CN108400327A - A kind of preparation method of lithium sulfide - Google Patents
A kind of preparation method of lithium sulfide Download PDFInfo
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- CN108400327A CN108400327A CN201810026837.1A CN201810026837A CN108400327A CN 108400327 A CN108400327 A CN 108400327A CN 201810026837 A CN201810026837 A CN 201810026837A CN 108400327 A CN108400327 A CN 108400327A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation methods of lithium sulfide, include the following steps：1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and kipp gas generator is connected in quartzy sintered pipes interface；3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide, and the mass ratio of the anhydrous slufuric acid lithium, hard charcoal and glucose is 1:2:5~10:1:5.The purity of lithium sulfide prepared by lithium sulfide preparation method using the present invention is up to 99.9% or more and low production cost, preparation method and process are simple, short preparation period, Preparation equipment is simple and easily operated, and safe preparation process is high, the raw material nonhazardous used, convenient for large-scale industrial production, after the glucose charing, it is tightly combined with lithium sulfate, the transformation efficiency of the lithium sulfide can be improved.
Description
Technical field
The invention belongs to technical field of chemistry, and in particular to a kind of preparation method of lithium sulfide.
Background technology
In recent years in portable data assistance, portable electronic device, domestic small electric power storing device, motor
The need for the lithium secondary battery of high performance that automatic two-wheeled cycle, electric vehicle, hybrid-electric car etc. as power source use
It asks and is continuously increased.The lithium sulfide of high-purity is common electrolyte in lithium ion battery, and lithium-sulfur cell compares energy due to it
Height, battery material is cheap, it is environmental-friendly the features such as next-generation lithium battery one of research hotspot.But lithium sulfide to water and its
It is sensitive so that production preserves, and preparation process is all subject to many limitations, and the price for eventually leading to lithium sulfide is extremely expensive, this is greatly
The development for constraining charcoal/lithium sulfide type lithium-sulfur cell.In addition, traditional lithium sulfur battery anode material is answered afterwards by first synthesizing
Prepared by the mode of conjunction, i.e. Carbon Materials first have to prepare Carbon Materials, then pass through again as elemental sulfur or the carrier of lithium sulfide
Various approach load to elemental sulfur or lithium sulfide in Carbon Materials carrier.This preparation is mutual in time with compound two processes
It is unsatisfactory that the synthetic method of separation determines that elemental sulfur or this kind of active material of lithium sulfide disperse in the composite, this can shadow
The utilization rate for ringing active material declines so as to cause battery performance.Therefore, a kind of side for preparing lithium sulfide of cheap and simple is found
Method, on the one hand improves the preparation process complexity that charcoal/lithium sulfide composite material faces, on the other hand expensive present situation avoids
The drawbacks of traditional preparation methods, improves dispersibility of the active material in lithium-sulphur cell positive electrode, is still a prodigious challenge.Most
Early lithium sulfide production method is the direct simple substance chemical combination using the two to prepare, such as anti-with the liquid ammonia solution and elemental sulfur of lithium
It answers, obtains lithium sulfide, then work out other preparation processes again, such as：Lithium is reacted with hydrogen sulfide in tetrahydrofuran, ethyoxyl lithium
The ethanol adducts of sulphur lithium hydride are decomposed, lithium carbonate is reacted with hydrogen sulfide.But the preparation side of these existing high-purity lithium sulfides
Method, reaction temperature is high, the period is long, the organic solvent that uses is there are inflammable and explosive, has the shortcomings that irritation and toxicity.
Application publication number is that the Chinese invention patent application of CN105016310A discloses a kind of preparation of high-purity lithium sulfide
Lithium hydroxide and N-Methyl pyrrolidone are mixed, mixed solution are obtained, by the mixed solution in indifferent gas by method and apparatus
It is heated to 130-140 DEG C under body protection, and is passed through hydrogen sulfide gas into the mixed solution, reacts 2~4 hours, obtains sulphur
The sulphur lithium hydride is sloughed hydrogen sulfide by lithium hydride slurries, obtains lithium sulfide slurries, removal wherein impurity and extra stink damp
Body, the dry lithium sulfide slurries obtain the lithium sulfide.This method is used to prepare the lithium sulfide of high-purity, has reaction temperature
Advantage low, using multiple solvent stability height, nonhazardous etc., but the preparation method program is more, preparation process is complicated.
