• Clean Technology
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• v.13 no.1 s.36
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• pp.79-84
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• 2007

Separation of ethylene from ethane and propylene from propane have been conducted using facilitated olefin transport membrane with SPEEK-Ag (Ag substituted sulfonated poly(ether ether ketone)). SPEEK was prepared by the sulfonation of PEEK using cone. $H_2SO_4$ and the reaction time affected the degree of sulfonation (DS) of the resulting SPEEK. SPEEK-Ag composite membrane was formed by soaking SPEEK in the polyester support into the Ag salt solution. With increasing the concentration of SPEEK in MeOH, the thickness of SPEEK on the polyester increased. The selectivity and the flux of SPEEK-Ag membrane for the separation of ethylene/ethane and propylene/propane were changed by the thickness of SPEEK layer on the top of polyester support. The anion of silver salt also affects the membrane performance.

• Clean Technology
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• v.10 no.3
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• pp.169-176
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• 2004

Sulfonated ionomer membranes, sulfonated poly(ether ether)ketone (SPEEK)-$AgNO_3$, were prepared and tested for separation of the isoprene/n-pentane mixtures. The facilitated transport membranes showed good selectivity and permeance of isoprene over n-pentane and long-term stability. Depending on various reaction conditions, the degree of sulfonation (DS) of SPEEK was measured by 1H NMR spectroscopy and the performance of the membranes was affected by the DS of SPEEK as a whole. As the DS of SPEEK was increased, the selectivity of isoprene over n-pentane increased and eventually reached a maximum selectivity of 850 ~ 900 and the stability of that was continued more than 100 h.

• Membrane Journal
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• v.25 no.5
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• pp.447-455
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• 2015

In this study, Polysulfone (PSf) and polyetherimide (PEI) as the anion exchange polymers were aminated in the different ratio whereas the polyether ether ketone (PEEK) as the cation exchange polymer was sulfonated. The bipolar membranes of SPEEK (sulfonated PEEK)/APSf (aminated PSf) and SPEEK/APEI (aminated PEI) were prepared by the double-casting method. The surfaces of bipolar membranes were fluorinated in accordance with the amination ratio and applied to produce the hypochlorite. As the amination increased, the hypochlorite concentration is also increased. Typically, for SPEEK/APSf 3 : 1 membrane, the produced hypochlorite concentration was 61.0 ppm and its durability was 220 min for the non-fluorinated membrane while for the fluorinated membrane, the concentration of 58.6 ppm and its durability lasted 570 min. Also for SPEEK/APEI 3 : 1 membrane, the hypochlorite concentrations of 60.1 ppm and 58.3 ppm for before- and after-fluorination, respectively were observed whereas the durability was remarkably developed from 150 min to 440 min. Therefore, the surface fluorination takes an important role for the development of the membrane durability.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.14 no.5
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• pp.2529-2535
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• 2013

Sol-gel method was utilized to prepare SPEEK/PWA electrolyte composite membranes. TEOS was used as a precursor and phosphotungstic acid(PWA) as a catalyst for the sol-gel reaction. It was observed through FE-SEM analysis that the PWA and silica nanoparticles were uniformly dispersed into the polymer matrix. The water uptake of SPEEK/PWA/silica composite membranes was less affected by TEOS concentration at higher TEOS contents, while the water uptake decreased as TEOS concentration increased at lower TEOS contents. The proton conductivity of the composite membranes showed similar trend as the water uptake of the composite membranes. The methanol permeability of SPEEK/PWA/silica composite membranes decreased as TEOS concentration increased.

• Journal of the Korean Chemical Society
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• v.57 no.5
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• pp.625-633
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• 2013

A type of polycyclotriphosphazene derivative (PCTPD), hexasulfanilic acid polycyclotriphosphazene (HSACP) and HSACP grafting SPEEK, sulfonated poly[2-(petachloropolycyclotriphosphazene-oxy)] etheretherketone (SPPSACPEEK) were synthesized, which were characterized by FTIR and $^{31}P$ NMR. Then three types of composite membranes such as HSACP grafting SPEEK, HSACP blending SPEEK, and nano $Y_2O_3$ doping and HSACP grafting SPEEK, respectively, were continuously prepared by solution-casting method. Comparing to SPEEK membranes with different amount of HSACP grafted or blended, grafting 15 wt% HSACP and doping 10 wt% nano $Y_2O_3$ SPEEK membrane conducted outstanding overall behavior of proton conductivity reaching $3.18 {\times}10^{-2}$ S/cm at $90^{\circ}C$ which was merely junior to SPEEK with 15 wt% HSACP grafted, methanol permeability coefficient getting $9.46{\times}10^{-8}cm^2{\cdot}s^{-1}$, swelling degree of 20.9% and solid residue of 98.98% which was superior to all specimen.

