Hydrothermal synthesis of ZSM-5 membranes

Outline content 1.1. In situ growth 2.2. Secondary growth 3.3. Work plan

1.1. In situ growth

crystallization conditions Time & Temperature 165 ℃， 4 h 165 ℃， 12 h 165 ℃， 24 h 185 ℃， 4 h 185 ℃， 24 h

165 ℃， 12 h substrate 165 ℃， 24 h

Concentration Crystallization Time nucleation crystal growth C1C1 t1t1 t3t3 24 h t2t2 t4t4

020 surface roughness

2.2. Secondary growth

Random orientation Thickness ~1.8μm / / / Reproducity of secondary growth Random orientation good intergrowth

0.36TPAOH:1TEOS:58H 2 O:4EtOH aging Crystallization 98 ℃， 48 h Centrifugation r/min for 10 min The amount of seed can be easily controlled. The obtained seed can be stored in a desiccator for later use. weighing Ultrasonication 15 min Preparation of seed

Impact of seed concentration

Random orientation seed obtained after centrifugation 5 mg/mL in EtOH 25SiO 2 ： 9TPAOH ： 1450H 2 O: 100EtOH 100 ℃ ， 48 h A gel layer formedDiscrete zeolite particles PH = 12.49PH = 6.16 Seed coated

Effect of Al It facilitate the formation of the gel layer on the support. It retard zeolitization in this gel layer. JH Koegler, H Bekkum, et al., Zeolites,1997,19(4): Re Lai, Yushan Yan, George R. Gavalas, Micropor Mesopor Mater, 2000,37(1-2):9-19

good stable unstable agglomerate Si/Al Zeta potential(mv) Adv. Funct. Mater. 2008, 18, 952–958 Figure1. Zeta potential vs. PH for zeolite silicalite-1 crystals in aqueous suspension.

100% （ 101 ） 21.9% （ 051 ） 56.8% （ 051 ） 59.0% （ 051 ） PDF ： # ZSM-5:Al 2 O 3 54SiO 2 0mg/mL 2mg/mL 5mg/mL CPO(101)/(051) = ? Concentration （ mg/mL ） CPO I: intensity of （ 101 ） and （ 051 ） P: PDF# S: 0mg/mL 、 2mg/mL 、 5mg/mL

I:intensity of a peak P:powder reference S:film sample Characteristic planes and growing axis for MFI type zeolite Plane(Miller index)Growing axis Reference (501)a-axis[1] (051)b-axis[2] [(200)+(020)][a+b]-axis[1] (002)c-axis[2,3,4] (101) Oblique c-axis [3] (133) Oblique c-axis [1,2,4] [1] Microporous and Mesoporous Materials, (1): [2] Journal of Materials Chemistry, 1998, 8(10): [3]Microporous and Mesoporous Materials, 2009,123(1-3): [4]Microporous and Mesoporous Materials, 2008, 115(1-2): I:intensity of a peak P:powder reference S:film sample Fig.1. Typical shape of MFI-typ zeolite crystals CPO definition

100% （ 101 ） 21.9% （ 051 ） 56.8% （ 051 ） 59.0% （ 051 ） PDF ： # ZSM-5:Al 2 O 3 54SiO 2 0mg/mL 2mg/mL 5mg/mL CPO(101)/(051) = ? Concentration （ mg/mL ） CPO I: intensity of （ 101 ） and （ 051 ） P: PDF# S: 0mg/mL 、 2mg/mL 、 5mg/mL

3.3. Work plan

1 Sub-layer SiO 2 、 TiO 2 ZrO 2 、 Al 2 O 3 2 Cationic polymer layer 3 Characterization AFM XRD(pole figure 、 GID) Zeta potential measurement

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