Provided are methods of making a MOF UiO-66 comprising reacting zirconium oxychloride with terephthalic acid or derivative thereof and acetic acid in a solvent to provide a reaction solution; diluting the reaction solution with water, heating the diluted reaction solution and reducing the reaction temperature of the reaction mixture to provide the MOF UiO-66 having a micropore volume greater than or equal to 0.45 cc/g and a crystal size of between about 20 nm and about 1000 nm. Also provided are methods of making a MOF UiO-66 where a zirconium hydroxide acetate and zirconium hydroxide are reacted with a carboxylic acid or derivative thereof and acetic acid in a solvent to produce the metal-organic framework MOF UiO-66 having a micropore volume at least 0.35 cc/gram.