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By Meiling Ji

Hydrothermal synthesis of ZSM-5 membranes. By Meiling Ji. Outline content. 1. In situ growth. 2. Secondary growth. 3. Work plan. 1. In situ growth. 165 ℃， 4 h. crystallization conditions Time & Temperature. 165 ℃， 12 h. 185 ℃， 4 h. 165 ℃， 24 h. 185 ℃， 24 h. substrate.

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By Meiling Ji

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  1. Hydrothermal synthesis of ZSM-5 membranes By MeilingJi

  2. Outlinecontent 1. In situ growth 2. Secondary growth 3. Work plan

  3. 1. In situ growth

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

  5. substrate 165℃，12 h 165℃，12 h 165℃，24 h 165℃，24 h

  6. Concentration nucleation C1 crystal growth t1 t2 t4 t3 24 h Crystallization Time

  7. surface roughness 020

  8. 2. Secondary growth

  9. Reproducity of secondary growth 332/051 Random orientation good intergrowth 101 151/303 Random orientation Random orientation 200/020 133 Random orientation Thickness ~1.8μm

  10. Preparation of seed 0.36TPAOH:1TEOS:58H2O:4EtOH aging Ultrasonication 15 min Crystallization 98℃，48 h Centrifugation 10000 r/min for 10 min weighing • The amount of seed can be easily controlled. • The obtained seed can be stored in a desiccator for later use.

  11. Impact of seed concentration 0mg/mL 2mg/mL 5mg/mL

  12. Seed coated Random orientation 25SiO2：9TPAOH：1450H2O: 100EtOH 100 ℃ ，48 h seed obtained after centrifugation 5 mg/mL in EtOH A gel layer formed Discrete zeolite particles PH = 12.49 PH = 6.16

  13. JH Koegler, H Bekkum, et al., Zeolites,1997,19(4): 262-269. • Effect of Al • It facilitate the formation of the gel layer on the support. • It retard zeolitization in this gel layer. Re Lai, Yushan Yan, George R. Gavalas, Micropor Mesopor Mater, 2000,37(1-2):9-19

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

  15. 5mg/mL 2mg/mL 100%（101） 21.9%（051） 0mg/mL 100%（101） 56.8%（051） 100%（101） 59.0%（051） PDF：#44-0003 ZSM-5:Al2O354SiO2

  16. CPO definition Characteristic planes and growing axis for MFI type zeolite I:intensity of a peak P:powder reference S:film sample I:intensity of a peak P:powder reference S:film sample [1] Microporous and Mesoporous Materials, 1999. 28(1): 185-194 [2] Journal of Materials Chemistry, 1998, 8(10): 2217-2221. [3]Microporous and Mesoporous Materials, 2009,123(1-3):113-112 [4]Microporous and Mesoporous Materials, 2008, 115(1-2): 113-122. Fig.1. Typical shape of MFI-typ zeolite crystals

  17. 5mg/mL 2mg/mL 100%（101） 21.9%（051） 0mg/mL 100%（101） 56.8%（051） 100%（101） 59.0%（051） PDF：#44-0003 ZSM-5:Al2O354SiO2

  18. 3. Work plan

  19. Work plan +++++++ +++++++ +++++++

  20. Q&A Thanks for your time！

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