脱铝超稳Y沸石上金刚烷的制备

PREPARATION OF ADAMANTANE OVER DUSY CATALYST

采用水处理与HCl处理相结合的方式对超稳Y沸石(USY)进行脱铝改性,制备了一系列脱铝超稳Y沸石(DUSY)和PW/DUSY1催化剂,用X射线衍射、N2吸附和氨程序升温脱附等表征方法对这些催化剂的物化性质进行了表征,并在桥式四氢双环戊二烯(endo-TCD)异构化制备金刚烷(ADH)反应中考察了它们的催化性能。结果表明,以DUSY1为催化剂,当活化温度350℃、反应温度260℃、反应时间4 h、初始压力1.1 MPa、催化剂与原料的质量比0.7、溶剂环己烷与原料的摩尔比5.0时,endo-TCD的转化率达到99.7%,ADH的收率达到30.1%。

The dealuminated USY （DUSY） modified by deep hydrothermal treatment combined with HCl leaching were prepared. The catalysts of 12-tungstophosphoric acid （PW） supported on DUSY were obtained by impregnation at room temperature. The catalytic performances of DUSY and PW/ DUSY1 catalysts were investigated in the preparation of adamantine （ADH） by isomerization of endo-tetrahydrodicyclotadiene （endo-TCD） in a 100 ml batch stainless-steel autoclave with stirring. And their physico-chemical properties were characterized by X-ray diffraction （XRD）, N2 adsorption isotherm and temperature programmed desorption of ammonia （NH3-TPD）. It was found that when over DUSY1 catalyst, the conversion of endo-TCD up to 99.7% and the yield of adamantine up to 30.1% can be obtained under the following optimal conditions, activated temperature of 350℃, reaction temperature of 260℃, initial pressure of 1.1 MPa, the mass ratio of catalysts to endo-TCD of 0.7, the molar ratio of cyclohexane to endo-TCD of 5.0 and reaction time of 4 h.