METHOD OF OBTAINING WATER-FREE ACETYLACETONATES OF REFRACTORY METALS Russian patent published in 2008 - IPC C07C49/92 C07C45/77 C07F7/00 

FIELD: chemistry.

SUBSTANCE: method involves reaction of metal oxychloride with ammonium hydrocarbonate and acetylacetone in water with further cooling of reaction mix, precipitation separation, flushing, dehydratation and drying of obtained product. The process is performed by continuous or gradual feeding, along with continuous stirring, of water metal oxychloride solution to water ammonium hydrocarbonate with at feed rate under 2.5 ml of water metal oxychloride solution per minute per each 100 ml of water ammonium hydrocarbonate solution, followed by acetylacetone feeding at the mol ratio of metal oxychloride:ammonium hydrocarbonate:acetylacetone from 1.0:2.8:4.4 to 1.0:3.0:4.4, cooling of reaction mix at (-4) - (-6)°C for 7-9 hours, sequential precipitation flushing with water and acetone, dehydratation and drying of obtained product in air at 60-70°C for 4-6 hours. Water zirconium or hafnium oxychloride solution is used as water metal oxychloride solution.

EFFECT: simplified technology and higher environmental safety of the process.

2 ex