Invention content
The present invention provides a kind of preparation method of lithium sulfide in view of the drawbacks of the prior art.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of lithium sulfide, includes the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Further, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 1:2:5~10:1:5 mixing, are expert at
It mills under room temperature 6~9 hours in planetary ball mill, ball milling speed is 200~600 revs/min.
Further, the anhydrous slufuric acid lithium, glucose and hard charcoal are 5~20 microns in later granularity of milling.
Further, the preheating temperature of the quartzy sintered pipes is 230 DEG C~290 DEG C.
Further, the flow that the hydrogen is passed through quartzy sintered pipes is 0.2~1.0L/h.
Further, the heating temperature of the quartzy sintered pipes is between 400-900 DEG C.
Further, anhydrous slufuric acid lithium, glucose and the hard charcoal mixture of the quartzy sintered pipes be passed through hydrogen with
2~6h is reacted afterwards.
Further, the anhydrous slufuric acid lithium and glucose need the heat drying in vacuum drying chamber in advance.
Further, the drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 100-120 DEG C and 70-100 DEG C,
The drying time of the anhydrous slufuric acid lithium and glucose is 2~4h.
Further, the hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, and the Preparation equipment is kipp gas generator.
Compared with prior art, the present invention has at least the following advantages：
1, the purity of the preparation method of a kind of lithium sulfide of the invention, the lithium sulfide of preparation is high, the vulcanization lithium content of preparation
Up to 99.9% or more.
2, the preparation method of a kind of lithium sulfide of the invention, low production cost, preparation method and process are simple, prepare week
Phase is short, and Preparation equipment is simple and easily operated, is convenient for large-scale industrial production.
3, the preparation method of a kind of lithium sulfide of the invention, the safe preparation process of the lithium sulfide is high, the original that uses
Material non-toxic is done harm to, and after the glucose charing, is tightly combined with lithium sulfate, can be improved the transformation efficiency of lithium sulfide.
Specific implementation mode
With reference to embodiment, the invention will be further described, and following embodiment is descriptive, is not limited
, protection scope of the present invention cannot be limited with this.
Embodiment 1
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 1:2:5 mixing, in model SK2-4-
It mills under room temperature 6 hours in the planetary ball mill of 12PC3, ball milling speed is 400 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 20 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 290 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 1.0L/h；The heating temperature of the quartz sintered pipes is 900 DEG C；Inside the quartz sintered pipes
Anhydrous slufuric acid lithium, glucose and hard charcoal mixture react 6h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need
It will the heat drying in vacuum drying chamber in advance；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 110 DEG C and 90
DEG C, the drying time of the anhydrous slufuric acid lithium and glucose is 2h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared,
The Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 1 kilogram, 2 kilograms, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 6 hours, then can be generated 0.8 kilogram of lithium sulfide.
Embodiment 2
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 10:1:5 mixing, in model SK2-4-
It mills under room temperature 9 hours in the planetary ball mill of 12PC3, ball milling speed is 600 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 5 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 230 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 0.6L/h；The heating temperature of the quartz sintered pipes is 650 DEG C；It is described quartz sintered pipes it is anhydrous
Lithium sulfate, glucose and hard charcoal mixture react 4h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need thing
The first heat drying in vacuum drying chamber；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 100 DEG C and 70 DEG C, institute
The drying time for stating anhydrous slufuric acid lithium and glucose is 4h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, described
Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 10 kilograms, 1 kilogram, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen and is reacted 4 hours, then can generate 4.5 kilograms of lithium sulfides.
