CN112678780B - Preparation method of high-purity lithium sulfide - Google Patents
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Abstract
The invention relates to a preparation method of high-purity lithium sulfide, belonging to the technical field of preparation of lithium sulfide. The invention aims to provide a preparation method of high-purity lithium sulfide. The method mainly adopts a lithium sulfide precursor (one or more of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate) to react with a related reducing agent at a high temperature to prepare a substance containing lithium sulfide, then the lithium sulfide in the mixture is leached and purified, and finally a lithium sulfide product with the purity of more than 99.9 percent and controllable appearance is obtained by spray drying. The method is simple and easy to operate, does not need to adopt toxic organic solvents, is safe and environment-friendly, and the obtained lithium sulfide has high purity which can reach more than 99.9 percent, controllable appearance and high sphericity.
Description
Technical Field
The invention relates to a preparation method of high-purity lithium sulfide, belonging to the technical field of preparation of lithium sulfide.
Background
With the rapid development of new energy vehicles, the demand of new energy vehicles on power batteries mainly focuses on two aspects of long endurance and high safety. At present, the cell energy density of a liquid lithium ion battery product can reach 240-260 kw.h/kg and is already close to the limit of 300 kw.h/kg.
In recent years, many electric vehicles have been in fire accidents at home and abroad, the main reason is that the power battery is easy to generate potential safety hazards due to the fact that the liquid lithium ion battery adopts low-flash-point electrolyte and high-energy-density ternary cathode materials.
How to solve the contradiction between high energy density and high safety is urgent. Lithium sulfide (Li 2S) is used as a positive electrode material of the lithium-sulfur battery and has high theoretical specific capacity (1166 mA · h/g). Meanwhile, lithium sulfide can also be used as a basic material for synthesizing sulfide solid electrolyte in the solid battery, so that the ionic conductivity of the solid battery is improved, the overall performance of the solid battery is improved, the excellent electrochemical properties of the lithium sulfide determine that the lithium sulfide has a wide application prospect in the development of the lithium battery in the future, but the requirement on the purity of the lithium sulfide is higher and higher in the synthesis process of the solid electrolyte, and therefore the demand on high-purity lithium sulfide products is more and more urgent.
The earliest methods for producing lithium sulfide were directly prepared by combining the two elements, such as reacting lithium in liquid ammonia with elemental sulfur to obtain lithium sulfide material, but the reaction conditions were too severe and dangerous, and thus, the method is not suitable for large-scale production. In recent years, new methods for synthesizing lithium sulfide have been developed due to the development of technologies such as lithium-sulfur batteries. The existing lithium sulfide preparation and synthesis methods are mainly divided into two categories, namely a synthesis method and a pyrolysis method, wherein the synthesis method comprises the following steps: the metal lithium or the organic lithium reacts with the elemental sulfur in an organic solvent to prepare the lithium-containing material, such as patents CN108190845A, CN109019526A, etc., which have high requirements for process control. The metal lithium or organic lithium reacts with hydrogen sulfide in an organic solvent, such as patents CN103813980A, CN105016310A, CN108358175A, etc., these methods need to use highly toxic hydrogen sulfide gas, and have high requirements for the safety of the process. The high-temperature pyrolysis method comprises the following steps: the lithium sulfide precursor (one or more of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate) is reacted with relevant reducing agents at high temperature for preparation, such as patents CN106229487A, CN108400327A and the like, and the methods can prepare the substance containing the lithium sulfide, but no corresponding standard or requirement is provided for quality and index control of the prepared lithium sulfide product, so that the authenticity of some patents which claim that the product with the purity of 99.9 percent can be prepared by a simple method only and no lithium sulfide corresponds to the standard or requirement exists.
CN108400327A discloses a preparation method of lithium sulfide, which comprises the following steps: 1) Grinding and mixing anhydrous lithium sulfate, glucose and hard carbon, and then transferring the mixture into a quartz sintering tube of a vacuum tube furnace; 2) Preheating the quartz sintering tube, vacuumizing the vacuum tube furnace, and connecting a Kipp's generator at the interface of the quartz sintering tube; 3) Introducing hydrogen into the quartz sintering tube, heating the quartz sintering tube, and reacting to prepare the lithium sulfide, wherein the mass ratio of the anhydrous lithium sulfate to the hard carbon to the glucose is 1. The purity of the lithium sulfide prepared by the method is up to more than 99.9 percent, and the production cost is low. The method has serious authenticity problems, the lithium sulfide prepared by the method of the patent is not high-purity lithium sulfide but a mixture containing the lithium sulfide, because the calcined product has more or less excessive carbon after the method is calcined by a simple reduction reaction, and simultaneously, the problem of side reaction impurities such as lithium carbonate and the like possibly exists, so that more impurities exist, the corresponding index control (including index types and index contents) is not given in the embodiment, and meanwhile, a large number of experiments prove that the method and the steps of the patent cannot obtain 99.9 percent of lithium sulfide products.
