Method for producing lithium hexafluorophosphate
A technology of lithium hexafluorophosphate and lithium fluoride, which is applied in chemical instruments and methods, phosphorus compounds, lead-acid batteries, etc., can solve the problems of many production links of lithium hexafluorophosphate, the reaction yield does not exceed 65%, and the production cost remains high. Easy to popularize and apply, high product quality, good social value and economic value
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Embodiment 1
[0019] The method of the present invention comprises the steps of: adding 500 g of phosphorus pentachloride to a 5 L airtight reaction vessel with magnetic stirring, jacket insulation, and a cooler at the gas outlet, cooling to -40° C., and protecting the reaction vessel under nitrogen protection Slowly add 300g of anhydrous hydrogen fluoride with a water content of less than 10ppm after rectification and purification to make it react with phosphorus pentachloride to generate a mixed gas of phosphorus pentafluoride and hydrogen chloride, and the mixed gas passes through a cooler (-40°C) at the gas outlet ) to remove some impurities and residual acid after cooling. In the 1# reaction kettle with magnetic stirring and cooling jacket, dissolve 55g of high-purity lithium fluoride in 1000g of anhydrous hydrogen fluoride to form anhydrous hydrogen fluoride solution of lithium fluoride, and introduce cooled pentafluoride under stirring The mixed gas of phosphorus fluoride and hydroge...
Embodiment 2
[0023] Return 1250 g of mother liquor after crystallization and filtration in 1# and 2# reactors in Example 1 to 1# and 2# reactors respectively, and add 55 g of high-purity lithium fluoride and anhydrous hydrogen fluoride solution under stirring to form fluoride Anhydrous hydrogen fluoride solution of lithium, repeat the reaction process of embodiment 1, obtain 300g lithium hexafluorophosphate product. The test result product purity is greater than 99.9%, the product free acid (calculated by HF) 95ppm, moisture (Karl Fischer method) 5ppm, alkali metal ion content (calculated by K, Na) 4ppm, heavy metal ion content (calculated by Fe) 2ppm , Insoluble matter content 500ppm.
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