Synthesis of Zeolite Composite Membranes for CO2 Separation
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1 Synthesis of Zeolite Composite Membranes for CO2 Separation April Sang Hoon Hyun, Dong Wook Shin, Young Eun Lee, Moon Hee Han*, and Churl Hee Cho* School of Materials Science & Engineering Yonsei University Seoul , Korea * Center of Functional Materials Research Korea Institute of Energy Research (KIER) Yuseong-Gu, Daejeon , Korea NanoPore Materials Lab.
2 Research Significance The ceramic membrane has been getting more attention and is being rapidly developed for the application of CO 2 separation / recovery in recent years. This is due to the worldwide restrictions against emission of CO 2 gas which causes the green-house effect. In particular, ceramic membranes have good thermal, chemical and structural stability, long life application, and capacity of having catalytic and electrical properties. In spite of their excellent properties, the potential applications of ceramic membranes for CO 2 / gas separation have not been fully realized because of current limitations such as lack of confidential manufacturing techniques, difficulty of microstructure control, and high production cost. Intensive studies should be continued in future for the development of these membranes and their practical application to CO 2 / gas separation. In this work, zeolite composite membranes (ZSM-5 and NaY types) have been synthesized using a hydrothermal treatment of porous α-alumina tubes in the reaction solution which was optimized for making each type of zeolite crystals. The CO 2 separation efficiency of synthetic zeolite membranes has been evaluated via measuring and examining both the gas permeabilities of various gases and the separation factors of CO 2 to N 2 in their mixtures. The effects of process parameters on CO 2 separation of zeolite membranes are also discussed. NanoPore Materials Lab.
3 Research Objectives - Optimization of zeolite types in the Na-Si-Al system for maximizing the high temperature CO 2 / N 2 separation efficiency - Development of the thin film technique for forming zeolite membrane layers on the porous ceramic support - Investigation of CO 2 / N 2 gas permeation and separation mechanisms in zeolite composite membranes at ordinary and high temperatures - Establishment of techniques for evaluating microstructures and defects of composite membranes - Development of zeolite composite membranes having the following performances and specifications: Time Item Membrane Type Mechanical Strength Pore size of Membrane layer Operating Temperature Permeability of mixed gas CO 2 / N 2 separation factor High temperature stability Final Tubular (L: 10 cm, D out < 1 cm) > 15 kg f / cm < 6.0 > 250 o C > 100 barrer > 50 > 30,000 h 1st year Tubular (L: 10 cm, D out < 1 cm) > 15 kg f / cm < 10 > 25 o C > 100 barrer > 10 > 100 h
4 Potential Applications of Ceramic Membranes for Gas Separation Field Separation Application Potential Degree H2/CO Syngas ratio adjustment Excellent Chemical H2/N2 Ammonia purge gas Excellent CO2/HC* Acid gas treatment Fair H2O/HC Natural gas treatment Excellent Petrochemical Environmental Others * Hydorcarbons H2/HC Refinery hydrogen recovery Excellent H2S/HC Sour gas treatment Excellent CO2/N2 Recovery of CO2 in effluent gas Good HC/Air HC recovery / pollution control Good O2/N2 O2 enrichment N2 generation Fair He/N2 He recovery Fair
5 Separation Mechanisms and Typical Configuration of Zeolite Composite Membranes for CO 2 separation Separation Mechanisms Expected in CO 2 / N 2 Separation : (1) Adsorption and Surface Diffusion (2) Activated Micropore Diffusion Typical Configuration: 1st zeolite layer ( < 10 ) (3) Molecular Sieving 2nd modification layer ( < 10 ) α-alumina Support < 1 µm < 10 µm < 2 mm
6 Overall Experimental Flow Chart Membrane Preparation α-alumina support Tubular type ( Dp=0.1~1.0 µm, Φp=34%~48%) by extrusion / slip-casting Powder Synthesis ZSM-5 NaY zeolite Silica sol + DI water + Sodium hydroxide + Aluminum nitrate + TPABr d (Solution #1) Water glass/colloidal silica+d.i.water+sodium aluminate+naoh (Solution #2) Hydrothermal treatment ( 90 ~ 180 o C) of support in reaction solution Reaction mixture Aging over 1~2 Days Drying Washing & filtering N 2 impermeability test Calcining (at 100~450 o C) Characterization CO 2 /N 2 permeability and separation factor measurement
