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ES2634502T3 - Preparación de estructuras zeolíticas funcionalizadas - Google Patents

Preparación de estructuras zeolíticas funcionalizadas Download PDF

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ES2634502T3
ES2634502T3 ES07757619.7T ES07757619T ES2634502T3 ES 2634502 T3 ES2634502 T3 ES 2634502T3 ES 07757619 T ES07757619 T ES 07757619T ES 2634502 T3 ES2634502 T3 ES 2634502T3
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zif
preparation
data
group
zeolitic structures
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Omar M. Yaghi
Hideki Hayashi
Rahul Banerjee
Kyo Sung Park
Bo Wang
Adrien Cote
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University of California
University of Michigan
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Abstract

Una estructura zeolítica, que comprende la estructura general: M-L-M, en la que L es un fragmento de unión y M-L-M tiene la estructura I:**Fórmula** en la que R1 es H, en la que R2 y R3 son cada uno individualmente hidrógeno, un alquilo, un arilo, halo, ciano, o nitro, en la que M1 y M2 son cada uno zinc, donde la estructura tiene topología zeolítica seleccionada del grupo consistente en DFT, GIS y MER.

Description

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Porosidad y estabilidad de ZIFs. Se prepararon ciertas ZiFs a la escala del gramo, para permitir investigación detallada de sus propiedades. Un rasgo estructural de estas ZIFs es que ellas poseen poros grandes (11.6 y 14.6 Å en diámetro para ZIF-8 y -11, respectivamente) conectados a través de pequeñas aberturas (3.4 y 3.0 Å a través para ZIF-8 y -11, respectivamente). Los tamaños de poro son aproximadamente dos veces más grandes que los de sus contrapartes de zeolita, en virtud de las unidades de unión IM más largas; sin embargo, la existencia de cadenas laterales o anillos en la unión lleva los tamaños de abertura al límite inferior para tamices moleculares (Tabla 2).
Tabla 2. Característica estructural de ZIF-8 y -11 (compuestos de referencia) calculada a partir de análisis de cristal
individual por rayos X
ZIF-n
Diámetro de abertura de poro, Å anillo de 8 anillo de 6 anillo de 4 Diámetro de abertura de poro,Å Área superficial, m2/g Volumen de poro cm3/g
ZIF-8 -3.4 * 11.6 1,947 0.663 ZIF-11 3.0 3.0 * 14.6 1,676 0.582
Todos los cálculos se basaron en la Rutina de Volumen Libre del software CERIUS2 (versión 4.2; MatSci; Accelrys, Inc., San Diego; radio de muestra 1.4 Å, malla media) y en las estructuras de cristal individual por rayos X de ZIF-8 y -11 con retiro de huéspedes y promedio de efectos de desorden. *los tamaños de abertura de los anillos 4 son despreciables tanto en ZIF-S como -11.
Síntesis típica de ZIF. Se compraron bencimidazol, 2-metilimidazol, pentahidrato de nitrato de indio y hexahidrato de nitrato de cobalto, de la compañía Aldrich Chemical Co. e imidazol, N,N-dimetilformamaida (DMF), Nmetilpirrolidinona (NMP) de la compañía Fisher Scientific International Inc. Se obtuvo N,N-dietilformamida (DEF) BASF Corporation. Se compró el tetrahidrato de nitrato de zinc de la compañía EM Science. Todos los materiales de partida fueron usados sin purificaciones adicionales. Todas las operaciones experimentales fueron ejecutadas en aire. (Las síntesis de ZIF son ejemplificadas aquí por las síntesis de ZIF-8). Se disolvió una mezcla sólida de tetrahidrato de nitrato de zinc Zn(NO3)2·4H2O (0.210 g, 8.03x10-4 mol) y 2-metilimidazol (H-MeIM) (0.060 g, 7.31x10-4 mol) en 18 ml de DMF en un vial de 20-ml. Se tapó el vial y se calentó a una rata de 5°C/min a 140°C en un horno programable y se mantuvo esta