Potassium Chloride → Phosphorodifluoridic acid, potassium salt

HRID 571571

反応式

HRID 571571 の反応式
[P:1]([F:5])([F:4])(=[O:3])[OH:2].F[P-](F)(F)(F)(F)F.[Li+:13].[Cl-].[K+:15].C(=O)(OC)OC>>[P:1]([F:5])([F:4])([O-:3])=[O:2].[K+:15].[P:1]([F:5])([F:4])([O-:3])=[O:2].[Li+:13]

参加物

6

反応物 4

HCID 4873Potassium ChlorideHCID 12021Dimethyl CarbonateHCID 61681Difluorophosphoric acidHCID 23688915Lithium hexafluorophosphate

生成物 2

HCID 23694906Phosphorodifluoridic acid, potassium saltHCID 23697195Lithium phosphorodifluoridate

反応条件

温度
130 °C

実験手順

Difluorophosphoric acid (reagent, produced by Fluorochem Ltd.) (18.6 g) was weighed into a 250 ml-volume PFA vessel, and 4.1 g of lithium hexafluorophosphate (reagent, produced by Stella Chemifa Corporation) was added. Furthermore, 13.5 g of potassium chloride (reagent, produced by Wako Pure Chemical Industries, Ltd.) and 20.0 g of dimethyl carbonate were added, and the mixture was stirred for 1 hour under nitrogen flow and after heating at 130° C. for 17 hours, cooled to room temperature to obtain a mixed crystal of potassium difluorophosphate and lithium difluorophosphate. Anion analysis was performed in the same manner as in Example 2-6, as a result, the obtained difluorophosphate ion was 91% in terms of the relative area.

後処理

  1. additionwas added
  2. temperaturecooled to room temperature

出典と根拠

ORDレコード
ord-6d10dc91474a4f76a6d086d2e6d987c3
出典データセット
uspto-grants-2015_05
特許番号
US09028786B2

関連ノート

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