Preparation method of lithium sulfide
A technology of lithium sulfide and lithium element, applied in chemical instruments and methods, inorganic chemistry, lithium compounds, etc., can solve the problems of high production cost of lithium sulfide, harsh process requirements, long preparation process time, etc., and achieves low production cost and process. The effect of simple requirements and short preparation process
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[0028] The embodiment of the present invention provides a kind of preparation method of lithium sulfide, comprises the following steps:
[0029] S1. Dissolving the simple substance of lithium in the cyclic ether containing benzene series to obtain solution A; wherein, the mass ratio of the simple substance of lithium to the benzene series is 1: (1-10), when the simple substance of lithium and the benzene series When the mass ratio of lithium is in the range of 1: (1-10), the lithium element can completely react with the benzene series. The mass ratio of the lithium element to the benzene series can be, for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1: 9 or 1:10.
[0030] Specifically, the lithium element is selected from at least one of lithium strips, lithium sheets, lithium butyl, and lithium powder; the benzene series is selected from at least one of naphthalene, tetralin, and biphenyl; the ring The ether is at least one selected from tetrahydrofuran and dioxolane. ...
Embodiment 1
[0043] Carry out the following process steps in an anhydrous and oxygen-free argon glove box:
[0044] S1. Dissolve 0.6 g of butyl lithium in 10 mL of tetrahydrofuran solution with a concentration of 0.2 g / mL of naphthalene, stir until the butyl lithium is completely dissolved, and the solution turns dark green to black, and solution A is obtained.
[0045] S2. Dissolve 1.39g of sulfur powder in 8mL of carbon disulfide, stir until completely dissolved, and obtain solution B.
[0046] S3. In the condition of a cold water bath at 5°C, under the condition of stirring, add the solution A to the solution B, and the solution B does not boil; after the addition is completed, continue to stir for 60 minutes to obtain a suspension .
[0047] S4. The suspension is subjected to solid-liquid separation by centrifugation, and the solid phase is collected and washed twice with a tetrahydrofuran solution, and then dried to obtain a solid-phase lithium sulfide powder.
[0048] as the picture ...
Embodiment 2
[0052] Carry out the following process steps in an anhydrous and oxygen-free argon glove box:
[0053] S1. Dissolve 1.0 g of lithium powder in 10 mL of dioxolane solution with a biphenyl solubility of 0.6 g / mL, stir until the lithium butyl is completely dissolved, and the solution turns dark green to black, and solution A is obtained.
[0054] S2. Dissolve 1.39g of sulfur powder in 8mL of dimethyl sulfoxide, stir until completely dissolved, and obtain solution B.
[0055] S3. In the condition of a cold water bath at 10°C, under the condition of stirring, add the solution A to the solution B, and the solution B does not boil; after the dropwise addition, continue to stir for 60 minutes to obtain a suspension .
[0056] S4. The suspension is subjected to solid-liquid separation by centrifugation, and the solid phase is collected and washed twice with a dioxolane solution, and then dried to obtain a solid-phase lithium sulfide powder.
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