Zeolite MFI Membranes on Low Cost Polymer Supports

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1 Zeolite MFI Membranes on Low Cost Polymer Supports Han Zhang Ph.D. defense, June 27, 2017 Advisers: Prof. Michael Tsapatsis Prof. Christopher W. Macosko Committee: Prof. Alon McCormick (Chair) Prof. Paul Dauenhauer Prof. Ilja Siepmann

2 1. Background Zeolites and zeolite membranes 2

3 Introduction to zeolites Zeolites are microporous, aluminosilicate minerals made from interlinked tetrahedra of silica (SiO 4 ) and alumina (AlO 4 ). The pore structure of zeolite MFI. M. Snyder, M. Tsapatsis. Angew. Chem. Int. Ed. 2007, 46,

4 Introduction to zeolite MFI membrane separation C 1 -C 4 C 5 -C 12 C 12 -C 16 C 15 -C 18 C 17 -up C 20 -up Global xylene demand Global xylene demand p-xylene m-xylene o-xylene 5.8 Å 6.8 Å 6.8 Å b.p. 138 ⁰C b.p. 144 ⁰C b.p. 139 ⁰C Thermal separation: 1. Fractional crystallization 2. Parex process p-xylene 99.9% purity Total: 47.2 million tons (2014), 80.1 million tons (2022 projected) PET bottles Images: 4

5 Introduction to zeolite MFI membrane separation C 1 -C 4 n-butane iso-butane C 5 -C 12 + C 12 -C 16 Separated by distillation C 15 -C 18 C 17 -up n-butane iso-butane C 20 -up Fuel gas Gasoline blending Chemical feedstock Refrigerant Global butane demand: 210 million tons (2013); 250 million tons, i.e. $203 billion (2020 projected) Image: 5

6 How to make MFI membrane Seeded secondary growth Crystal Structure (nm) Shaped Crystal (10-100nm) For a Review: Mark A. Snyder, Michael Tsapatsis, Angew. Chem. Int. Ed. 2007, 46, Oriented Monolayer of Crystals 6

7 Requirements What requirements for an excellent membrane? High permeance (thin, b-oriented) High selectivity (eliminate defects) MFI nanosheet 3.2 nm thick K. Varoon, et al. Science 2011, 334, 72. 7

8 Multilamellar MFI nanosheets M. Choi, et al. Nature 2009, 461,

9 MFI nanosheets Layered zeolite MFI nanosheets Purification Polymer M. Choi, et al. Nature 2009, 461, 246. K. Varoon, et al. Science 2011, 334, 72. K. Varoon, et al. AIChE J. 2013, 59, Density gradient centrifugation 9

10 Quartz support Quartz fiber disc 350 nm stober silica coating MFI nanosheets coating 50 nm stober silica coating K.V. Agraval, et al., AICHE J. 2013, 59,

11 b-oriented, sub-100 nm MFI membrane After secondary growth Cross section 500 nm 500 nm Calcined at 500 ⁰C to remove organic templates 11

12 Performance Permeance of i = Separation Factor SF of i/j = molar flow of i membrane area pressure difference concentration of i in permeate concentration of j in permeate concentration of i in feed concentration of j in feed p-xylene o-xylene At 150 ⁰C Permeance: 1~ mol/m 2 -s-pa SF: up to 10,000 M.Y. Jeon, et al., Nature 2017, 543, 690. n-butane iso-butane At 25 ⁰C Permeance: 1~ mol/m 2 -s-pa SF: up to 75 K.V. Agraval, et al., Adv. Mater. 2015, 27,

13 Motivation of my research project Commercialization of MFI membrane is not successful High cost (ceramic support, ~$5000/m 2 ) Low scalability Possible solution Replace the ceramic supports by polymer supports (~$20) Polymer flat sheets and hollow fibers Challenge Improve nanosheet exfoliation yield Membrane growth on polymer support How to remove templates without damaging polymer support 13

14 2. Mild detemplation methods Low temperature calcination UV/ozone treatment 14

15 Thermal and UV/ozone treatment of powder MFI Elemental analysis of C(a) and N (b) after calcination at different T max Detemplation from bulk starts at 280 ⁰C I. Jirka, et al. Micropor. Mesopor. Mater. 2011, 137, 8. A.N. Parikh, et al. Micropor. Mesopor. Mater. 2004, 76,

16 Permeance (mol/pa-s-m 2 ) SF Low temperature thermal calcination 1E-6 1E-7 1E-8 1E-9 1E-10 1E-11 p-/o-xylene SF n-/i-butane SF 1E Calcination temperature ( o C) p-xylene permeance n-butane permeance The nominal lowest detemplation temperature is 280 ⁰C

17 UV/ozone treatment Single gas permeance 17

18 Summary Two mild detemplation methods confirmed by MFI membranes: 1. Thermal treatment at 280 ⁰C. 2. UV/ozone treatment for 6 h. Next steps: 1. Grow MFI membrane on polymer support. 2. Treated with these two mild detemplation treatment. 18

19 3. MFI membrane grown on polymer support and mild detemplation treatment 19

20 MFI membrane growth on polyethersulfone support stainless steel mesh mesh-pes support 1 2 Non-solvent induced phase separation 1. Polymer solution casting onto mesh 2. Immersion in water bath 20

21 MFI membrane on PES support zeolite membrane with mesh-pes as support Nanosheet coating on mesh-pes coating After secondary growth N 2 permeance at room temperature : mol/m 2 -s-pa 500 nm Ready to remove templates with mild detemplation treatment 21