Disclosure of Invention
Aiming at the defects, the technical problem to be solved by the invention is to provide a preparation method of high-purity lithium sulfide.
The preparation method of the high-purity lithium sulfide sequentially comprises the following steps:
a. mixing materials: lithium sulfide precursor and saccharide reducing agent according to Li 2 Mixing the O and the C in a molar ratio of 1.5-6 to obtain a uniform mixture; wherein the lithium sulfide precursor is at least one of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate;
b. heating for reaction: under the protection of vacuum or inert gas, the mixture is mixed and stirred for reaction for 2 to 6 hours at the temperature of between 200 and 300 ℃; then reacting for 2-6 h at 400-600 ℃; reacting at 675-775 ℃ for 2-6 h, and cooling to obtain a reacted material;
c. leaching, filtering and drying: and adding anhydrous alcohol into the reacted materials, filtering, and drying the filtrate to obtain the high-purity lithium sulfide.
Preferably, the sugar reducing agent is at least one of glucose, sucrose, fructose and maltose.
Preferably, in step a, the particle diameters of the lithium sulfide precursor and the reducing agent are both 200 to 400 mesh.
Preferably, in step b, the vacuum is at a pressure of less than 20Pa.
Preferably, in the step c, the mass ratio of the reacted materials to the anhydrous alcohol is 1.
More preferably, in step c, the anhydrous alcohol is at least one of ethanol, methanol and pentylalcohol.
Preferably, in step c, the drying is spray drying.
More preferably, in the step c, the drying is spray drying at a low temperature of 50 to 70 ℃.
Preferably, in the step c, the filter residue after filtration is washed with 5 to 10 weight percent of hydrogen peroxide.
Preferably, the purity of the high-purity lithium sulfide is more than or equal to 99.9%.
Compared with the prior art, the invention has the following beneficial effects:
the invention mainly adopts lithium sulfide precursors (one or more of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate) to react with related reducing agents at high temperature to prepare a substance containing lithium sulfide, then the lithium sulfide in the mixture is leached and purified, and finally the lithium sulfide product with purity of more than 99.9 percent and controllable appearance is obtained by spray drying. The method is simple and easy to operate, does not need to adopt toxic organic solvents, is safe and environment-friendly, and the obtained lithium sulfide has high purity which can reach more than 99.9 percent, controllable appearance and high sphericity.
Drawings
FIG. 1 is an XRD pattern of a lithium sulfide product prepared in example 1 of the present invention.
FIG. 2 is an SEM image (x 100) of a lithium sulfide product prepared in example 1 of the present invention.
FIG. 3 is an SEM image (magnification 500) of a lithium sulfide product prepared in example 1 of the present invention.
Detailed Description
The preparation method of the high-purity lithium sulfide sequentially comprises the following steps:
a. mixing materials: lithium sulfide precursor and saccharide reducing agent according to Li 2 Mixing the O and the C in a molar ratio of 1.5-6 to obtain a uniform mixture; wherein the lithium sulfide precursor is at least one of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate;
b. heating for reaction: under the protection of vacuum or inert gas, the mixture is evenly mixed and reacted for 2 to 6 hours at the temperature of between 200 and 300 ℃; then reacting for 2-6 h at 400-600 ℃; reacting at 675-775 ℃ for 2-6 h, and cooling to obtain a reacted material;
c. leaching, filtering and drying: and adding anhydrous alcohol into the reacted materials, filtering, and drying the filtrate to obtain the high-purity lithium sulfide.
By adopting the method, the high-purity lithium sulfide can be prepared, the purity of the lithium sulfide is more than or equal to 99.9 percent, and the method is simple.
The step a is a material mixing process, and a lithium sulfide precursor (one or more of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate) is mixed with a related reducing agent to provide a raw material basis for the subsequent reduction reaction.
