剂对EO 和丁醇反应催化活性最高。对催化剂进行了XRD 表征,并 采用Hammett 指示剂法测定了催化剂的碱强度: pKa>9. 3 的总碱量为3. 0mmol /g 催化剂,碱强 度( H_) ≥18. 4,属中等碱强度催化剂。KF /Al2O3 固体碱催化剂用于催化合成乙二醇丁醚最佳 工艺条件为: 反应温度110℃,反应压力0. 20 ~ 0. 30 MPa,催化剂用量为0. 5% ( m/m) , n( BuOH) ∶n( EO) 为5 ∶1,反应时间100 ~ 120 min,EO 转化率达99. 47%。
Abstract:
In order to solve the problems that the traditional catalysts are dealt in difficult and polluted environments in ethylene glycol monobutyl ether production,the KF/Al2O3 solid base catalysts are prepared via impregnation method and their catalytic properties for the etherification to synthesize ethylene glycol monobutyl ether from ethylene oxide( EO) and butanol are evaluated. The influences of loading amount of KF over Al203 support,calcinate temperature of catalysts are examined. The results indicate that the catalyst possesses the best catalytic activity under the conditions of catalyst calcinate temperature 600 ℃ and 30% of loading amount of KF. The catalysts are characterized by means of Xray diffraction( XRD) and surface alkalinity are determined by Hammett indicator method. The results show that its base strength is higher than 18. 4 and the base amount( pKa>9. 3) is 3. 0 mmol /g Cat. The optimal etherification condition is as follows: reaction temperature 110℃,pressure 0. 20 ~ 0. 30 MPa,reaction time 100 ~120 min,w( catalyst) = 0. 5% and n( BuOH) ∶n( EO) = 5 ∶1. Under such reaction conditions,the conversion of EO reaches 99. 47%.

参考文献/References:

[1] 于德起. 国内乙二醇单醚的发展现状与预测[J]. 精 细石油化工,2002( 5) : 49-54.
[2] 陈永福,秦怡生. 乙二醇醚类的市场需求和生产技 术进展[J]. 精细石油化工进展,2002,3( 4) : 28-34.
[3] CEH Marketing Research Report[R]. Glycol Ethers, 1996,10: 663.
[4] Edelmann K,Sandner B. Star-shaped oligo ( ethylene glycol) ethers( OEGE) as a new type of plasticizer for polymer gel electrolytes[J]. Solid State Ionics,2004, 170( 3-4) : 225-232.
[5] 陈忠明,陶克毅. 固体碱催化剂的研究进展[J]. 化 学进展,1994,( 2) : 18-25.
[6] Hajime Kabashima,Hideto Tsuji,Shinichi Nakata,et al. Activity for bas-catalyzed reactions and characterization of alumina-supported KF catalysts[J]. Applied Catalysis,2000,194-195: 227-240.
[7] 闫向阳,刘建平,杨新丽. KF/γ- Al2O3 制备条件对 催化合成八乙酸蔗糖酯的影响[J]. 应用化工, 2009,38( 7) : 1004-1006
[8] 魏彤,王谋华,魏伟,等. 固体碱催化剂[J]. 化学通 报,2002,65( 9) : 594-600.
[9] 朱建华,须沁华. KF 负载制备固体强碱的研究[J]. 化学学报,1997,55: 474-479.
[10] 黄军左,黄克明,苏秋芳. 镁铝复合氧化物催化合成 醇醚醋酸酯的研究[J]. 合成技术及应用,2005,19 ( 1) : 9-10.
[11] 董国君,王越,李婷.氧化锆负载硝酸盐固体碱催化剂 的制备与表征[J].应用化工,2008,37( 3) : 310-313.
[12] 杨洪丽,李为民,姚建. 钙基负载型固体碱催化酯交 换反应活性评价[J]. 燃料化学学报,2008,36( 2) : 241-245.
[13] 顾明兰. 溶胶-凝胶法制备纳米氟化钾/三氧化二铝 催化剂的研究[D]. 南京: 南京工业大学化工学 院,2005. 126

相似文献/References:

