一步法合成AlSBA-15-SO_3H有机无机杂化固体酸及其催化邻苯二甲酸酐甲酯化反应的研究  

One-pot Synthesis of AlSBA-15-SO_3H Organic-inorganic Hybrid Solid Acid Catalysts for the Esterification of Phthalic Anhydride with Dimethyl Carbonate

作　　者：郑岩[1] 李军平[2] 赵宁[2] 魏伟[2] 孙予罕[2] 

机构地区：[1]天津科技大学,天津300457 [2]中国科学院山西煤炭化学研究所煤转化国家重点实验室,山西太原030001

出　　处：《精细化工》2006年第10期972-976,共5页Fine Chemicals

摘　　要：以正硅酸乙酯和3-巯丙基三甲氧基硅烷为硅源,异丙醇铝〔A l(iPr)3〕为铝源,一步法合成了有机无机杂化固体酸A lSBA-15-SO3H。通过X射线粉末衍射(XRD)、氮气等温吸附脱附、氨的程序升温脱附(NH3-TPD)和29S i,27A l固体核磁等方法对样品进行了表征。结果表明,有机无机杂化固体酸相对于单一丙磺酸改性的有机固体酸SBA-15-SO3H总酸量显著增加,最高可提高1.77 mmol/g。A lSBA-15-SO3H在催化活化邻苯二甲酸酐(PAH)和碳酸二甲酯(DMC)酯化反应中,邻苯二甲酸酐的转化率随着反应温度升高而增加,最高可达100%,且其转化率与催化剂总酸量成线性关系。AlSBA-15-SO3H organic-inorganic hybrid solid acid with various n（ Si）/n（Al） ratios were prepared using tetraethoxysilane, 3-mercaptopropyltrimethoxysilane and aluminum isopropoxide [ Al （iPr）3] as the precursors by one-pot method. The samples were characterized by the XRD, BET （surface area）, NH3-TPD and 29Si,27 Al MAS-NMR techniques. The results showed that upon the introduction of Al into the SBA-15-SO3H,the total acidity of the samples increased and the enhancing acidity was up to 1.77 mmol/g. The samples were also used to catalyze the esterification of phthalic anhydride （PAH） with dimethyl carbonate （DMC）. Conversion of PAH increased with increasing temperature and was up to 100%. Moreover,conversion of PAH was linear with the total acidity of the catalysts.

关 键 词：固体酸催化剂 酯化反应 邻苯二甲酸酐 碳酸二甲酯 

分 类 号：TQ426.91[化学工程]