The invention needs to use the reducing agent of saccharides instead of simple substance carbon, if the simple substance carbon is used for reaction, the reaction temperature is higher than that of the saccharides, side reaction is more easily generated to generate lithium oxide, the lithium oxide is easy to react with organic solvents such as alcohols and the like, and the subsequent purification is not favorable, therefore, the invention adopts the reducing agent of saccharides. More preferably, the sugar reducing agent is at least one of glucose, sucrose, fructose and maltose.
More preferably, in step a, the particle diameters of the lithium sulfide precursor and the reducing agent are both 200 to 400 mesh. Before mixing, the lithium sulfide precursor and the saccharide reducing agent can be respectively ground and then uniformly mixed, preferably, the lithium sulfide precursor and the saccharide reducing agent are mixed and then ground to 200-400 meshes, so that not only can the grinding time be saved, but also the lithium sulfide precursor and the saccharide reducing agent can be further uniformly mixed in the grinding process, and the efficiency is higher.
The raw material lithium sulfide precursor used in the step a of the invention is AR grade (analytically pure) or above. The reducing agent is also of AR grade or above.
The step b is a main preparation process, three stages of heating and heat preservation processes correspond to three different reaction stages respectively, firstly, the mixed material reacts at 200-300 ℃ for 4-6 h, the melting coating reaction occurs in the stage, the carbonization coating reaction occurs in the reaction at 400-600 ℃ for 2-6 h, and finally, the reduction calcination reaction occurs in the reaction at 675-775 ℃ for 2-6 h.
b is carried out under the condition of air isolation, preferably, inert gas is used as protective gas or the reaction container is vacuumized, and the pressure of the vacuum is preferably lower than 20Pa. The inert gas may be common argon or helium gas, etc.
The step c is a leaching, filtering and drying process. Since lithium sulfide is soluble in alcohols, anhydrous alcohols are used to leach the lithium sulfide.
Preferably, in the step c, the mass ratio of the reacted materials to the anhydrous alcohol is 1.
The common alcohols can dissolve the lithium sulfide, and preferably, the anhydrous alcohol is at least one of ethanol, methanol and amyl alcohol.
And dissolving lithium sulfide, and filtering to obtain a filtrate, namely a lithium sulfide solution. And drying the lithium sulfide solution to obtain the high-purity lithium sulfide. The usual drying methods are suitable for the present invention, preferably the drying is spray drying.
More preferably, the drying is spray drying at a low temperature of 50 to 70 ℃.
Preferably, in the step c, the filtered filter residue is washed by 5-10 wt% of hydrogen peroxide. The filter residue is washed by hydrogen peroxide, so that the EHS accident caused by hydrogen sulfide generated by lithium sulfide hydrolysis is mainly prevented, and the lithium sulfide is converted into lithium sulfate after the hydrogen peroxide is used for oxidation, so that no hydrogen sulfide is generated.
By the method, the lithium sulfide with the purity of more than or equal to 99.9 percent can be prepared.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
1) 60g of AR-grade anhydrous lithium sulfate and 49.1g of AR-grade sucrose are mixed and ground to 200-300 meshes;
2) Melting and coating the uniformly ground material obtained in the previous step for 4 hours at 200 ℃ under the protection of inert gas or in a vacuum environment;
3) Continuously carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 6 hours at 400 ℃ under the protection of inert gas or in a vacuum environment;
4) Continuously reducing and calcining the carbonized and coated material obtained in the previous step for 2 hours at the temperature of 775 ℃ in an inert gas protection or vacuum environment;
5) After the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:200, dissolving in absolute ethyl alcohol, then filtering, reserving filtrate, and washing filter residues with 5% mass fraction hydrogen peroxide.
6) And (3) performing spray drying granulation on the filtrate obtained in the previous step at a low temperature of 50 ℃ by using an organic solvent spray dryer to obtain a material, namely a spherical lithium sulfide product with the purity of 99.9%, wherein an XRD (X-ray diffraction) diagram is shown in figure 1, the upper part in figure 1 is a sample map, and the lower part is a standard card. The SEM images are shown in fig. 2 and 3, where the magnification of fig. 2 is 100 times (× 100) and the method magnification of fig. 3 is 500 times (× 500).