[1]仝玉萍,陆路德,汪信,等.Eu2Sn2O7纳米晶的盐助甘氨酸燃烧法制备及结构表征[J].南京理工大学学报(自然科学版),2010,(03):386.
 TONG Yu-ping,LU Lu-de,WANG Xin,et al.Preparation and Structure Characterization of Eu2Sn2O7 Nanocrystals by Salt-assistant Glycine Combustion Method[J].Journal of Nanjing University of Science and Technology,2010,(01):386.
[2]蒋文俊,许建,赵春宝,等.改性层状双氢氧化镁铝的制备及在PA6中的阻燃应用[J].南京理工大学学报(自然科学版),2009,(02):272.
 JIANG Wen-jun,XU Jian,ZHAO Chun-bao,et al.Preparation of Modified Mg-Al Layered Double Hydroxide and Its Flame-retardant Application in PA6 Composites[J].Journal of Nanjing University of Science and Technology,2009,(01):272.
[3]朱俊武,张莉莉,吴继科,等.硬脂酸法制备层状K_2Pr_2Ti_3O_(10)及其酸交换性质研究[J].南京理工大学学报(自然科学版),2008,(02):248.
 ZHU Jun-wu,ZHANG Li-li,WU Ji-ke,et al.Preparation of Layered K2Pr2Ti3O10 by Stearic Acid Method and Its Acid-exchanging Property[J].Journal of Nanjing University of Science and Technology,2008,(01):248.
[4]俞马宏* *,崔学军,黄炼军.过氧化尿素的制备及其热稳定性研究[J].南京理工大学学报(自然科学版),2005,(01):59.
 YU Ma-hong,CUI Xue-jun,HUANG Lian-jun.Preparation and Thermostability of Urea Peroxide[J].Journal of Nanjing University of Science and Technology,2005,(01):59.
[5]黄龙祥,吕春绪.4-苯基-4-(1,2,4-三唑-1-基)-3-丁烯-2-酮及其衍生物的合成[J].南京理工大学学报(自然科学版),2003,(01):110.
 HuangLongxiang LuChunxu.Preparation of 4-Pheny-4-(1,2,4-Triazole-1-yl)-3-Buten-2-One and Its Derivatives[J].Journal of Nanjing University of Science and Technology,2003,(01):110.
[6]刘晓东,李健生,张爱娟,等.氧化铝微滤膜的制备及表征[J].南京理工大学学报(自然科学版),2002,(04):406.
 LiuXiaodong LiJiansheng ZhangAijuan SunXiuyun WangLianjun.The Preparation and Characterization of Alumina Microfiltration Membrane[J].Journal of Nanjing University of Science and Technology,2002,(01):406.
[7]叶明泉,邓国栋,韩爱军,等.超细鲜骨粉的制备及其营养功能研究[J].南京理工大学学报(自然科学版),1999,(01):10.
 Ye Mingquan Deng Guodong Han Aijun Li Fengshen Song Hongchang.A Study on the Preparation and Nutritive Functions of Ultrafine Fresh Bone Powder[J].Journal of Nanjing University of Science and Technology,1999,(01):10.
[8]杨宇,杨绪杰,王瑛,等.酰胺酸、酰亚胺键扩链二胺的合成与表征[J].南京理工大学学报(自然科学版),1997,(04):45.
 Yang Yu Yang Xujie Wang Ying Lu Lude Wang Xin.Preparation and Characterization of Novel Diamines Chain extented by Amic Acid Linkage and by Imide Linkage[J].Journal of Nanjing University of Science and Technology,1997,(01):45.
[9]陆明,孙荣康,吕春绪,等.六硝基芪合成新方法[J].南京理工大学学报(自然科学版),1994,(05):8.
 Lu Ming.ANew Method for Synthesising Hexanitrostilbene.[J].Journal of Nanjing University of Science and Technology,1994,(01):8.
[10]刘 斌,胡文胜,李亚娟.纳米CuO-Co3O4-NiO复合氧化物的制备与 电化学性能[J].南京理工大学学报(自然科学版),2014,38(06):829.
 Liu Bin,Hu Wensheng,Li Yajuan.Preparation of nano CuO-Co3O4-NiO composite oxide and its electrochemical properties[J].Journal of Nanjing University of Science and Technology,2014,38(01):829.

备注/Memo

备注/Memo:
基金项目:国家自然科学基金( 20671045) 作者简介:郭登峰( 1964-) ,男,教授,硕士生导师,主要研究方向: 有机合成及工业分析,E-mail: gdf166@163. com。
更新日期/Last Update: 2012-02-28