磺酸基键合硅胶的制备及其酸催化性能研究

磺酸基键合硅胶的制备及其酸催化性能研究

屈文¹，苏继新^1*，潘齐¹，聂玉伦²

1. 山东大学环境科学与工程学院，山东济南 250100； 2. 中国科学院生态研究中心，北京 100044

收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2006-10-24 发布日期:2006-10-24
通讯作者: 屈文

Synthesis and acid catalytic activity of HSO3-functionalized silica

QU Wen¹，SU Ji-xin^1*， PAN Qi¹，NIE Yu-lun²

1. School of Environmental Science and Engineering, Shandong University, Jinan 250100， Shandong;2. Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100044

Received:1900-01-01 Revised:1900-01-01 Online:2006-10-24 Published:2006-10-24
Contact: QU Wen

摘要/Abstract

摘要： 以氯丙基氯硅烷和苯基氯硅烷为偶联剂对硅胶进行表面改性，进一步磺化得到以磺酸基为活性中心的固体酸，磺化剂分别为硫酸和亚硫酸铵。以BET、红外光谱、总有机碳对固体酸及其前驱体进行了表征并测定了固体酸酸密度；利用总有机碳计算前驱体的键合量，苯基、氯丙基硅胶键合量分别为1.40mmol/g,1.95mmol/g；以这两种前驱体制得的固体酸酸密度分别为0.32mmol/g,0.26mmol/g；BET数据表明键合反应发生后苯基磺酸和丙基磺酸样品的比表面积由521m2/g降至406m2/g,432m2/g。将制得固体酸应用于乙酸丁酯的合成，经五次使用仍保持较高转化率。

关键词: 硅胶表面改性, 固体酸, 乙酸丁酯合成 , 磺化

Abstract: The phenyl and chloropropyl silica derived from chlorosilane were applied to synthesize HSO3-functionalized silica by using H2SO4 or (NH4)2SO3 as sulfonation agents. The solid acid and their precursors were characterized by BET, IR, TOC (total organic carbon). The surface coverage density of phenyl-silica and chloropropy1-silica are 1.40mmol/g and　1.95mmol/g, while the acid exchange capacities are 0.32mmol/g and 0.26mmol/g, respectively. The specific surface area of phenyl-silica and chloropropy1-silica respectively decreased slightly from 521m2/g to 406m2/g and 432m2/g. The solid acids were used as catalysts in the synthesis of acetic acid butylester. The results indicate that the catalysts can be reused 5 times with a high conversion ratio.

Key words: synthesis of acetic acid butylester , sulfonation, solid acid, silica surface modification

中图分类号:

TQ426.91

屈文,苏继新*,潘齐,聂玉伦 . 磺酸基键合硅胶的制备及其酸催化性能研究[J]. J4, 2007, 42(11): 11-14 .

QU Wen,SU Ji-xin*,PAN Qi,NIE Yu-lun . Synthesis and acid catalytic activity of HSO3-functionalized silica[J]. J4, 2007, 42(11): 11-14 .

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