Lithium hexafluorophosphate synthesis

Yield:-

Reaction Conditions:

Stage #1: lithium oxalatewith hydrogen fluoride at 20;
Stage #2: with phosphorus pentachloride;hydrogen fluoride at 30; for 4 h;Cooling;Overall yield = 87.64 %; Overall yield = 194.52 g;

Steps:

3 Embodiment 3

Under the room temperature condition, with the jacket in the reaction container 1 by adding 101.9g lithium oxalate, 1300gHF, and stirred for a night, the lithium oxalate in HF completely soluble. In the reactor 2 is in advance in 200g water-free HF, then slowly adding phosphorus pentachloride 416.46g, into the low-temperature cooling medium in the jacket, in order to control the temperature, then the process is generated in the reaction vessel the highly purified phosphorus 1 in, a gas eduction rate control 2L/Min, the pay attention to the temperature change in the process, the temperature control 30 °C the following, after the gas, is continuously stirred for 4 hours. After filtration, the product obtained by evaporation crystallization mode 401.23g, through the rapid drying products after 368.85 g. Finally the obtained product by 700g ethanol, and the quality of the product is obtained after filtering 194.52g, wherein the theoretical yield 221.93g, the yield of products reaches 87.64%. The product purity of the obtained product to 99.93%, moisture content is 5.2 PPM, for including sour quantity 24 PPM.

References:

CN105218348,2016,A Location in patent:Paragraph 0021; 0022