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Nonaqueous Interfacial Polymerization-Derived Polyphosphazene Films for Sieving or Blocking Hydrogen Gas.

ABSTRACT: A series of cyclomatrix polyphosphazene films have been prepared by nonaqueous interfacial polymerization (IP) of small aromatic hydroxyl compounds in a potassium hydroxide dimethylsulfoxide solution and hexachlorocyclotriphosphazene in cyclohexane on top of ceramic supports. Via the amount of dissolved potassium hydroxide, the extent of deprotonation of the aromatic hydroxyl compounds can be changed, in turn affecting the molecular structure and permselective properties of the thin polymer networks ranging from hydrogen/oxygen barriers to membranes with persisting hydrogen permselectivities at high temperatures. Barrier films are obtained with a high potassium hydroxide concentration, revealing permeabilities as low as 9.4 × 10^-17 cm³ cm cm^-2 s^-1 Pa^-1 for hydrogen and 1.1 × 10^-16 cm³ cm cm^-2 s^-1 Pa^-1 for oxygen. For films obtained with a lower concentration of potassium hydroxide, single gas permeation experiments reveal a molecular sieving behavior, with a hydrogen permeance of around 10^-8 mol m^-2 s^-1 Pa^-1 and permselectivities of H₂/N₂ (52.8), H₂/CH₄ (100), and H₂/CO₂ (10.1) at 200 °C.

SUBMITTER: Radmanesh F

PROVIDER: S-EPMC10012169 | biostudies-literature | 2023 Mar

REPOSITORIES: biostudies-literature

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Nonaqueous Interfacial Polymerization-Derived Polyphosphazene Films for Sieving or Blocking Hydrogen Gas.

Radmanesh Farzaneh F Tena Alberto A Sudhölter Ernst J R EJR Hempenius Mark A MA Benes Nieck E NE

ACS applied polymer materials 20230209 3

A series of cyclomatrix polyphosphazene films have been prepared by nonaqueous interfacial polymerization (IP) of small aromatic hydroxyl compounds in a potassium hydroxide dimethylsulfoxide solution and hexachlorocyclotriphosphazene in cyclohexane on top of ceramic supports. Via the amount of dissolved potassium hydroxide, the extent of deprotonation of the aromatic hydroxyl compounds can be changed, in turn affecting the molecular structure and permselective properties of the thin polymer netw ...[more]

PMID: 36935655

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Project description:Molecular layer deposition (MLD) provides the opportunity to perform condensation polymerization one vaporized monomer at a time for the creation of precise, selective nanofilms for desalination membranes. Here, we compare the structure, chemistry, and morphology of two types of commercial interfacial polymerzation (IP) membranes with lab-made MLD films. M-phenylenediamine (MPD) and trimesoyl chloride (TMC) produced a cross-linked, aromatic polyamide often used in reverse osmosis membranes at MLD growth rates of 2.9 Å/cycle at 115 °C. Likewise, piperazine (PIP) and TMC formed polypiperazine amide, a common selective layer in nanofiltration membranes, with MLD growth rates of 1.5 Å/cycle at 115 °C. Ellipsometry and X-ray reflectivity results suggest that the surface of the MLD films is comprised of polymer segments roughly two monomers in length, which are connected at one end to the cross-linked bulk layer. As a result of this structure as well as the triple-functionality of TMC, MPD-TMC had a temperature window of stable growth rate from 115 to 150 °C, which is unlike any non-cross-linked MLD chemistries reported in the literature. Compared to IP films, corresponding MLD films were denser and morphologically conformal, which suggests a reduction in void volumes; this explains the high degree of salt rejection and reduced flux previously observed for exceptionally thin MPD-TMC MLD membranes. Using X-ray photoelectron spectroscopy and infrared spectroscopy, MLD PIP-TMC films evidenced a completely cross-linked internal structure, which lacked amine and carboxyl groups, pointing to a hydrophobic bulk structure, ideal for optimized water flux. Grazing-incidence wide-angle X-ray scattering showed broad features in each polyamide with d-spacings of 5.0 Å in PIP-TMC compared to that of 3.8 Å in MPD-TMC. While MLD and IP films were structurally identical to PIP-TMC, MPD-TMC IP films had a structure that may have been altered by post-treatment compared to MLD films. These results provide foundational insights into the MLD process, structure-performance relationships, and membrane fabrication.

Dataset Information

Nonaqueous Interfacial Polymerization-Derived Polyphosphazene Films for Sieving or Blocking Hydrogen Gas.

Publications

Nonaqueous Interfacial Polymerization-Derived Polyphosphazene Films for Sieving or Blocking Hydrogen Gas.

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