temperatura por 24 h, luego se enfrió a una rata de 0.4°C/min a temperatura ambiente. Después de retirar el licor madre de la mezcla, se añadió cloroformo (20 ml) al vial. Se colectaron cristales incoloros poliédricos de la capa superior, se lavaron con DMF (10 ml x 3), y se secaron en aire por 10 min (rendimiento: 0.032 g, 25% basado en H-MeIM). El producto fue formulado usando microanálisis elemental como Zn(MeIM)2·(DMF)·(H2O)3 (C11H23N5O4Zn; calculado C, 37.25; H, 6.54; N, 19.74. Hallado C, 37.69; H, 5.22; N, 19.58). La pureza del producto ZIF-8 fue confirmada también mediante análisis PXRD.
Estudios de difracción de rayos X en cristal individual. Todos los datos de intensidad fueron colectados en un difractómetro SMART APEX CCD (Bruker-AXS, Madison, WI) con radiación de grafito transformada en monocromática MoK α(λ=0.71073 Å). Las estructuras fueron resueltas por métodos directos, y se hicieron síntesis sucesivas de diferencia de Fourier con el paquete de software SHELXTL (Bruker-AXS). Los datos de cristal son como sigue: ZIF-1 (crb, forma monoclínica): monoclínico, grupo espacial P21/n; a=9.740, b=15.266, c=14.936 Å, β=98.62°; V=2195.8 Å3, R1= 0.0423. ZIF-2 (crb, ortorrómbico form): ortorrómbico, grupo espacial Pbca; a=9.679, b=c=24.114 Å; V=5707 Å3, R=0.0591. ZIF-3 (dft): tetragonal, grupo espacial P42/mnm; a=b=18.970, c=16.740 Å; V=6024.3 (1) Å3, R1=0.0610. ZIF-4 (cag): ortorrómbico, grupo espacial Pbca; a=b=15.395, c=18.426 Å; V=4342.2 Å3, R1=0.0406. ZIF-5 (gar): cúbico, grupo espacial Ia3d; ao=21.9619 Å; V=0592.8 Å3, R1=0.0191. ZIF-6 (gis): tetragonal, grupo espacial I41/amd; a=b=18.515, c=20.245 Å; V=6940.2 Å3, R1=0.0642. ZIF-7: [forma sod-Zn(II)-PhIM]: hexagonal, grupo espacial R3; a=b=22.989, c=15.763 Å; V=7214 Å3, R1=0.0707. ZIF-8: [forma sod-Zn(II)-MeIM]: cúbico, grupo espacial I4/3m; ao=16.9910 Å; V=4905.2 Å3, R1=0.0314. ZIF-9 [forma sod-Co(II)-PhIM]: hexagonal, grupo espacial R3; a=b=22.9437, c=15.747 Å; V=7178.8 Å3, R1=0.0979. ZIF-10 (mer): tetragonal, grupo espacial I4/mmm; a=b=27.0608, c=19.406 Å; V=14211 Å3, R1=0.0636. ZIF-11 [forma rho-Zn(II)-PhIM]: cúbico, grupo espacial Pm3m; ao=28.7595 Å; V=23787.2 Å3, R1=0.0787. ZIF-12 [forma rho-Co(II)-PhIM]: cúbico, grupo espacial Pm3m; ao=28.7595 Å; V=23787.2 Å3, R1=0.1064. Las coordenadas atómicas están disponibles para descarga del Cambridge Crystallographic Data Centre citando los números de depósito 602535 (ZIF-1), 602536 (ZIF-2), 602537 (ZIF-3), 602538 (ZIF-4), 602539 (ZIF-5), 602540 (ZIF-6), 602541 (ZIF-7), 602542 (ZIF-8), 602543 (ZIF-9), 602544 (ZIF-10), 602545 (ZIF-11), 602546 (ZIF-12).
Estudios PXRD. Se colectaron datos de rayos X para polvo, usando un difractómetro D8-Advance ϴ-2ϴ (Bruker) en geometría de reflectancia Bragg-Brentano empleando radiación enfocada de línea CuKα filtrada de Ni a 1,600 W (40 kV, 40 mA) de potencia y equipado con un detector de centelleo Na(T1) ajustado con una rendija de entrada de radiación 0.2 mm. Las muestras fueron montadas sobre soporte de muestra con fondo cero, dejando caer los polvos desde una espátula de hoja ancha y luego nivelando la superficie de la muestra con una cuchilla de rasurar. Todas las muestras fueron molidas antes del experimento PXRD.
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= 0.0826] Completitud a theta = 24.71° 99.4 % Método de refinamiento matriz completa de mínimos cuadrados sobre F2 datos/restricciones/parámetros 1582 / 0 / 58 Bondad de ajuste sobre F 1.013 Indices R finales [I>2sigma(I)] R1 = 0.0642, wR2 = 0.2260 R índices (todos los gatos) R1 = 0.1037, wR2 = 0.2394. Diferencia más grande de pico y hueco 0.735 y -0.318 e.E-3 .