22 Cracks after UV/ozone treatment for 1.5 h 200 µm 50 µm 20 µm 1 µm 22

23 Peeled-off after UV/ozone treatment for 4 h 1 mm Possible reason: polymer damaged by UV light. 23

24 Polybenzimidazole (PBI) Tg ~ 495 ⁰C 10 cm 200 nm 24

25 Cracks formed after treatment at 250 ⁰C for 8 h 100 µm 20 µm MFI membrane grown on PBI support PBI: polybenzimidazole, Tg ~ 495 ⁰C Reason: mismatch of linear thermal expansion coefficients between MFI membrane layer and PBI support 25

26 Summary Successful MFI membrane growth on polymer support. But both the two mild detemplation methods lead to cracks. How about remove organic templates first? 26

27 4. Open-pore MFI nanosheets 27

28 Direct piranha solution treatment Piranha treatment Sonication Multilamellar MFI Detemplated MFI nanosheets in water Piranha solution is a mixture of H 2 SO 4 and H 2 O 2 (3:1) 28

29 Intensity (a.u.) Direct piranha solution treatment Piranha 4 times Piranha 3 times Piranha 2 times (d) (c) (b) 1 µm 1 µm ML-MFI (a) theta (degree) 4 times 3 times 2 times 1 time 29

30 Coating on porous PBI support No n-/iso-butane selectivity 30

31 Open-pore nanosheets after exfoliation 10 cm 10 cm 200 nm 200 nm 31

32 Schematic representation of the spinning apparatus Parameters: dope solution composition, dope solution flow rate, bore solution flow rate, gap distance, take up speed, coagulation bath temperature. 32

33 Spinning machine Polyethersulfone (PES), polybenzimidazole (PBI), and polyimide (PI) hollow fibers have been successfully fabricated. 33

34 Hollow fiber membrane module Membrane module Permeate side 34

35 Nanosheet coating on hollow fiber Outer surface Cross section PES Dry state PES Wet state 200 nm 200 µm Coating on PBI Coating on PES PBI Dry state PBI Wet state 50 µm 20 µm Photos from Xuekui Duan 35

36 Potential application Hybrid membrane-distillation process Nitish Mittal, et al., J. Membr. Sci. 2016, 520,

37 Conclusion Open-pore MFI nanosheets were synthesized by piranha solution treatment. Butane isomer selective membranes from simple coating of the open-pore MFI nanosheets. Attempt to coat nanosheets on hollow fibers 37

38 5. Exfoliation of layered zeolite 38

39 MFI nanosheets Layered zeolite Yield was low Purification Polystyrene MW 35,000 K. Varoon, et al. Science 2011, 334, 72. K. Varoon, et al. AIChE J. 2013, 59, Density gradient centrifugation 39

40 Exfoliation of clay Stepwise mechanism for clay exfoliation by melt compounding polymer diffusion shear stress T.D. Fornes, et al. Polymer 2001, 42,

41 Exfoliation of layered materials Measure stress response Clay + polystyrene Sample Apply strain deformation K. Haraguchi, et al. Macromolecules 2005, 38, M. Dolgovskij. Thesis γ = γ 0 sin ωt σ = σ 0 sin(ωt + δ) G = (σ 0 / γ 0 ) cos δ G = (σ 0 / γ 0 ) sin δ tan δ = G / G house-of-cards structure Use G (storage modulus) plateau value to access exfoliation level 41

42 Nanosheet exfoliation by melt-compounding Multi-lamellar MFI T, viscosity, shear force, diffusivity Exfoliation yield was indicated by G plateau value (exfoliated nanosheets can form network in polymer matrix) Polymer Polystyrene (Mw 1,300 ) and multi-lamellar MFI at 4% loading 42

43 Clay exfoliation constant viscosity mixing PS 1,300 PS 13,000 PS 21,000 PS bimodal PS1,100+PS130,000 No plateau 43

44 Conclusion ML-MFI exfoliation: balance yield and particle size Clay exfoliation: optimum molecular weight of 13,000 44

45 Summary Ultra-thin MFI membrane Lowest nominal detemplation temperature: 280 C UV/ozone treatment for 6 h Polymer hollow fibers PBI, PES, PI Nanosheet coating Open-pore nanosheets Piranha solution treatment Selective membrane on polymer support by simple coating Nanosheet exfoliation Shear stress dominates MFI exfoliation Optimal molecular weigh 13,000 for clay exfoliation 45

46 Acknowledgements Prof. Michael Tsapatsis, Prof. Christopher W. Macosko Committee members: Prof. Alon McCormick, Prof. Paul Dauenhauer, Prof. Ilja Siepmann Tsapatsis group members, especially: Dr. Qiang Xiao, Xuekui Duan, Dr. Neel Rangnekar, Prashant Kumar, Dr. Kumar Varoon Agraval, Dr. Berna Topuz, Dr. Xianghai Guo and Dr. Nanjun Li Macosko group members, especially: David Lundberg, Jun Xu, Dr. David Giles, Dr. Donglin Tang, Dr. Zaifei Wang Frank Onorato (industrial consultant) Charfac staff: Dr. Nick Seaton, Dr. Jason Myers, Dr. Bing Luo My family and friends in China and US. Financial support: ARPA-E (Award No. DE-AR ( )) 46

47 Thank You. 47

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