polyethersulfone/cloisite 5a mxed matrix …mmm kepingan rata tidak simetri dihasilkan daripada...

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I I . POLYETHERSULFONE/CLOISITE I 5A MXED MATRIX MEMBRANES FOR GAS SEPARATION NOOR MAIZURA BINTI ISMAIL i L ] F : I I r i. [,_ r .-, 'l I.]NTVERSITI TEKNOLOGI MALAY.SIA

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Page 1: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

I

I

. POLYETHERSULFONE/CLOISITE I 5A MXED MATRIX MEMBRANES FORGAS SEPARATION

NOOR MAIZURA BINTI ISMAIL

iL]F

:II

r

i.[,_r .-,

'l

I.]NTVERSITI TEKNOLOGI MALAY.SIA

Page 2: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

POLYETHERSULFONE/CLOISITE 1 5A MIXED MATRX MEMBRANES FORGAS SEPARATION

NOOR MAIZURA BINTI ISMAIL

A thesis submiued in fulfilment of the

requirements for the award of the degree ofDoctor of Philosophy (Gas Engineering)

Faculty of Chemical and Energy Engineering

Universiti Teknologi Malaysia

OCTOBER 2015

Page 3: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

u1

Dedicated to my beloved husband

(Syuby bin Mohd Sidek)

my childrens

(Noorul Syuhada, Noorul Syafiqah, Syulvon Aiman)

rny parents

(Ismail bin Maidin, Zakiah binti Seman)

Siblings(Muhammad Nazri, Noor Maizia, Mohd Zalvi)

and friends for their continuous support and

encouragement throughout this study

Page 4: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

1V

ACKNOWLEDGEMENT

Bismillahirrahmanirrahim. All praises to ALLAH the Almighty, on whomultimately we depend for sustenance and inspiration to embark and complete thisstudy.

First and foremost, my sincere appreciation goes to my supervisor, Prof. Dr.Ahmad Fauzi Ismail, for giving me the opportunity to carry out this study andproviding me with continuous support. His timely and constructive comments as wellas enthusiasm have helped me to write this thesis into its final fcirm. I am alsograteful for the sincere and untiring efforts of my co-supervisor, Assoc. Prof. Dr.Azeman Mustafa who assisted me in all stages of this thesis writing.

In addition, I would like to acknowledge Prof. Dr.Tetsuo soga (NagoyaInstitute of Technology, Japan), for kindly providing me assistance with the sampleanalysis during the attachment. I am also indebted to Prof. Dr. Takeshi Matsuura(University of Ottawa, Canada) for his patient in giving me useful critics andvaluable advice throughout the entire course of this study. Special thanks to themembers of Advanced Membrane Technology Research Center (AMTEC) for thetechnical supports and assistance. Extended thanks dedicated to Mr. Sohaimi, Mr. NgBe Cheer, Mr. Razis Saidin, Dr. Juhana Jaafar, Dr. Farhana Azis, Dr. zulhairunAbdul Karim, Mrs. Siti Munira Jamil, Mrs. Nur Aimie Abdullah Sani, Ms. NadzirahMokhtar, Mr. Nik Abdul Hadi Mohd Nordin and others.

I would also like to acknowledge the generous financial assistance from theMinistry of Education Malaysia for the SLAB (Skim Latihan Akademik Bumiputra)scholarship and study leave provided by Universiti Malaysia Sabah.

Finally, my heartfelt gratitude to my beloved husband, children, parents andsiblings, who have strengthen and support me with their unconditional love, endlessencouragement, understanding and inspiration.

Page 5: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

ABSTRACT

Fabrication of mixed matrix membrane (MMM) with superior gas transportproperties is challenging due to the poor dispersion of the filler in the membrane andthe complicated interaction of polymer-clay surface. The purpose of this study is todevelop polymer-clay based MMM for carbon dioxide (COz) removal from methane(CH+) and to study the effects of interface voids and clay dispersion on gas

separation. Asymmetric flat sheet MMM from polyethersulfone (PES) and sonicatedcloisitel5A (C15A) clay particles was prepared by a controlled fabricationparameters and phase inversion technique. The impacts of adding C15A on theMMM properties were investigated by using morphological, structural, thermal,mechanical, functional group and performance analyses. In the first phase of thestudy, the effect of different loading of C15A was investigated. Significant changeson the membrane morphology and thermal stability were observed for the fabricatedMMMs. At 1 weighr% ClsA loading (PES/C15A1), MMM showed the best gas

