摘要
采用蒸气促进的干胶法,在工业硅胶上原位合成出TS-1纳米晶.先用TS-1合成液浸渍硅胶,再于130℃下和水蒸气作用2 d,得到硅胶上负载的TS-1纳米晶.采用XRD,FTIR,UV-Vis和NMR谱以及N2吸附、ICP、SEM和TEM等对所得样品进行了表征.结果表明,将TS-1纳米晶负载在硅胶上,其晶粒大小为20nm左右,Ti进入了分子筛的骨架;所得的TS-1/silica gel复合材料的比表面积为113.2 m2/g,平均中孔孔径达到23.7 nm.将其用于苯的羟基化反应,以n(C6H6)/n(H2O2)=3进料,环丁砜为溶剂,于100℃下反应2h,苯的转化率达到8.7%,苯酚的选择性超过99%,苯的氧化速率(TOF)为11.37,其催化活性明显高于传统水热合成的TS-1.
TS-1 nanocrystals were synthesized on silica gel via dry gel conversion method, at first silica gel was impregnated with TS-1 synthesis solution and then followed by steam treatment at 130℃ for 2 d. The product was characterized with XRD, FTIR, UV-Vis, NMR, N2 adsorption, ICP, SEM and TEM. The results indicate that TS-1 crystals were grown on silica gel with a size of ca. 20 nm, a BET specific surface area of 113.2 m^2/g and a mesopore size of 23.7 nm. The product exhibited a higher catalyst performance than TS-1 powders, which was prepared by conventionally hydrothermal synthesis, for benzene hydroxylation with n（ benzene）/n（H2O2） =3 and sulfolane as the solvent at 100℃ for 2 h. The benzene conversion and TOF were 8.7% and 11.37, respectively, with more than 99% of phenol selectivity.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2007年第8期1411-1415,共5页
Chemical Journal of Chinese Universities
基金
国家自然科学基金(批准号:20141003和20201007)资助
关键词
纳米晶
TS-1
干胶转化法
硅胶
Nanocrystal
TS-1
Dry gel conversion method
Silica gel
