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PREPARATION OF SUPPORTED PALLADIUM MEMBRANE AND SEPARATION OF HYDROGEN
Morooka, Shigeharu,Kusakabe, Katsuki,Aoki, Kanna,Yokoyama, Shuichi 한국화학공학회 1996 Korean Journal of Chemical Engineering Vol.13 No.5
Palladium acetate was sublimed at a reduced pressure at 400℃, carried into the macropores of the porous wall of an α-alumina support tube and was decomposed there. A thin palladium membrane which was thus formed showed a hydrogen permeance of 10^6 ㏖·m ²·s ¹·Pa ¹ and a hydrogen/nitrogen permselectivity higher than 1000. The membrane was stable against hydrogen embrittlement even when the permeation temperature was varied between 100 and 300℃, and it was stable to sulfur or chlorine. To test the ability of this system for the separation of hydrogen and deuterium. a palladium disk was used instead of the prepared membrane since a definite membrane thickness was necessary for calculation. When H₂ and D₂ permeated through the membrane independently, the H/D permselectivity was approximately 7 at 150-200℃ under a feed side pressure of 0.4 MPa and a permeate side pressure of 0.1 MPa. When a mixture of H₂ and D, was fed, the H/D permselectivity was reduced to 1.2-1.6.
Development of A Microchannel Catalytic Reactor System
Kusakade, Katsuki,Morooka, Shigeharu,Maeda, Hideaki 한국화학공학회 2001 Korean Journal of Chemical Engineering Vol.18 No.3
The purpose of this article is to demonstrate the applicability of microreactors for use in catalytic reactions at elevated temperatures. Microchannels were fabricated on both sides of a silicon wafer by wet chemical etching after pattern transfer using a negative photoresist. The walls of the reactor channel were coated with a platinum layer, for use as a sample catalyst, by sputtering. A heating element was installed in the channel on the opposite surface of the reactor channel. The reactor channel was sealed gas-tight with a glass plate by using an anodic bonding technique. A small-scale palladium membrane was also prepared on the surface of a 50-㎛ thick copper film. In the membrane preparation, a negative photoresist was spin-coated and solidified to serve as a protective film. A palladium layer was then electrodeposited on the other uncovered surface. After the protective film was removed, the resist was again spin-coated on the copper surface, and a pattern of microslits was transferred by photolithography. After development, the microslits were electrolitically etched away, resulting in the formation of a palladium membrane as an assemblage of thin layers formed in the microslits. The integration of the microreactor and the membrane is currently under way.
Preparation of Microporous Silica Membranes for Gas Separation
Kim, Young Seok,Kusakabe, Katsuki,Morooka, Shigeharu,Yang, Seung Man 한국화학공학회 2001 Korean Journal of Chemical Engineering Vol.18 No.1
Microporous silica membranes for hydrogen separation were prepared on a γ-alumina coated α-alumina tube by sol-gel method. The reactants of sol-gel chemistry were tetraethoxysilane (TEOS) and methacryloxypropyltrimethoxysilane (MOTMS). The silane coupling agent, MOTMS, was added as a template in order to control the pore structure to the silicon alkoxide, TEOS. In particular, the microparous membranes were prepared by changing the molar ratio of MOTMS with respect to other substances, and their pore characteristics were analyzed. Then, the effects of thermal treatment on the micropore structure of the resulting silica membranes were investigated. The pore size of the silica membrane prepared after calcination at 400-700℃ was in the range of 0.6-0.7 nm. In addition, permeation rates through the membranes were measured in the range of 100-300℃ using H₂, CO₂, N₂, CH₄, C₂H_6, C₃H_6 and SF_6. The membrane calcined at 600℃ showed a H₂ permeance of 2×10^(-7)×10^(-7) molm^-2 s^-1Pa^-1 at permeation temperature 300℃, and the separation factors for equimolar gas mixtures were 11 and 36 for a H₂/CO₂ mixture and 54 and 132 for a H₂/CH₄mixture at permeation temperatures of 100℃ and 300℃, respectively.