Example 2
1) Mixing and grinding 300g of AR-level lithium sulfite and 320g of AR-level glucose to 300-400 meshes;
2) Melting and coating the uniformly ground material obtained in the previous step for 3 hours at 250 ℃ under the protection of inert gas or in a vacuum environment;
3) Continuously carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 3 hours at 500 ℃ under the protection of inert gas or in a vacuum environment;
4) Continuously reducing and calcining the carbonized and coated material obtained in the previous step for 3 hours at the temperature of 750 ℃ under the protection of inert gas or in a vacuum environment;
5) After the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:250, dissolving in anhydrous methanol, filtering, reserving filtrate, and washing filter residue with 10 mass percent hydrogen peroxide.
6) And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 60 ℃ by using an organic solvent spray dryer, wherein the obtained material is a spherical lithium sulfide product with the purity of 99.9%, the XRD diagram is similar to that of figure 1, and the SEM diagram is similar to that of figures 2 and 3.
Example 3
1) Taking 666g of AR-level lithium dithionate and 700g of AR-level fructose, mixing and grinding the materials to 200-400 meshes;
2) Melting and coating the uniformly ground material obtained in the previous step for 2.5 hours at 300 ℃ under the protection of inert gas or in a vacuum environment;
3) Continuously carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 2 hours at the temperature of 600 ℃ under the protection of inert gas or in a vacuum environment;
4) The carbonized and coated materials obtained in the previous step are continuously reduced and calcined for 4 hours at 725 ℃ under the protection of inert gas or in a vacuum environment;
5) After the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:300, dissolving anhydrous amyl alcohol, then filtering, reserving filtrate, and washing filter residues with 8% of hydrogen peroxide by mass fraction.
6) And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 54 ℃ by using an organic solvent spray dryer, wherein the obtained material is a spherical lithium sulfide product with the purity of 99.9%, the XRD diagram is similar to that of figure 1, and the SEM diagram is similar to that of figures 2 and 3.
Example 4
1) Mixing and grinding 690g of AR-grade lithium sulfate monohydrate and 600g of AR-grade glucose to 200-250 meshes;
2) Melting and coating the uniformly ground material obtained in the previous step for 6 hours at 220 ℃ under the protection of inert gas or in a vacuum environment;
3) Carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 6 hours at 450 ℃ under the protection of inert gas or in a vacuum environment;
4) The carbonized coating material obtained in the previous step is continuously reduced and calcined for 6 hours at 675 ℃ under the protection of inert gas or vacuum environment;
5) After the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:275, then filtering, reserving the filtrate, and washing the filter residue with 7% hydrogen peroxide by mass fraction.
6) And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 70 ℃ by using an organic solvent spray dryer, wherein the obtained material is a spherical lithium sulfide product with the purity of 99.9%, the XRD diagram is similar to that of figure 1, and the SEM diagram is similar to that of figures 2 and 3.
Example 5
1) 900g of AR-grade lithium sulfite and 740g of AR-grade fructose are mixed and ground to 350-400 meshes;
2) Melting and coating the uniformly ground material obtained in the previous step for 3.5 hours at 280 ℃ in an inert gas protection or vacuum environment;
3) Continuously carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 4 hours at 480 ℃ under the protection of inert gas or in a vacuum environment;
4) The carbonized and coated material obtained in the previous step is continuously reduced and calcined for 5 hours at 700 ℃ under the protection of inert gas or vacuum environment;
5) After the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:280 is dissolved in anhydrous methanol, then filtration is carried out, the filtrate is reserved, and the filter residue is washed by hydrogen peroxide with the mass fraction of 9%.
6) And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 65 ℃ by using an organic solvent spray dryer, wherein the obtained material is a spherical lithium sulfide product with the purity of 99.9%, the XRD diagram is similar to that of figure 1, and the SEM diagram is similar to that of figures 2 and 3.
Example 6
360g of AR-grade lithium dithionate and 350g of AR-grade glucose are mixed and ground to 250-300 meshes;
melting and coating the uniformly ground material obtained in the previous step at 250 ℃ for 3.8h under the protection of inert gas or in a vacuum environment;
carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 3 hours at 550 ℃ under the protection of inert gas or in a vacuum environment;
continuously reducing and calcining the carbonized coating material obtained in the previous step for 2 hours at the temperature of 775 ℃ under the protection of inert gas or in a vacuum environment;
after the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:300, dissolving anhydrous amyl alcohol, then filtering, reserving filtrate, and washing filter residues by 6 mass percent hydrogen peroxide.
