On April 17, 2013, Qian, Guodong; Rao, Xingtang; Cai, Jianfeng; Yu, Jiancan; Cui, Yuanjing; Yang, Yu; Wang, Zhiyu; Fan, Xianping; Wang, Minquan published a patent.Safety of 5,5′-(Pyridine-2,5-diyl)diisophthalic acid The title of the patent was Metal organic framework substance for acetylene adsorption and storage and its preparation method. And the patent contained the following:
The metal organic framework substance material uses transition metal ions and a multi-dentate organic ligand 5,5′-(pyridine-2,5-diyl)-isophthalic acid to form three-dimensional network structure through coordination bonds or intermol. forces. Transition metal ions are preferably divalent copper, zinc, cobalt, nickel, cadmium ion. The metal organic framework substance material, has simple manufacture process, has high sp. surface area 2,000-2,200 m2/g and high pore volume 1.0-1.3 cm3/g. The method includes (1) dissolving di-Me 5-amino-m-phthalate in 15 weight% hydrobromic acid solution, stirring and cooling to 0-5°C, dripping 2.5mol/L sodium nitrite solution, diazotizing to obtain diazo salt solution; (2) dissolving cuprous bromide in 15 weight% hydrobromic acid solution, cooling to 0°C, dripping diazo salt solution under stirring, reacting at 0°C for 20-30 min, reacting at room temperature for ≥5 h, filtering to sep. organic layer, water washing, dissolving organic layer in dichloromethane, drying with anhydrous MgSO4, filtering, purifying by column chromatog. to obtain di-Me 5-bromo-m-phthalate; (3) dissolving di-Me 5-bromo-m-phthalate and bis(pinacolato)diboron in dried dioxane, adding potassium acetate and bis(triphenylphosphine) palladium dichloride, reacting at 65-70°C for 12 h, extracting with Et acetate, drying organic layer with anhydrous magnesium sulfate, removing organic solvent, purifying by column chromatog. to obtain di-Me pinacol 5-borate-1,3-phthalate. The method further includes (4) dissolving di-Me pinacol 5-borate-1,3-phthalate and 2,5-dibromopyridine in dioxane solution, adding potassium carbonate and catalyst bis(triphenylphosphine) palladium dichloride, reflux stirring under Ar protection at 70-90°C for 8-24 h, extracting with chloroform, collecting organic phase, evaporating solvent off, re-crystallizing with toluene to obtain product di-Me 5,5′-(pyridin-2,5-diyl)-m-phthalate; (5) dissolving in 3.0 mol/L NaOH solution, refluxing at 100°C for 12 h, cooling to room temperature, regulating pH to 1-2, ageing for 12 h, filtering, water washing, drying to obtain 5,5′-(pyridin-2,5-diyl)-m-phthalic acid; and (6) dissolving Cu, Zn, Cd, Co or Ni nitrate, acetate, chloride, carbonate, sulfate or perchlorate with 5,5′-(pyridin-2,5-diyl)-m-phthalic acid in water or/and organic solvent, reacting at 40-120°C to obtain title product. The material introduces pyridine-containing basic unit to multi-dentate organic ligand, and can effectively improve adsorption and storage amount of acetylene. The material is provided with relatively high acetylene adsorption amounts under 273 K and 298 K temperature condition, may be used at low pressure, and is expected to be used as a novel effective acetylene adsorbing and storing material. The experimental process involved the reaction of 5,5′-(Pyridine-2,5-diyl)diisophthalic acid(cas: 1431292-15-7).Safety of 5,5′-(Pyridine-2,5-diyl)diisophthalic acid
The Article related to metal pyridin diyl phthalic acid framework acetylene adsorption storage, Unit Operations and Processes: Separation Processes and other aspects.Safety of 5,5′-(Pyridine-2,5-diyl)diisophthalic acid