Synthesis and Characterization of Branched Sulfonated Poly(ether Sulfone-Ketone) Copolymer and Organic-Inorganic Nano Composite Membranes

2007 ◽  
Vol 534-536 ◽  
pp. 121-124
Author(s):  
Dong Hoon Lee ◽  
Hye Suk Park ◽  
Dong Wan Seo ◽  
Tae Whan Hong ◽  
Soon Chul Ur ◽  
...  

Branched sulfonated poly(ether sulfone-ketone) copolymer was prepared with bisphenol A, 4,4-difluorobenzophenone, sulfonated chlorophenyl sulfone (40mole% of bisphenol A) and THPE (1,1,1-tris-p-hydroxyphenylethane) as a branching agent. THPE was used 0.4 mol% of bisphenol A to synthesize branched copolymers. Organic-inorganic nano composite membranes were prepared with copolymer and a series of SiO2 nanoparticles (20 nm, 4, 7 and 10 wt%). The composite membranes were cast from dimethylsulfoxide solutions. The films were converted from the salt to acid forms with dilute hydrochloric acid. The membranes were studied by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. Branched copolymer and nano composite membranes exhibited proton conductivities from 1.12x10-3 to 6.04x10-3 S/cm2, water uptake from 52.9 to 62.4%, IEC from 0.81 to 1.21 meq/g and methanol diffusion coefficients from 1.2x10-7 to 1.5x10-7 cm2/S.

2007 ◽  
Vol 26-28 ◽  
pp. 835-838 ◽  
Author(s):  
Young Gi Jeong ◽  
Hye Seok Park ◽  
Dong Wan Seo ◽  
Seung Woo Choi ◽  
Whan Gi Kim

The Sulfonated poly(2,6-dimethyl-1,4-phenylene oxide) / poly(2,6-diphenyl-1,4-phenylene oxide) (S-PPO) was prepared by oxidative coupling polymerization with 2,6-dimethyl phenol, 2,6-diphenyl phenol, CuCl(І) and pyridine, and followed sulfonation with chlorosulfonic acid. Copolymer was consisted of 2,6-diphenyl phenol 30 mol% and 2,6-dimethyl phenol 70 mol%. Organic-inorganic nano composite membranes were prepared with copolymer and a series of SiO2 nanoparticles (20 nm, 4, 7 and 10 wt%). The composite membranes were cast from dimethylsulfoxide solution. The membranes were studied by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. S-PPO copolymer and nano composite membranes exhibited proton conductivities from 0.79×10-3 to 0.98×10-3 S/cm, water uptake from 21.70 to 24.77 %, IEC from 0.720 to 0.955 meq/g and methanol diffusion coefficients from 2.97×10-7 to 3.70×10-7 cm2/S.


2007 ◽  
Vol 534-536 ◽  
pp. 97-100
Author(s):  
Dong Hoon Lee ◽  
Hye Suk Park ◽  
Dong Wan Seo ◽  
Whan Gi Kim

Novel bisphenol-based wholly aromatic sulfonated poly(ether sulfone-ketone) copolymer and organic-inorganic composite membranes were prepared for operation 80°C in polymer electrolyte membrane fuel cell (PEMFCs). The copolymer were synthesized by direct aromatic nucleophilic substitution polycondensation of 4,4-difluorobenzophenone, 2,2’-disodiumsulfonyl- 4,4’-fluorophenylsulfone (40mole% of bisphenol A) and bisphenol A. Polymerization proceeded quantitatively to high molecular weight in N-methyl-2-pyrrolidinone at 180°C. Organic-inorganic composite membranes were obtained by mixing organic polymers with hydrophilic SiO2 obtained by sol-gel process. The polymer and a series of composite membranes were studied by FT-IR, 1HNMR, differential scanning calorimetry (DSC) and thermal stability. The proton conductivity as a function of temperature decreased as SiO2 content increased, but methanol permeability decreased. The nano composite membranes were found to poses all requisite properties; Ion exchange capacity (1.2meq./g), glass transition temperatures (164-183), and low affinity towards methanol (4.63-1.08x10-7 cm2/S).


2011 ◽  
Vol 695 ◽  
pp. 37-40
Author(s):  
Young Don Lim ◽  
Dong Wan Seo ◽  
Soon Ho Lee ◽  
Md. Monirul Islam ◽  
Hyun Mi Jin ◽  
...  

