IMPROVEMENT OF TECHNOLOGY FOR PREPARATION OF ALKALI METAL TRIS(PENTAFLUOROETHYL)TRIFLUOROPHOSPHATES
Journal: HERALD OF TECHNOLOGICAL UNIVERSITY
Rubrics: 2. CHEMICAL TECHNOLOGY
Authors:
1.
AO Rossiyskiy nauchnyy centr «Prikladnaya himiya»
2.
Perm State University
Type:
Article
Pages:
from 58
to 62
Status:
Language:
Russian
Keywords:
TRIS(PERFLUOROETHYL)TRIFLUOROPHOSPHATES, PHOSPHORANE, PHOSPHONATES, PHOSPHINATES, ELECTRICAL CONDUCTIVITY, BATTERIES, CONDUCTIVE SALTS, TECHNOLOGY
Funding:
Issledovanie osuschestvleno pri podderzhke Rossiyskogo nauchnogo fonda, grant № 24-23-00511, https://rscf.ru/project/24-23-00511/.
Abstract:
Alkali metal salts with the bulky tris(pentafluoroethyl)trifluorophosphate anion (FAP-3 anion, [(C2F5)3PF3]-) are promising as conductive salts in electrolytes and as modifying additives for the components of ion batteries, as well as sources of the most branched perfluoroethyl-substituted fluorophosphoric anion. This work discusses the fundamentals of the technology for producing perfluorinated alkali metal salts through the one-pot reaction of the carbonate or bicarbonate of a monovalent metal (Li, Na, K, Rb, Cs) with tris(pentafluoroethyl)trifluorophosphoric acid (HFAP-3, H+[PF3(C2F5)3]-), obtained by treating the starting tris(pentafluoroethyl)difluorophosphorane ((C2F5)3PF2) with hydrofluoric acid (HF). The main differences between the proposed technology and those described earlier are the absence of the need for a solvent and the single-reactor nature of the process, which simplifies and reduces the cost of production. The article discusses ways to optimize the process and presents the optimal temperature and time characteristics for maximum reaction yield. The spectral characteristics of the reaction products were studied using nuclear magnetic resonance (NMR). It was found that, in addition to the target products, the mixture contains by-products, the structures of which were determined using 19F and 31P NMR, and for bis(pentafluoroethyl)phosphinate and pentafluoroethylphosphonate lithium, also using X-ray structural analysis (XRD). Based on the conducted studies, an optimized laboratory technology for producing these salts is proposed, along with the principal and technological process schemes and a process flow diagram. Direct production costs (DPC) were calculated. It is shown that the production of perfluorinated salts using single-reactor technology with carbonates and bicarbonates is, on average, more economically feasible than the traditional method using alkali metal fluorides.
Alkali metal salts with the bulky tris(pentafluoroethyl)trifluorophosphate anion (FAP-3 anion, [(C2F5)3PF3]-) are promising as conductive salts in electrolytes and as modifying additives for the components of ion batteries, as well as sources of the most branched perfluoroethyl-substituted fluorophosphoric anion. This work discusses the fundamentals of the technology for producing perfluorinated alkali metal salts through the one-pot reaction of the carbonate or bicarbonate of a monovalent metal (Li, Na, K, Rb, Cs) with tris(pentafluoroethyl)trifluorophosphoric acid (HFAP-3, H+[PF3(C2F5)3]-), obtained by treating the starting tris(pentafluoroethyl)difluorophosphorane ((C2F5)3PF2) with hydrofluoric acid (HF). The main differences between the proposed technology and those described earlier are the absence of the need for a solvent and the single-reactor nature of the process, which simplifies and reduces the cost of production. The article discusses ways to optimize the process and presents the optimal temperature and time characteristics for maximum reaction yield. The spectral characteristics of the reaction products were studied using nuclear magnetic resonance (NMR). It was found that, in addition to the target products, the mixture contains by-products, the structures of which were determined using 19F and 31P NMR, and for bis(pentafluoroethyl)phosphinate and pentafluoroethylphosphonate lithium, also using X-ray structural analysis (XRD). Based on the conducted studies, an optimized laboratory technology for producing these salts is proposed, along with the principal and technological process schemes and a process flow diagram. Direct production costs (DPC) were calculated. It is shown that the production of perfluorinated salts using single-reactor technology with carbonates and bicarbonates is, on average, more economically feasible than the traditional method using alkali metal fluorides.
Keywords:
TRIS(PERFLUOROETHYL)TRIFLUOROPHOSPHATES, PHOSPHORANE, PHOSPHONATES, PHOSPHINATES, ELECTRICAL CONDUCTIVITY, BATTERIES, CONDUCTIVE SALTS, TECHNOLOGY
TRIS(PERFLUOROETHYL)TRIFLUOROPHOSPHATES, PHOSPHORANE, PHOSPHONATES, PHOSPHINATES, ELECTRICAL CONDUCTIVITY, BATTERIES, CONDUCTIVE SALTS, TECHNOLOGY