And (3) performing spray drying granulation on the filtrate obtained in the previous step at a low temperature of 55 ℃ by using an organic solvent spray dryer to obtain the material, namely the spherical lithium sulfide product with the purity of 99.9%, wherein the XRD pattern is similar to that of figure 1, and the SEM pattern is similar to that of figures 2 and 3.
Comparative example 1
Taking 60g of AR-grade anhydrous lithium sulfate and 20.7g of simple substance carbon, mixing and grinding the materials to 200-300 meshes;
reacting the uniformly ground material obtained in the previous step for 4 hours at 200 ℃ under the protection of inert gas or in a vacuum environment;
continuously reacting the materials obtained in the previous step for 6 hours at 400 ℃ under the protection of inert gas or in a vacuum environment;
continuously reducing and calcining the material obtained in the previous step for 2 hours at 775 ℃ under the protection of inert gas or in a vacuum environment;
after the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:200, dissolving in absolute ethyl alcohol, then filtering, reserving filtrate, and washing filter residues with 6% mass fraction hydrogen peroxide.
And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 50 ℃ by using an organic solvent spray dryer, thus obtaining the material, namely the spherical lithium sulfide product with the purity of 96%.
Comparative example 2
60g of AR anhydrous lithium sulfate and 49.1g of AR-grade sucrose are mixed and ground to 200-300 meshes;
melting and coating the uniformly ground material obtained in the previous step for 4 hours at 200 ℃ under the protection of inert gas or in a vacuum environment;
carrying out carbonization coating reaction on the molten coating material obtained in the previous step for 6 hours at 400 ℃ under the protection of inert gas or in a vacuum environment;
continuously reducing and calcining the carbonized coating material obtained in the previous step for 2 hours at the temperature of 775 ℃ under the protection of inert gas or in a vacuum environment;
and cooling the material obtained in the previous step to normal temperature to obtain a lithium sulfide product with the purity of 91.99%.
Comparative example 3
60g of AR anhydrous lithium sulfate and 49.1g of AR-grade sucrose are mixed and ground to 200-300 meshes;
reducing and calcining the uniformly ground material obtained in the previous step for 12 hours at the temperature of 775 ℃ under the protection of inert gas or in a vacuum environment;
after the materials obtained in the previous step are cooled to normal temperature, the materials are mixed according to the mass solid-liquid ratio of 1:200, dissolving absolute ethyl alcohol, then filtering, reserving filtrate, and washing filter residue by 6 mass percent hydrogen peroxide.
And (3) carrying out spray drying granulation on the filtrate obtained in the previous step at a low temperature of 50 ℃ by using an organic solvent spray dryer, thus obtaining the material, namely the lithium sulfide product with the purity of 95.18%.
The detection method and indexes of the related embodiment are as follows:
the samples of examples 1 to 6 and comparative examples 1 to 3 were tested:
sample pretreatment: taking 1g of the final lithium sulfide product, dissolving the lithium sulfide product with deionized water, and then fixing the volume to 100ml to obtain a solution A; taking 50ml of the solution A by using a pipette, adding 15ml of 30% hydrogen peroxide, removing excessive hydrogen peroxide by ultrasonic oscillation for one hour to obtain a solution B, and fixing the volume of the solution B to 100ml to obtain a solution C;
S 2- content titration detection: taking 20ml of 0.1mol/L iodine water, adding 10ml of 0.05mol/L glacial acetic acid, shaking up, adding 1ml of solution A, dripping 0.05mol/L sodium thiosulfate solution to form light yellow, adding 5ml of 1g/L starch solution, continuously dripping 0.05mol/L sodium thiosulfate solution until blue disappears, and calculating to obtain S 2- The content;
Li 2 and (3) detecting the content of O and related impurities: the content of carbonate and hydroxyl in the solution C is detected by conventional acid-base titration, the content of lithium ions and other metal cations in the solution C is detected by conventional ICP (inductively coupled plasma), and the detected content is detectedThe results are converted by calculation into the corresponding impurity content in the lithium sulfide.
The results are shown in Table 1.
