• Korean Chemical Engineering Research
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• 제57권6호
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• pp.749-757
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• 2019

Methyltrimethoxysilane (MTMS)과 trimethylethoxysilane (TMES)을 출발물질로 사용하여 여러 종류의 용매에 용해시킨 후 다양한 종류의 촉매를 사용해 물과의 가수분해 및 중축합반응을 진행시켜 비불소계 발수 코팅 용액을 제조하였다. 또한 이 코팅 용액을 냉연 강판 위에 스핀 코팅하고 열 경화시켜 발수 코팅 도막을 제조 하였다. 이 과정 중 촉매와 용매의 종류 변화가 생성된 코팅 도막의 발수성에 미치는 영향을 연구하였다. 강산인 염산과 질산을 촉매로 사용한 경우에는 용액 내에 siloxane polymer들의 응집이 발생한 흰색의 불투명 상태를 나타냈다. 반면에 약산인 아세트산, 인산과 옥살산을 사용한 경우에는 투명하고 침전이 없는 안정한 용액 상태를 보였다. 이로 인해 강산인 염산과 질산을 사용한 경우의 코팅 도막의 접촉각은 각각 $58^{\circ}$와 $92^{\circ}$로 낮은 발수성을 보인 반면에 약산인 아세트산, 인산과 옥살산으로 제조된 경우에는 각각 $101^{\circ}$, $103^{\circ}$, $116^{\circ}$의 접촉각을 보여 높은 발수성을 나타내었다. 또한 이소프로판올과 에탄올을 용매로 사용한 경우에는 용액 내에서 siloxane polymer들의 응집이 일어나 불투명한 침전이 발생한 상분리 현상을 보인 반면 메탄올, 에틸아세테이트와 메틸에틸케톤을 용매로 사용한 경우에는 투명하고 침전이 없는 안정된 상태를 나타내었다.

• 한국막학회:학술대회논문집
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• 한국막학회 1999년도 The 7th Summer Workshop of the Membrane Society of Korea
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• pp.39-42
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• 1999

Perfluoropolymers represent the ultimate resistance to hostile chemical environments and high service temperature, attributed to the presence of fluorine in the polymer backbone, i.e. to the high bond energy of C-F and C-C bonds of fluorocarbons. Copolymers of Tetrafluoroethylene (TEE) and 2, 2, 4Trifluoro-5Trifluorometoxy- 1, 3Dioxole (TTD), commercially known as HYFLON AD, are amorphous perfluoropolymers with glass transition temperature (Tg)higher than room temperature, showing a thermal decomposition temperature exceeding 40$0^{\circ}C$. These polymer systems are highly soluble in fluorinated solvents, with low solution viscosities. This property allows the preparation of self-supported and composite membranes with desired membrane thickness. Symmetric and asymmetric perfluoropolymer membranes, made with HYFLON AD, have been prepared and evaluated. Porous and not porous symmetric membranes have been obtained by solvent evaporation with various processing conditions. Asymmetric membranes have been prepared by th wet phase inversion method. Measure of contact angle to distilled water have been carried out. Figure 1 compares experimental results with those of other commercial membranes. Contact angles of about 120$^{\circ}$for our amorphous perfluoropolymer membranes demonstrate that they posses a high hydrophobic character. Measure of contact angles to hexandecane have been also carried out to evaluate the organophobic character. Rsults are reported in Figure 2. The observed strong organophobicity leads to excellent fouling resistance and inertness. Porous membranes with pore size between 30 and 80 nanometers have shown no permeation to water at pressures as high as 10 bars. However high permeation to gases, such as O2, N2 and CO2, and no selectivities were observed. Considering the porous structure of the membrane, this behavior was expected. In consideration of the above properties, possible useful uses in th field of gas- liquid separations are envisaged for these membranes. A particularly promising application is in the field of membrane contactors, equipments in which membranes are used to improve mass transfer coefficients in respect to traditional extraction and absorption processes. Gas permeation properties have been evaluated for asymmetric membranes and composite symmetric ones. Experimental permselectivity values, obtained at different pressure differences, to various single gases are reported in Tab. 1, 2 and 3. Experimental data have been compared with literature data obtained with membranes made with different amorphous perfluoropolymer systems, such as copolymers of Perfluoro2, 2dimethyl dioxole (PDD) and Tetrafluorethylene, commercialized by the Du Pont Company with the trade name of Teflon AF. An interesting linear relationship between permeability and the glass transition temperature of the polymer constituting the membrane has been observed. Results are descussed in terms of polymer chain structure, which affects the presence of voids at molecular scale and their size distribution. Molecular Dyanmics studies are in progress in order to support the understanding of these results. A modified Theodoru- Suter method provided by the Amorphous Cell module of InsightII/Discover was used to determine the chain packing. A completely amorphous polymer box of about 3.5 nm was considered. Last but not least the use of amorphous perfluoropolymer membranes appears to be ideal when separation processes have to be performed in hostile environments, i.e. high temperatures and aggressive non-aqueous media, such as chemicals and solvents. In these cases Hyflon AD membranes can exploit the outstanding resistance of perfluoropolymers.