Embodiment 3
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 5:1.5:5 mixing, in model SK2-4-
It mills under room temperature 7.5 hours in the planetary ball mill of 12PC3, ball milling speed is 200 revs/min, the anhydrous slufuric acid lithium, grape
Sugar and hard charcoal are 13 microns in later granularity of milling；The preheating temperature of the quartz sintered pipes is 260 DEG C；The hydrogen is logical
The flow for entering quartzy sintered pipes is 0.8L/h；The heating temperature of the quartz sintered pipes is 400 DEG C；The nothing of the quartz sintered pipes
Water lithium sulfate, glucose and hard charcoal mixture react 2h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need
The heat drying in vacuum drying chamber in advance；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 120 DEG C and 100
DEG C, the drying time of the anhydrous slufuric acid lithium and glucose is 3h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared,
The Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 5 kilograms, 1.5 kilograms, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 2 hours, then can be generated 4.5 kilograms of lithium sulfides.
Embodiment 4
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 8:2:5 mixing, in model SK2-4-
It mills under room temperature 8 hours in the planetary ball mill of 12PC3, ball milling speed is 600 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 10 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 290 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 0.6L/h；The heating temperature of the quartz sintered pipes is 900 DEG C；It is described quartz sintered pipes it is anhydrous
Lithium sulfate, glucose and hard charcoal mixture react 6h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need thing
The first heat drying in vacuum drying chamber；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 120 DEG C and 100 DEG C,
The drying time of the anhydrous slufuric acid lithium and glucose is 4h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, institute
It is kipp gas generator to state Preparation equipment.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 8 kilograms, 2 kilograms, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 6 hours, then can be generated 2.8 kilograms of lithium sulfides.
Embodiment 5
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 5:2:5 mixing, in model SK2-4-
It mills under room temperature 8 hours in the planetary ball mill of 12PC3, ball milling speed is 550 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 9 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 290 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 0.7L/h；The heating temperature of the quartz sintered pipes is 400 DEG C；It is described quartz sintered pipes it is anhydrous
Lithium sulfate, glucose and hard charcoal mixture react 6h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need thing
The first heat drying in vacuum drying chamber；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 100 DEG C and 70 DEG C, institute
The drying time for stating anhydrous slufuric acid lithium and glucose is 4h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, described
Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 5 kilograms, 2 kilograms, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 6 hours, then can be generated 4 kilograms of lithium sulfides.
Embodiment 6
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 10:2:5 mixing, in model SK2-4-
It mills under room temperature 9 hours in the planetary ball mill of 12PC3, ball milling speed is 600 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 6 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 290 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 1.0L/h；The heating temperature of the quartz sintered pipes is 900 DEG C；It is described quartz sintered pipes it is anhydrous
Lithium sulfate, glucose and hard charcoal mixture react 6h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need thing
The first heat drying in vacuum drying chamber；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 100 DEG C and 70 DEG C, institute
The drying time for stating anhydrous slufuric acid lithium and glucose is 4h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, described
Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 10 kilograms, 2 kilograms, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 6 hours, then can be generated 7.5 kilograms of lithium sulfides.
Embodiment 7
A kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and is connect in quartzy sintered pipes interface
Upper kipp gas generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
Wherein, the anhydrous slufuric acid lithium, hard charcoal and glucose in mass ratio 1:1:5 mixing, in model SK2-4-
It mills under room temperature 9 hours in the planetary ball mill of 12PC3, ball milling speed is 600 revs/min, the anhydrous slufuric acid lithium, glucose
In later granularity of milling it is 6 microns with hard charcoal；The preheating temperature of the quartz sintered pipes is 290 DEG C；The hydrogen is passed through
The flow of quartzy sintered pipes is 1.0L/h；The heating temperature of the quartz sintered pipes is 900 DEG C；It is described quartz sintered pipes it is anhydrous
Lithium sulfate, glucose and hard charcoal mixture react 6h after being passed through hydrogen；The anhydrous slufuric acid lithium and glucose need thing
The first heat drying in vacuum drying chamber；The drying temperature of the anhydrous slufuric acid lithium and glucose is respectively 100 DEG C and 70 DEG C, institute
The drying time for stating anhydrous slufuric acid lithium and glucose is 4h；The hydrogen is added in dilute sulfuric acid by zinc granule and is prepared, described
Preparation equipment is kipp gas generator.
