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A lithium sulfide and lithium iodide technology, applied in the directions of alkali metal sulfide/polysulfide, lithium storage battery, electrochemical generator, etc., can solve the problems of low solvent selectivity, harsh preparation conditions, complex synthesis process, etc. Simple and easy process steps and mild reaction conditions
Inactive Publication Date: 2020-08-11
TIANMU LAKE INST OF ADVANCED ENERGY STORAGE TECH CO LTD +2
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Problems solved by technology
The above-mentioned synthesis process uses toxic hydrogen sulfide as a raw material, which has high requirements for equipment and process control, which is not conducive to the safety of the preparation process
(2) Using elemental sulfur as the sulfur source: the patent with the notification number CN106784754B dissolves sublimated sulfur powder in anhydrous toluene and reacts with tetrahydrofuran solution mixed with carbon nanotubes and lithium triethylborohydride to prepare carbon nanotubes-lithium sulfide Composite material powder, but the cost of the raw material lithium triethyl borohydride used is relatively high
(3) Using carbon disulfide as a source of sulfur: the patent with the notification number CN103764566B utilizes elemental lithium and elemental sulfur and / or is selected from CS 2 , COS, SO 2 , SO sulfur-containing compounds are in a liquid state and react in an aliphatic or cycloaliphatic hydrocarbon solvent to prepare carbon-coated lithium sulfide. The solvent used in this synthesis method must be in a liquid state at the reaction temperature and the reaction temperature is between 80 ° C and 200 ° C. Therefore The selectivity of the solvent is small
The patent application with publication number CN108358175A dissolves lithium sulfide, sulfur-rich compounds (one or more of sulfur and sulfur-rich compounds), metal lithium and aromatic compounds in ether organic solvents, and reacts to obtain lithium sulfide, but the The synthesis process needs to first react lithium sulfide with sulfur-rich compounds and dissolve them in ether organic solvents to obtain unsaturated Li2S x Solution (1
The patent application whose publication number is CN109019526A utilizes an organic solvent method to prepare lithium sulfide, dissolves metallic lithium and sulfur in organic solvents respectively, and finally mixes and reacts at low temperature to obtain lithium sulfide, but the solvent selection of this synthesis method is limited (ethylenediamine and At least one of propylenediamine), and it is required to react in a jacketed reactor and pass cooling water into the jacket, and the preparation conditions are relatively harsh
Method used
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Embodiment 1
[0031] Step 1: Weigh 30.842 g of biphenyl and dissolve it in a corresponding volume of anhydrous ethylene glycol dimethyl ether solvent at a concentration of 1 mol / L. After the biphenyl is completely dissolved, add 1.3882 g of lithium metal with a length of 1 cm and a width of 1 mm Silk, let it stand until it is completely dissolved;
[0032]Step 2: Weigh 3.206 g of elemental sulfur into the above lithiated solution, and stir at room temperature for 6 h;
[0033] Step 3: Take out the product, separate the precipitate and supernatant with a centrifuge, the speed is 8000 r / min, and the centrifugation time is 20min, and the supernatant is recovered for reuse; the precipitate is centrifuged with anhydrous ethylene glycol xylene solvent Wash 3 times at 6000r / min, centrifuge for 10 min; dry in a vacuum oven at 100 °C for 16 h, and heat-treat at 200 °C for 8 h under the protection of argon to remove residual solvent to obtain lithium sulfide material. figure 1 is the XRD pattern of ...
Embodiment 2
[0035] Step 1: Weigh 25.636 g of naphthalene and dissolve it in a corresponding volume of anhydrous tetrahydrofuran solvent at a concentration of 0.1 mol / L. After the biphenyl is completely dissolved, add 1.3882 g of lithium metal with a length of 2 mm, a width of 2 mm, and a thickness of 0.5 mm. Let it stand until it dissolves completely;
[0036] Step 2: Weigh 3.206 g of elemental sulfur into the above lithiated solution, and stir at room temperature for 4 h;
[0037] Step 3: Take out the product, separate the precipitate and supernatant with a centrifuge at a speed of 8000 r / min, and centrifuge for 20 minutes, recover the supernatant for reuse, and wash the precipitate with anhydrous tetrahydrofuran solvent for 3 times, The rotational speed was 6000 r / min, and the centrifugation time was 10 min; the samples were dried on a heating platform at 60 °C for 24 h under the protection of argon, and then heat-treated in a vacuum oven at 180 °C for 12 h to remove residual solvents t...
Embodiment 3
[0039] Step 1: Weigh 26.7692 g of lithium iodide and dissolve it in a corresponding volume of ultra-dry acetonitrile solvent at a concentration of 10 mol / L;
[0040] Step 2: Weigh 3.206 g of elemental sulfur into the above lithiated solution, and stir at room temperature for 8 h;
[0041] Step 3: Take out the product, separate the precipitate and supernatant with a centrifuge at a speed of 8000 r / min, and the centrifugation time is 20 min. The precipitate is centrifuged and washed 3 times with an ultra-dry acetonitrile solvent at a speed of 6000 r / min, and the centrifugation time is 10 min; followed by drying in a vacuum oven at 140 °C for 12 h, and heat treatment at 320 °C under argon protection for 6 h to remove residual solvents to obtain lithium sulfide materials.
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Abstract
The invention mainly relates to the field of lithium battery materials, and provides a method for synthesizing lithium sulfide by taking a lithiation solution and elemental sulfur as raw materials through direct reaction, which comprises the following steps: preparing the lithiation solution, an organic ether solution containing a metal lithium-aromatic compound, a lithium iodide solution and an n-butyl lithium solution; adding elemental sulfur into the lithiation solution for mixing; and sequentially carrying out a room-temperature reaction, separation and precipitation, drying and heat treatment on the mixed solution to obtain the lithium sulfide. The synthesis method of lithium sulfide has the advantages of cheap and easily available raw materials, simple process, no harmful gas generation, and mild and controllable synthesis process.
Description
technical field [0001] The invention belongs to the field of lithium battery materials, and in particular relates to a method for synthesizing lithium sulfide. Background technique [0002] Solid-state electrolytes are generally divided into three categories: polymers, oxides, and sulfides. Solid-state batteries using polymer electrolytes are close to existing lithium-ion batteries in terms of manufacturing process, but the conductivity of polymer electrolytes at room temperature is low. Oxide electrolytes have good thermal, chemical, and electrochemical stability, but their room temperature ionic conductivity is limited to 10 −3 –10 −4 S / cm and leads to poor interfacial contact with electrode materials due to its high rigidity. Sulfide electrolytes have high lithium-ion conductivity and good interfacial contact due to relatively "soft" mechanical properties, so they are currently the most research-worthy electrolyte systems. Lithium sulfide is an indispensable raw mater...
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