Laser-supported high-temperature MAS NMR for time-resolved in situ studies of reaction steps in heterogeneous catalysis

被引：34

作者：

Ernst, H ^{[1
]}

Freude, D ^{[1
]}

Mildner, T ^{[1
]}

Wolf, I ^{[1
]}

机构：

[1] UNIV LEIPZIG,ABT GRENZFLACHENPHYS,D-04103 LEIPZIG,GERMANY

来源：

SOLID STATE NUCLEAR MAGNETIC RESONANCE | 1996年 / 6卷 / 02期

关键词：

catalysis; C-13 magic-angle-spinning nuclear magnetic resonance; H-1 magic-angle-spinning nuclear magnetic resonance; in situ reactions; zeolite Y; ZSM-5;

D O I：

10.1016/0926-2040(95)01214-1

中图分类号：

O64 [物理化学（理论化学）、化学物理学];

学科分类号：

070304 ; 081704 ;

摘要：

The temperature of zeolite samples containing various adsorbed molecules was rapidly changed (within 15 s) from room temperature to 600 K by means of a laser beam. The location of the sealed glass ampoule in a boron nitride container decreases the temperature gradient in the sample and avoids laser-induced reactions. The technique facilitates time-dependent magic-angle-spinning (MAS) NMR spectroscopy of high-temperature reactions which take place within 60 s. The H-D exchange in the hydrogen form of zeolites loaded with fully deuterated molecules, the methanol-to-gasoline conversion and the catalytic ethylbenzene disproportionation in zeolites were monitored by C-13 and H-1 MAS NMR by means of a ''stop and go'' method.

引用

页码：147 / 156

页数：10

共 22 条

[1] DIRECT OBSERVATION OF SHAPE SELECTIVITY IN ZEOLITE ZSM-5 BY MAGIC-ANGLE-SPINNING NMR [J].

ANDERSON, MW ;

KLINOWSKI, J .

NATURE, 1989, 339 (6221) :200-203

[2] SOLID-STATE NMR-STUDIES OF THE SHAPE-SELECTIVE CATALYTIC CONVERSION OF METHANOL INTO GASOLINE ON ZEOLITE ZSM-5 [J].

ANDERSON, MW ;

KLINOWSKI, J .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1990, 112 (01) :10-16

[3]

[Anonymous], ANN REP NMR SPECTROS

[4] FORMATION OF SURFACE-BONDED METHOXY GROUPS IN THE SORPTION OF METHANOL AND METHYL-IODIDE ON ZEOLITES STUDIED BY C-13 MAS NMR-SPECTROSCOPY [J].

BOSACEK, V .

JOURNAL OF PHYSICAL CHEMISTRY, 1993, 97 (41) :10732-10737

[5]

ERNST H, 1994, STUD SURF SCI CATAL, V84, P1717

[6] TEMPERATURE-SWITCHED MAS NMR - A NEW METHOD FOR TIME-RESOLVED IN-SITU STUDIES OF REACTION STEPS IN HETEROGENEOUS CATALYSIS [J].

ERNST, H ;

FREUDE, D ;

MILDNER, T .

CHEMICAL PHYSICS LETTERS, 1994, 229 (03) :291-296

[7] TEMPERATURE-JUMP MAS NMR WITH A LASER HEATER [J].

FERGUSON, DB ;

KRAWIETZ, TR ;

HAW, JF .

JOURNAL OF MAGNETIC RESONANCE SERIES A, 1994, 109 (02) :273-275

[8] TRANSIENT METHODS FOR IN-SITU NMR OF REACTIONS ON SOLID CATALYSTS USING TEMPERATURE JUMPS [J].

FERGUSON, DB ;

HAW, JF .

ANALYTICAL CHEMISTRY, 1995, 67 (18) :3342-3348

[9] ENHANCED RESOLUTION IN THE H-1-NMR SPECTRA OF ZEOLITE H-ZSM-5 BY HETERONUCLEAR DIPOLAR-DEPHASING SPIN-ECHO MAS [J].

FREUDE, D .

CHEMICAL PHYSICS LETTERS, 1995, 235 (1-2) :69-75

[10]

Haw J. F., 1994, NMR Techniques in Catalysis, V1st, P139

← 1 2 3 →