The heating zone range of the quartz heating-pipe according to vulcanization reason yield number and adjust, yield pursuit it is high when,
The effective heating area domain maximum of the quartz sintered pipes can be more than 300mm.For example, using the preparation condition of the present embodiment, by institute
Anhydrous slufuric acid lithium, hard charcoal and glucose are stated respectively according to 1 kilogram, 1 kilogram, 5 kilograms of mass ratio in quartzy sintered pipes
The effective heating areas 300mm domain is reacted, and is passed through hydrogen 6 hours, then can be generated 0.8 kilogram of lithium sulfide.
More than, it is merely preferred embodiments of the present invention, but the protection domain invented is not limited thereto, it is any ripe
Know those skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in should all be contained
Lid is within protection scope of the present invention.Therefore, the scope of protection of the invention shall be subject to the scope of protection specified in the patent claim.
Claims (10)
1. a kind of preparation method of lithium sulfide, which is characterized in that include the following steps：
1) anhydrous slufuric acid lithium, glucose and hard charcoal are milled and is moved into the quartzy sintered pipes of vacuum tube furnace after mixing；
2) the quartzy sintered pipes are preheated, then by electron tubes type stove evacuation, and connects and open in quartzy sintered pipes interface
General generator；
3) it is passed through hydrogen in the quartzy sintered pipes and heats the quartzy sintered pipes, reaction prepares the lithium sulfide.
2. the preparation method of lithium sulfide according to claim 1, which is characterized in that the anhydrous slufuric acid lithium, hard charcoal and
Glucose in mass ratio 1:2:5~10:1:5 mixing, mill 6~9 hours, speed of milling is in planetary ball mill under room temperature
200~600 revs/min.
3. the preparation method of lithium sulfide according to claim 2, which is characterized in that the anhydrous slufuric acid lithium, glucose and
Hard charcoal is 5~20 microns in later granularity of milling.
4. the preparation method of lithium sulfide according to claim 2, which is characterized in that the preheating temperature of the quartz sintered pipes
It is 230 DEG C~290 DEG C.
5. the preparation method of lithium sulfide according to claim 4, which is characterized in that the hydrogen is passed through quartzy sintered pipes
Flow is 0.2~1.0L/h.
6. the preparation method of lithium sulfide according to claim 5, which is characterized in that the heating temperature of the quartz sintered pipes
Between 400-900 DEG C.
7. the preparation method of lithium sulfide according to claim 6, which is characterized in that the anhydrous slufuric acid of the quartz sintered pipes
Lithium, glucose and hard charcoal mixture react 2~6h after being passed through hydrogen.
8. the preparation method of lithium sulfide according to claim 7, which is characterized in that the anhydrous slufuric acid lithium and glucose need
It will the heat drying in vacuum drying chamber in advance.
9. the preparation method of lithium sulfide according to claim 8, which is characterized in that the anhydrous slufuric acid lithium and glucose
Drying temperature is respectively 100-120 DEG C and 70-100 DEG C, and the drying time of the anhydrous slufuric acid lithium and glucose is 2~4h.
10. according to the preparation method of claim 1-9 any one of them lithium sulfides, which is characterized in that the hydrogen is by zinc granule
It is added in dilute sulfuric acid and is prepared, the Preparation equipment used is the kipp gas generator.
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Cited By (4)
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| CN112520703A (en) * | 2020-08-03 | 2021-03-19 | 浙江工业大学 | Green preparation method of lithium sulfide |
| CN113991073A (en) * | 2021-09-27 | 2022-01-28 | 杭州电子科技大学 | Preparation method of lithium sulfide electrode material |
| CN114275742A (en) * | 2021-12-24 | 2022-04-05 | 中南大学 | Preparation method of lithium sulfide capable of realizing continuous production |
| WO2023036284A1 (en) * | 2021-09-10 | 2023-03-16 | 深圳市研一新材料有限责任公司 | Lithium sulfide for solid electrolyte, and preparation method therefor and use thereof |
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| CN112520703A (en) * | 2020-08-03 | 2021-03-19 | 浙江工业大学 | Green preparation method of lithium sulfide |
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| CN113991073B (en) * | 2021-09-27 | 2023-08-11 | 杭州电子科技大学 | Preparation method of lithium sulfide electrode material |
| CN114275742A (en) * | 2021-12-24 | 2022-04-05 | 中南大学 | Preparation method of lithium sulfide capable of realizing continuous production |
| 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 |
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