Preparation methods and application examples of tetraethylcyanocopper hexafluorophosphate_Industrial additives

Background and overview^[1]

Tetraethylcyanocopper hexafluorophosphate is a reddish-brown crystalline powder and must be stored away from oxidants. Tetraethylcopper hexafluorophosphate can be obtained from the reaction of Cu₂O and hexafluorophosphoric acid.

Preparation^[1]

Place 8.1 g of solid Cu2O into a round-bottomed flask equipped with a stirring rod and a dropping funnel. Suspend the inorganic solid in 20 mL of acetonitrile CH3CN. Use an ice bath to cool the suspension. Fill the dropping funnel with 65% molar equivalents (relative to the amount of Cu(I) ions) of hexafluorophosphoric acid. The reaction mixture was added to the suspension. The reaction mixture rises after solid copper(I) oxide reacts with acid. The acetonitrile is evaporated to give the product tetraethylcyanocopper hexafluorophosphate. Store solids under inert conditions to prevent oxidation.

Apply^[2]

Tetraethylcyanocopper hexafluorophosphate can be useful to prepare a copper compound with photoluminescence properties. The method is as follows:

(1) Add 1-phenyl-2-(2-fluorophenyl)benzimidazole (0.01mol, 2.88g) to 25ml anhydrous tetrahydrofuran solution, then slowly add potassium diphenylphosphate (0.01 mol, 2.24g), refluxed at 60°C for 18 hours under argon protection. After the reaction was completed, the tetrahydrofuran in the system was recovered by rotary evaporation, and then the remaining solid was washed with 5 ml of water and 3 ml of methanol in sequence, and dried in vacuum to obtain ligand L ( Figure 4); wherein Figure 4 is the synthesis route diagram of ligand L.

(2) Combine the ligand L (0.01mol, 4.53g) prepared in step (1), triphenylphosphonium (0.02mol, 5.24g), 4-pyridinethiol (0.01mol, 1.11g) and Tetraethylcyanocopper hexafluorophosphate (0.01 mol, 3.73 g) was added to 50 ml of methylene chloride solution, and the silane reaction was stirred for 2 hours; after the reaction was completed, it was filtered, and the obtained filtrate was transferred to a reagent bottle and left to sit naturally for 72 hours to obtain product crystals. , filter and recover the dichloromethane-soluble phthalocyanine pigment liquid, wash the product with 5 ml of methanol, and dry it in vacuum to obtain a copper compound (C72H57N3P3SCu) with photoluminescence properties, with a yield of 78%;