Three phosphate esters >1–>3 were successfully synthesized from the reaction of 2-, 3- and 4-hydroxybenzaldehyde with phosphoryl chloride. Reactions of >1–>3 with benzidine in the presence of glacial acetic acid gave the corresponding novel phosphorus organic polymers >4–>6 containing the azomethane linkage. The structures of the synthesized compounds were confirmed by Fourier transform infrared spectroscopy, nuclear magnetic resonance and elemental analysis. Interesting physiochemical properties for the polymeric materials >4–>6 were observed using a combination of several techniques such as gel permeation chromatography, scanning electron microscopy, Brunauer–Emmett–Teller and nitrogen adsorption–desorption isotherm, Barrett–Joyner–Halenda and H-sorb 2600 analyzer. The mesoporous polymers >4–>6 exhibit tunable porosity with Brunauer–Emmett–Teller surface area (SABET = 24.8–30 m2·g–1), pore volume (0.03–0.05 cm3·g–1) and narrow pore size distribution, in which the average pore size was 2.4–2.8 nm. Polymers >4–>6 were found to have high gas storage capacity and physico-chemical stability, particularly at a high pressure. At 323 K and 50 bars, polymers >4–>6 have remarkable carbon dioxide uptake (up to 82.1 cm3·g–1) and a low hydrogen uptake (up to 7.4 cm3·g–1). The adsorption capacity of gasses for polymer >5 was found to be higher than those for polymers >4 and >6.
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