Coordenadas atómicas (x 104) y parámetros de desplazamiento isotrópico equivalente (Å2x 103) para ZIF-6. U(eq) es definido como un tercio del trazo del tensor Uij ortogonalizado.
x y z U(eq)
C(1)
3409(5) 5000 0 70(3)
C(2)
3477(6) 2500 1276(4) 75(3)
C(3A)
2317(9) 4963(9) 396(8) 82(5)
C(3B)
2316(9) 5323(8) -183(8) 79(4)
C(4A)
2410(10) 2869(8) 1020(9) 95(7)
C(4B)
2660(13) 2882(11) 590(17) 144(11)
N(1)
3019(3) 4683(3) 470(3) 81(2)
N(2)
3138(4) 3101(3) 1127(3) 86(2)
Zn(1)
3365(1) 4135(1) 1250 72(1)
O(1)
5000 2500 2250(20) 363(18)
Detalles experimentales y de refinamiento para ZIF-10 (MER). Se colocó un cristal prismático incoloro (0.20 x 0.10 x
0.10
mm3) de ZIF-10 en un capilar de borosilicato de 0.3 mm de diámetro junto con una pequeña cantidad de licor madre, el cual fue sellado a la llama y montado sobre un difractómetro Bruker SMART APEX CCD mientras se congelaba instantáneamente a 233(2) K en una corriente de nitrógeno líquido enfriada con N2 líquido. Se recolectó un total de 66076 reflexiones, de las cuales 3376 eran únicas y 1771 eran mayores a 4σ(I). El intervalo de ϴ fue de
1.06
a 26.37°. El análisis de los datos mostró una despreciable reducción durante la recolección. La estructura fue resuelta en el grupo espacial monoclínico I4/mmm con Z = 32 usando métodos directos. Se encontró que los átomos C5 y C8 estaban desordenados y con cada grupo modelado como su propia variable independiente libre. Todos los átomos diferentes a hidrógeno fueron refinados de manera anisotrópica con átomos de hidrógeno generados como esferas montadas sobre las coordenadas de sus átomos progenitores. El refinamiento final de matriz completa de mínimos cuadrados sobre F2 convergió a R1 = 0.0636 (F >2σF)) y wR2 = 0.2457 (todos los datos) con GOF = 1.059. Toda la densidad electrónica residual en el mapa F final estaba asociada cercanamente con las moléculas huésped dentro del poro de ZIF-10. Datos de cristal y refinamiento de estructura para ZIF-10: Fórmula empírica, C6 H6 N4
00.69 Zn; peso fórmula, 210.52; temperatura, 223 K; longitud de onda, 0.71073 Å; sistema cristalino, tetragonal; grupo espacial, I4/mmm; dimensiones de celda unitaria, a = 27.0608(18) Å, σ= 90°, b = 27.0608 Å, β= 90°, c =
19.406 Å, γ= 90°; volumen, 14211 Å3, Z, 32; densidad (calculada), 0.787 Mg/m3; coeficiente de absorción, 1.359 mm1; F(000), 3376; tamaño de cristal, 0.2 x 0.1 x 0.1 mm3; intervalo theta para recolección de datos, 1.06 a 26.37°. Intervalos de índice -33<=h<=33, -33<=k<=33,-24<=l<=24 Reflexiones colectadas 66076 Reflexiones independientes 3998 [R(int) = 0.1371] Completitud a theta = 26.37° 99.2 % corrección de absorción semi empírica de equivalentes Max. y min. transmisión 0.873 y 0.850 Método de refinamiento matriz completa de mínimos cuadrados sobre F2 datos/restricciones/parámetros 3998/0/118 bondad de ajuste sobre F2 1.059 Indices R finales [I>2sigma(I)] R1 = 0.0636, wR2 = 0.2183 Indices R (todos los datos) R1 = 0.1291, wR2 = 0.2457. Diferencia más grande de pico y hueco 0.557 y -0.501 e.E-3 .
Coordenadas atómicas (x 104) y parámetros de desplazamiento isotrópico equivalente (Å2 x 103) para ZIF-10. U(eq) está definido como un tercio del trazo del tensor Uij ortogonalizado.
x y z U(eq)
C(1)
3671(3) 1045(3) 2279(5) 109(3)
C(2)
3282(3) 1718(3) 2500 72(3)
C(3)
1874(2) 1874(2) 1477(5) 64(2)
C(4)
1918(3) 1376(3) 2479(4) 103(3)
C(5A)
2136(10) 255(8) 2226(19) 166(14)
C(5B)
2009(8) 250(6) 1709(11) 103(8)
C(8A)
3158(8) 1633(10) 354(8) 80(7)
C(8B)
3327(10) 1419(10) 358(8) 103(8)
C(6)
2684(4) 0 1521(5) 76(3)
10
imagen8

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US20070202038A1 (en) 2007-08-30
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