7 Zeolite Membrane Synthesis and Separation Factor Measurement Systems Rupture disk Valve Pressure gage Thermocouple Temperature controller Vent Metering Valve Condensor Water trap Furnace <Schematic diagram of hydrothermal reactor system> H Supercritical Fluid Reidel Model vol% of reactor volume 6.47 vol% Pressure (psi) * 10 vol% 20 vol% 50 vol% 70 vol% 90 vol% 93 vol% 95 vol% 98 vol% Liquid Critical point vol% Gas Temperature ( o C) <P-T phase diagram of water in reactor> <Gas permeability / separation factor measurement system>
8 Morphologies of Zeolite Crystals (a) (b) 1 µm 3 µm (a) Z : ZSM-5 (b) Y Y Y : NaY Y Y Y (a) ZSM-5 zeolites synthesized at 170 o C for 24 h from solution #1 (b) NaY-type zeolites synthesized at 100 o C for 7 h from solution #2
9 Characterization of Silica-Modified ZSM-5 Composite Membrane SEM image of membrane surface Single gas permeation and CO 2 /N 2 separation factor of ZSM-5 composite membrane before and after silica modification Before silica modification After silica modification Permeate flux (mmol/m 2. s) CO 2 N Separation factor α(co 2 /N 2 ) Separation Factor T = 25 o C P = 4.5 bar X CO2 (feed) CO 2 /N 2 separation factor as a function of inlet CO 2 concentration
10 Background of Yonsei Ceramic Membranes Synthesis technique Sol-gel coating Sol-gel coating /silane coupling Sol-gel coating Pressurized sol-gel coating /Hydrothermal treatment Sol dipping /Hydrothermal treatment Organic templating aprroach Organic templating aprroach Hydrothermal treatment * Knudsen ideal separation factor of CO 2 /N 2 = 0.8 Material and structure (Tubular type) γ-al2o3/α-al2o3 Silane modified γ-al2o3/tio2 SiO2 modified γ-al2o3/α-al2o3 ZSM-5/α-Al2O3 SiO2 tightened ZSM-5/α-Al2O3 TPABr-templated SiO2/αAl2O3 Nanoporous amorphous silica Surface modified-ion exchanged NaY dddd zeolite/α-al 2 O 3 CO2/N2 Separation factor (> 50) (> 50) Reference (1,2,3) (3) (4) (1,5) (6) (7) Expected until 2004 Expected until ) Journal of American Ceramic Society, 77(12) (1994) 2) Journal of American Ceramic Society, 79(1) (1996) 3) Journal of Membrane Science, 120, (1996) 4) Journal of Materials Science, 34, (1999) 5) Journal of Materials Science, 34, (1999) 6) Journal of Materials Science Letters, 20, (2001) 7) Journal of Materials Science, 37, (2002)
11 Conclusions ZSM-5 and NaY type zeolites could be synthesized by the hydrothermal treatment of each reaction solution at 170 o C for 24h and 100 o C for 7h, respectively. Tubular zeolite composite membranes were also synthesized by the hydrothermal treatment of a α-alumina tube (pore size 0.1 ~ 1.0 µm) in the synthesis solution at the same conditions as those in case of powder synthesis. The ZSM-5 zeolite composite membrane surface-modified with the polymeric silica sol showed a high CO 2 / N 2 separation factor of 17.3 and a large permeability of 10-8 mol / m 2. s. Pa at room temperature. The permeation / separation mechanism of CO 2 through zeolite membranes was known to be a adsorption and surface diffusion. Compared to ZSM-5 zeolite membranes, the NaY type zeolite composite membrane under being developed seems to be more promising in practical points such as low synthesis temperature and easy surface modifications like ion-exchanging for applications of CO 2 or other gas separation.
12 References [1] S. H. Hyun and B. S. Kang, Synthesis of Nanoparticulate Silica Composite Membranes by the Pressurized Sol-Gel Technique, J. Am. Ceram. Soc., 77(12) 3093 (1994). [2] S. H. Hyun and B. S. Kang, "Synthesis of Titania Composite Membranes by the Pressurized Sol-Gel Technique," J. Am. Ceram. Soc., 79(1) (1996). [3] S. H. Hyun, S. Y. Jo, and B. S. Kang, "Surface Modification of -Alumina Membranes by Silane Coupling for CO 2 Separation," J. Membr. Sci., 120, (1996). [4] S. H. Hyun and B. S. Kang, " - Alumina Composite Membranes Modified with Microporous Silica for CO 2 Separation," J. Mater. Sci., 34, (1999). [5] S. H. Hyun, J. K. Song, B. I. Kwak, J. H. Kim, and S. A. Hong, "Synthesis of ZSM-5 Zeolite Composite Membranes for CO 2 Seperation," J. Mater. Sci., 34, (1999). [6] B. I. Kwak, S. H. Hyun, and G. T. Kim, "CO 2 Separation Characteristics of ZSM-5 Composite Membranes Synthesized by the Hydrothermal Treatment," J. Mater. Sci. Lett.,20, (2001) [7] S. M. Yang, Y. E. Lee, S. H. Hyun, and C. H. Lee, "Organic-Templating Approach to Synthesis of Nanoporous Silica Composite Membranes (I) : TPA- Templating and CO 2 Separation," J. Mater. Sci., 37, (2002). [8] Z.A.E.P. Vroon, K. Keizer, A.J. Burggraaf, and H. Verweij, Preparation and Characterization of Thin Zeolite MFI Membranes on Porous Supports, J. Membr. Sci., 144, (1998) [9] Y. Hasegawa, K. Watanabe, K. Kusakabe, and S. Morooka, The Separation of CO 2 Using Y-type Zeolite Membranes Ion-exchanged with Alkali Metal Cations, Separation and Purification Technology, 22-23, (2001).
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