锆掺杂Zr-MCM-41介孔分子筛制备及催化性能

Preparation and Catalytic Properties of Zirconium Doped Zr-MCM-41 Mesoporous Molecular Sieves

以氯化锆作为锆源,通过超声波和微波协调作用合成掺杂锆的介孔分子筛Zr-MCM-41,采用XRD、热重分析、粒度分析、扫描电镜等技术对样品进行表征。分别制备了Si/Zr摩尔比为60,70,80,90,100,110,120的分子筛ZrMCM-41,XRD衍射强度最高的比例为Si/Zr=80,用以作催化剂和催化合成柠檬酸三丁酯。得出酯化率最高的催化反应的反应物摩尔比为1∶5,反应温度为130~140℃,反应催化剂用量为柠檬酸用量的4%。同时考察了最佳反应条件的催化剂重复使用情况,并对粗产品精制进行红外分析。

Mesoporous molecular sieve Zr--MCM--41was synthesized under the ultrasonic microware coordination with zir conium chloride. And characterized by X--ray diffractomer system, thermo gravimetric analyzer, SEM and so on Respec- tively to make the mesoporous molecular sieve Zr-- MCM-- 41 which Si/Zr molar ratiois 60,70,80,90,100,110,120. Due to the particularity of zirconium,the keletal structure of MCM--41 began to confusion, the highest diffraction intensity is Si/Zr molar ratio as 80 which is using for catalyticing synthesis of tributyl citrate esters. Finding out the mole ratio of reactantsl ： 5, reaction temperature 130-130℃, reaction of catalyst when the esterification rate of the catalytic reaction is the 40/60 of the citric acid. And repeated catalyst for optimum reaction conditions.