Poly(ether sulfone)s (PES) containing 25-75 mol % valeric acid were prepared with bisphenol A, bis(4-chlorophenyl)sulfone and 4,4-Bis(4-hydroxylphenyl)valeric acid using potassium carbonate in DMAc (dimethylacetamide) at 160 °C. Copolymers containing carboxylacid group were reduced to hydroxy group by BH3solution 1M in THF and NaBH4 co-catalyst. Sulfonated poly(ether sulfone)s (S-PES) were obtained by reaction of 1,3-propanesultone and the reduced copolymer (PES-OH) with potassium t-butoxide. Composite membranes were prepared with copolymers and SiO2nanoparticles(20 nm, 4-10 wt%). The composite membranes were cast from DMSO.A series of composite membranes were studied by1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermo gravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol.


2007 ◽  
Vol 124-126 ◽  
pp. 943-946
Author(s):  
Tae Whan Hong ◽  
Dong Hun Lee ◽  
Hae Suck Park ◽  
Dong Hwan Suh ◽  
Whan Gi Kim

Branched sulfonated poly(ether ketone sulfone) copolymer was prepared from1,1,1- tris(4-hydroxyphenyl) ethane, 4,4-difluorophenylsulfone, 3,3'-disodiumsulfonylbenzophenone (40 mol% of bisphenol A) and bisphenol A by polycondensation with the elimination of water in toluene and NMP at 160) in the presence of anhydrous potassium carbonate. Composite membranes were successfully cast from the control of organic polymer with SiO2 4-10 wt% of polymer in DMSO. The films were converted from the salt to acid forms with dilute hydrochloric acid. Organicinorganic composite membranes for operation in polymer electrolyte membrane fuel cells (PEMFCs) were characterized and cell-tested. The physico-chemical properties of all membranes were investigated their thermal properties, water uptake, DSC and thermogravimetric analyzer (TGA). Branched copolymer and nano composite membranes exhibit proton conductivities from 1.7x10-3 to 8.3x10-3 S/cm2, water uptake from 22 to 26%, IEC from 1.28 to 1.46 meq/g and methanol diffusion coefficients from 1.2x10-7 to 1.7x10-7 cm2/S.


2010 ◽  
Vol 658 ◽  
pp. 392-395 ◽  
Author(s):  
Dong Wan Seo ◽  
Young Don Lim ◽  
Soon Ho Lee ◽  
Md. Monirul Islam ◽  
Hyun Mi Jin ◽  
...  

Organic-inorganic Nano composite membranes were prepared by Sulfonated amine-poly(ether sulfone)s (S-APES)s and SiO2. S-APESs were prepared by nitration, reduction and sulfonation of poly(ether sulfone) (ultrason®-S6010). Poly(ether sulfone) was reacted with ammonium nitrate and trifluoroacetic anhydride to produce the nitrated poly(ether sulfone), and was followed by reduction using tin(Ⅱ)chloride and sodium iodide as reducing agents to give the amino-poly(ether sulfone). The S-APES was obtained by reaction of 1,3-propanesultone and the amino-poly(ether sulfone) (NH2-PES) with sodium methoxide. The different degrees of nitration and reduction of poly(ether sulfone) were successfully synthesized by an optimized process. Organic-inorganic nano composite membranes were obtained by mixing S-APES (45 %) with hydrophilic SiO2 (20 nm, 4-10 %) obtained by sol-gel process. Different contents of SiO2 of the S-APES were studied by FT-IR, 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermo gravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. The ion exchange capacity (IEC), a measure of proton conductivity, was evaluated. The nano composite membranes exhibit conductivities (25 °C) from 3.51 x 10-3 to 4.10 x 10-3 S/cm, water swell from 57.25 to 60.50 %, IEC from 0.68 to 0.73 meq/g, and methanol diffusion coefficients from 2.81 x 10-7 to 3.33 x 10-7 cm2/S at 25 °C.


2012 ◽  
Vol 488-489 ◽  
pp. 506-510 ◽  
Author(s):  
Sikander Rafiq ◽  
Zakaria Man ◽  
Abdulhalim Maulud ◽  
Nawshad Muhammad ◽  
Saikat Maitra

Composite membranes were prepared by incorporating inorganic silica nanoparticles into blends of polysulfone/polyimide (PSF/PI) membranes via sol-gel route. Morphological structures of the developed membranes were carried out by scanning electron microscopy (SEM). Spectroscopic analysis of the hybrid membranes were done by fourier transform infrared spectroscopy (FTIR) analysis. Differential scanning calorimetry (DSC) analysis shows that the glass transition temperature (Tg) increased from 209oC to 238oC in the hybrid membranes followed by thermogravimetric analysis (TGA) that showed significant improvement in thermal stability of the developed membranes.


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