• Applied Chemistry for Engineering
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• v.24 no.3
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• pp.247-252
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• 2013

Sulfonated poly(ether ether ketone) (SPEEK) with a certain degree of sulfonation were synthesized by reacting PEEK and sulfuric acid at different reaction time. Then ion-selective composite carbon electrodes (ISCCE) were fabricated by coating the prepared SPEEK on the surface of carbon electrodes. The specific capacitance and resistance of the ISCCE were analyzed by electrical impedance spectroscopy. The ion exchange capacities (IEC) of the SPEEKs were measured in the range of 1.60~2.57 meq/g depending on the sulfonation time. The SPEEK more than 2.5 meq/g of IEC was considered unsuitable for fabricating the ISCCE because it was dissolved in water. The specific capacitance of the prepared ISCCE increased with increasing the IEC of coated SPEEKs and the capacitance was improved up to about 20% compared to that of uncoated carbon electrode. In addition, the electrical resistance of coating layer decreased significantly with increasing the IEC of coated SPEEKs. It is expected that the desalination efficiency of conventional capacitive deionization process can be improved by using the prepared ISCCE coated with SPEEK.

• Transactions of the Korean hydrogen and new energy society
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• v.20 no.2
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• pp.95-103
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• 2009

In order to improve the electrochemical, mechanical and electrocatalytic characteristics, engineering plastic of polyether ether ketone (PEEK) as polymer matrix was sulfonated (SPEEK) and the organic-inorganic blend composite membranes has been prepared by loading heteropoly acids (HPAs), including tungstophosphoric acid (TPA), molybdophosphoric acid (MoPA), and tungstosilicic acid (TSiA). And then these were covalently cross-linked (CL-SPEEK/HPA) as the electrolyte and MEA of polymer electrolyte membrane electrolysis (PEME). As a result, the optimum reaction conditions of CL-SPEEK/HPA was established and the electrochemical characteristics such as ion conductivity ($\sigma$) were in the order of magnitude: CL-SPEEK /TPA30 (${\sigma}=0.128\;S/cm^{-1}$) < /MoPA40 (${\sigma}=0.14\;S/cm^{-1})$ < /TSiA30 (${\sigma}=0.22\;S/cm^{-1}$) at $80^{\circ}C$, and mechanical characteristics such as tensile strength: CL-SPEEK /TSiA30 $\fallingdotseq$ /MoPA40 < /TPA30. Consequently, in regards of above characterisitics and oxidation durability, the CL-SPEEK/TPA30 exhibited a better performance in PEME than the others, but CL-SPEEK/MoPA40 showed the best electrocatalytic activity of cell voltage 1.71 V among the composite membranes. The dual effect of higher proton conductivity and electrocatalytic activity with the addition of HPAs, causes a synergy effect.

• Korean Chemical Engineering Research
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• v.46 no.1
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• pp.164-169
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• 2008

In this study, the facilitated transport membranes, poly (ether ether)ketone (SPEEK)-Ag salts layers on top of polycarbonate supports membrane, were prepared and tested for the separation of propylene/propane. SPEEK was synthesised using PEEK and $H_2SO_4$. Experiments were porformed at room temperature and feed pressures up to 30 psig. The SPEEK-Ag salt membranes showed good selectivity for propane over propylene. With increasing the concentration of SPEEK in MeOH, 5~20 wt%, the thickness of SPEEK membrane on the polycarbonate increased. The selectivity and permeance of SPEKK-Ag membrane for propylene/propane were changed by membrane thickness and concentration of Ag salts.

• Transactions of the Korean hydrogen and new energy society
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• v.28 no.1
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• pp.17-23
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• 2017

Polyether ether ketone (PEEK) composite including tungstophosphoric acid(TPA) membranes have been intensively investigated for polymer electrolyte membrane water electrolysis (PEMWE) and thus covalently linked sulfonated polyether ether ketone (CL-SPEEK) with captured TPA composite membranes were prepared and characterized. Sulfonated polyether ether ketone (SPEEK) was prepared in sulfonation of PEEK and was cross-linked with 1,4 diiodobutane. The carbonyl group of SPEEK was reduced with $NaBH_4$ and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The TPA captured composite was prepared in reaction of TPA with 3-mercaptopropyltrime thoxysilane (MPTMS). The polymer composite membranes showed better thermostability and electrochemical properties than SPEEK. The membranes were prepared by sol-gel casting method. The polymer composite membrane featured 0.1285 S/cm of proton conductivity at $80^{\circ}C$ and outstanding durability.

• Transactions of the Korean hydrogen and new energy society
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• v.28 no.4
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• pp.338-344
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• 2017

Polyoxometal molybdophosphoric acid (MoPA) bonded polyether ether ketone (PEEK) composite membrane for water electrolysis has been investigated. The composited membrane, covalently cross linked (CL) sulfonated polyether ether ketone (SPEEK) with a bonded MoPA, was prepared in sulfonation of PEEK, cross linkage reaction with 1,4-diiodobutane, and addition with MoPA. PEEK was covalently cross-linked with 1,4-diiodobutane to improve mechanical strength and was added with MoPA to increase proton conductivity. MoPA should be fixed to back bone of SPEEK to prevent bleeding out. Therefore, the carbonyl group of SPEEK was reduced with NaBH4 and 3-isocyanatepropyltriethoxysilane (ICPTES) was added. The MoPA bonded composite was produced in the reaction of MoPA with 3-mercaptopropyltrimethoxvsilane (MPTMS). In conclusion, MoPA bonded CL-SPEEK composite membrane featured 0.129 S/cm of proton conductivity at $80^{\circ}C$, and 2,156 hours of chemical stability in Fenton test. These properties are better than those of membranes of other SPEEK system.