A kind of synthetic method of phosphorus pentasulfide powder
A technology of phosphorus pentasulfide and a synthesis method, which is applied to phosphorus compounds of phosphorus sulfur/selenium/tellurium, etc., can solve the problems of complex preparation process, low product quality and high energy consumption, and achieves the effects of being environmentally friendly and easy to implement in industrialization.
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Embodiment 1
[0024] Under nitrogen protection, lithium sulfide and phosphorus pentachloride were evenly mixed at a molar ratio of 5:2, transferred to a reactor and sealed. Heat to 140°C at a heating rate of 2°C / min, and keep the temperature for 5h. After the reaction was completed, the temperature was lowered to room temperature, and the solid product in the reactor was added to toluene for solid-liquid separation. The separated solution was distilled at 150°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid into acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder. figure 1 The X-ray diffraction pattern of its product can only characterize the X-ray spectrum of lithium chloride. According to the law of conservation of materials, there must be phosphorus pentasulfide in the product.
Embodiment 2
[0026] Under the protection of argon, lithium sulfide and phosphorus pentachloride were uniformly mixed at a molar ratio of 5:3, transferred to the reactor and sealed. Heat to 300°C at a heating rate of 20°C / min, and hold for 1h. After the reaction was completed, the temperature was lowered to room temperature, and the solid product in the reactor was added to toluene for solid-liquid separation. The separated solution was distilled at 110°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid into acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder.
Embodiment 3
[0028] Under the protection of nitrogen and argon, lithium sulfide and phosphorus pentachloride were uniformly mixed at a molar ratio of 5:4, transferred to a reactor and sealed. Heat to 100°C at a heating rate of 0.5°C / min, and hold for 100h. After the reaction was completed, the temperature was lowered to room temperature, and the solid product in the reactor was added to toluene for solid-liquid separation. The separated solution was distilled at 120°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid into acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder.
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