TABLE 1
| Detecting item categories | CO 3 2- ％ | OH - ％ | Li 2 O％ | S 2- ％ | Na+K+Ca+Mg+Pb+Cu+Zn+Al+Fe+Sn％ |
| Example 1 | --- | --- | 65.20 | 69.55 | <0.01 |
| Example 2 | --- | --- | 65.19 | 69.56 | <0.01 |
| Example 3 | --- | --- | 65.21 | 69.54 | <0.01 |
| Example 4 | --- | --- | 65.17 | 69.55 | <0.01 |
| Example 5 | --- | --- | 65.20 | 69.56 | <0.01 |
| Example 6 | --- | --- | 65.20 | 69.55 | <0.01 |
| Comparative example 1 | --- | 3.2 | 63.54 | 66.78 | <0.01 |
| Comparative example 2 | 3.5 | -- | 61.41 | 63.99 | <0.01 |
| Comparative example 3 | --- | 1.8 | 64.56 | 66.21 | <0.01 |
In Table 1, "%" indicates weight percent, and "- - -" indicates no detection.
Claims (9)
1. The preparation method of the high-purity lithium sulfide is characterized by comprising the following steps in sequence:
a. mixing materials: lithium sulfide precursor and saccharide reducing agent according to Li 2 Mixing the O and the C in a molar ratio of 1.5-6 to obtain a mixed material; wherein the lithium sulfide precursor is at least one of lithium sulfate, lithium sulfite, lithium bisulfate and lithium dithionate;
b. heating for reaction: under the protection of vacuum or inert gas, the mixture is mixed and stirred for reaction for 2 to 6 hours at the temperature of between 200 and 300 ℃; then reacting for 2-6 h at 400-600 ℃; reacting at 675-775 ℃ for 2-6 h, and cooling to obtain a reacted material;
c. leaching, filtering and drying: adding anhydrous alcohol into the reacted materials, then filtering, and drying the filtrate to obtain high-purity lithium sulfide;
the purity of the high-purity lithium sulfide is more than or equal to 99.9 percent.
2. The method for preparing high-purity lithium sulfide according to claim 1, wherein: the sugar reducing agent is at least one of glucose, sucrose, fructose and maltose.
3. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in the step a, the particle diameters of the lithium sulfide precursor and the saccharide reducing agent are both 200-400 meshes.
4. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in the step b, the vacuum pressure is lower than 20Pa.
5. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in the step c, the mass ratio of the reacted materials to the anhydrous alcohol is 1.
6. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in the step c, the absolute alcohol is at least one of ethanol, methanol and amyl alcohol.
7. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in step c, the drying is spray drying.
8. The method for preparing high-purity lithium sulfide according to claim 1, wherein: in the step c, the drying is spray drying at a low temperature of between 50 and 70 ℃.
9. The method for preparing high-purity lithium sulfide according to claim 1, wherein: and c, washing the filtered filter residue with 5-10 wt% of hydrogen peroxide.
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| CN113793933B (en) * | 2021-09-10 | 2023-05-30 | 深圳市研一新材料有限责任公司 | Lithium sulfide for solid electrolyte and preparation method and application thereof |
| CN114275742B (en) * | 2021-12-24 | 2022-12-23 | 湖南恩捷前沿新材料科技有限公司 | Preparation method of lithium sulfide capable of realizing continuous production |
| CN114477099A (en) * | 2022-02-08 | 2022-05-13 | 天津大学 | Preparation method of battery-grade lithium sulfide |
| CN115231527B (en) * | 2022-07-29 | 2024-02-27 | 深圳博粤新材料科技有限公司 | Method for preparing lithium sulfide by reducing lithium sulfate through organic gas pyrolysis |
| WO2024128792A1 (en) * | 2022-12-16 | 2024-06-20 | 포스코홀딩스 주식회사 | Method for preparing lithium sulfide |
| WO2024128671A1 (en) * | 2022-12-16 | 2024-06-20 | 포스코홀딩스 주식회사 | Precursor for producing lithium sulfide and lithium sulfide powder |
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| CN110112390A (en) * | 2019-05-10 | 2019-08-09 | 浙江大学 | The preparation method and applications of easily-activated high carrying capacity lithium sulfide carbon composite |
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| JP2013227180A (en) * | 2012-04-26 | 2013-11-07 | Furukawa Co Ltd | Method for producing lithium sulfide |
| JP2015074567A (en) * | 2013-10-07 | 2015-04-20 | 古河機械金属株式会社 | Method for producing lithium sulfide |
| CN110112390A (en) * | 2019-05-10 | 2019-08-09 | 浙江大学 | The preparation method and applications of easily-activated high carrying capacity lithium sulfide carbon composite |
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