transport properties wrfh 37% and l00o/o improvement on CO2 permeance andCOzICH+ selectivity, respectively. For the second part of the study, the state ofdispersion of the silicate layers in MMM was investigated by qualitative andquantitative analyses. Partial intercalated and exfoliated silicate layers in PES/C15A1contributed to the enhancement of the membrane mechanical properties. The increaseof tortuosity in MMM reduced the CH+ peflneance with a significant improvementfor the COzlCHq selectivity from22.57 to 46.89. Particle size measurement, particledensity measurement and free-path spacing measurement also demonstrated that thedispersion state in PES/C15A1 was striking with the increase in aspect ratio,dispersed single silicate layers, particle density and evidence of several tactoidclasses. It was discovered that high C15A loading (5 weight%) deteriorated thePES/C15A5 performance due to the interfacial voids. Hence in the third phase, C154was functionalized with 3-aminopropyl triethoxysilane coupling agent. Selectivityimprovement was observed on the modified-Cl5A MMM suggesting a betterinteraction between the clay surface and PES matrix. From this study, incorporationof C15A has shown great CO2lCHa separation enhancement and can be regarded as

potential filler for MMM.

Page 6: POLYETHERSULFONE/CLOISITE 5A MXED MATRIX …MMM kepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikel tanah liat cloisitel5A (ClsA) disonikasi melalui

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ABSTRAK

Pembuatan membran campuran matrik (MMM) dengan sifat-sifatpengangkutan gas yang unggul adalah mencabar disebabkan penyerakan. pengisiyang rendah dan kerumitan saling tindak antara permukaan polimer-pengisi. Tujuankajian ini adalah untuk menghasilkan MMM berasaskan polimer-tanah liat untukpenyingkiran karbon dioksida (Coz) daripada metana (CH4) dan mengkaji kesanlompang antara permukaan dan penyerakan pengisi terhadap pemisahan gas. MMMkepingan rata tidak simetri dihasilkan daripada polietersulfona (PES) dan partikeltanah liat cloisitel5A (ClsA) disonikasi melalui parameter pembuatan terkawal danteknik fasa-balikan. Kesan penambahan C15A terhadap sifat membran telah dikajimenggunakan analisa morfologi, strukfur, terma, mekanikal, kumpulan fungsi danprestasi. Pada fasa pertama kajian ini, kesan muatan C15A yang berbeza dalarnpenghasilan PES/C15A MMM telah dikaji. Perubahan yang ketarapada morfologidan kestabilan terma dapat diperhatikan ke atas MMM yang dihasilkan. Pada lYoberat muatan C15A (PES/C15A1), MMM menunjukkan sifat pengangkutan gas yangterbaik dengan peningkatan penelapan COz sebanyak 37% dan kememilihanCOz/CHq sebanyak 100%. Pada fasa kedua kajian ini, keadaan penyerakan lapisansilikat dalam MMM dikaji dengan analisis kuantitatif dan kualitatif. Lapisan silikatyang.separa interkalat dan terkelupas dalam PES/C15A1 menyumbang kepadapeningkatan sifat mekanikal membran. Peningkatan kelikuan dalam MMM telahmengurangkan kadar penelapan CHa dengan meningkatkan kememilihan CO2/CH4dari 22.57 kepada 46.89. Pengukuran saiz partikel, pengukuran ketumpatan partikeldan pengukuran jarak laluan-bebas juga menunjukkan bahawa keadaan penyerakandalam PES/C15A1 adalah ketara dengan peningkatan dalam nisbah aspek,penyerakan lapisan silikat tunggal, ketumpatan partikel dan kehadiran kelas taktoid.Kajian ini mendapatikadar muatan C15A yangtinggi (5%) dalam PES/C15A5 bolehmenyebabkan penurunan prestasi MMM akibat pembentukan lompang antarapermukaan. Oleh itu, pada fasa ketiga, C15A telah difungsikan dengan agengandingan 3-aminopropil trietoksilana. Peningkatan kadar kememilihan dapatdiperhatikan pada MMM dengan C15A yang telah diubah suai menunjukkaninteraksi yang lebih baik antara permukaan tanah liat dan matriks PES. Kajian inimenunjukkan, penggabungan C15A dengan PES telah menyebabkan peningkatanyang ketara dalam pemisahan COzlCHq dan Cl5A mempunyai potensi yang besarsebagai pengisi untuk MMM.