Method for preparing high purity phosphorus pentafluoride gas
A technology of phosphorus pentafluoride and phosphorus pentoxide, which is applied in the direction of phosphorus halide/oxyhalide, can solve the problems of high impurities in products, difficulties in separation and purification, and the introduction of many impurities, so as to facilitate the implementation of industrialization and process equipment Simplicity and the effect of increasing the reaction yield
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Embodiment 1
[0024] Put phosphorus pentoxide into a stainless steel reaction kettle lined with polytetrafluoroethylene and equipped with stirring equipment and a cooling jacket, and use high-purity argon to drive out the air in the kettle; % of anhydrous hydrogen fluoride, the reaction time is 3h; after the reaction is completed, continue to maintain the temperature in the kettle at -20°C, and intermittently add an excess of 35% of 60% fuming sulfuric acid to the kettle while stirring until the addition is complete; After pure argon drives away the air in the closed pressure heating furnace (phosphorus pentafluoride generation furnace), the reaction intermediate product is introduced into the furnace, the temperature is controlled at 120±5°C, the gas pressure is 1.0±0.1MPa, and the reaction time is 0.5h; the heating is complete Finally, the product is introduced into a condenser to cool and remove impurities to obtain high-purity phosphorus pentafluoride; the cooling medium is industrial li...
Embodiment 2
[0027] Put phosphorus pentoxide into a stainless steel reaction kettle lined with polytetrafluoroethylene and equipped with stirring equipment and a cooling jacket, and use high-purity argon to drive out the air in the kettle; maintain the temperature in the kettle at 0°C, and feed an excess of 60% anhydrous hydrogen fluoride, and the reaction time is 5 hours; after the reaction is completed, continue to maintain the temperature in the kettle at -10°C, and intermittently add an excess of 40% of 60% fuming sulfuric acid to the kettle while stirring until the addition is complete; use high-purity After the argon gas drives away the air in the closed pressure heating furnace (phosphorus pentafluoride generation furnace), the reaction intermediate product is introduced into the furnace, the temperature is controlled at 150±5°C, the gas pressure is 1.2±0.1MPa, and the reaction time is 1.0h; after heating is complete , the product is introduced into a condenser to cool and remove imp...
Embodiment 3
[0030] Conditions as described in Example 2, adding a secondary condensation process at the end of the reaction, industrial liquid nitrogen as the cooling medium, and other reaction conditions are the same.
[0031] The reaction yield is over 98%, and the obtained product phosphorus pentafluoride can reach: PF 5 The main content is greater than 99.99%, the water content is less than 5ppm, and the HF content is less than 40ppm.
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