CN109574005A - A kind of preparation method of lithium-sulfur cell cathode biology carbon material - Google Patents
A kind of preparation method of lithium-sulfur cell cathode biology carbon material Download PDFInfo
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- CN109574005A CN109574005A CN201811459444.6A CN201811459444A CN109574005A CN 109574005 A CN109574005 A CN 109574005A CN 201811459444 A CN201811459444 A CN 201811459444A CN 109574005 A CN109574005 A CN 109574005A
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Abstract
A kind of preparation method of lithium-sulfur cell cathode biology carbon material, dandelion is added to the water, and is diluted to neutral filtering after concentrated acid reaction then is added thereto, is dried to obtain product C；The concentrated sulfuric acid and water are added in product C, is placed in reaction solution D in hydrothermal reaction kettle, solution D is diluted to neutral filtering, dry product E；By layer overlay electrically conductive graphite uniform on product, heating reaction obtains product F in tube furnace；Product F is rinsed, is filtered, drying obtains product G；Product G is mixed to obtain to mixture H with sulphur powder；Mixture H is placed in temperature reaction in tube furnace and obtains biological carbon negative pole material.The present invention is using dandelion as biomass material, and using first mixed acid pre-soaking, rear hydro-thermal method prepares biological carbon matrix precursor, activation time is controlled in later period activation, regulation obtains being suitable for the biological carbon material for storing up sulphur, is applied to lithium-sulfur cell, promotes its chemical property.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium-sulfur cell negative electrode material, and in particular to a kind of lithium-sulfur cell cathode biology
The preparation method of carbon material.
Background technique
The development of portable electronic device is more more and more urgent for the demand of advanced energy storage.Advanced energy resource system it is fast
Fast demand for development material must have low cost, long-life, high safety, high-energy, high-power, advantages of environment protection.Lithium
Sulphur battery can preferably combine These characteristics, in following high-energy (2500Whkg-1) have in storage system compared with
Good application prospect.In the lithium-sulfur cell of high-energy density, the theoretical capacity of sulphur is 1672mAhg-1, lithium an- ode
Theoretical capacity is 3860mAhg-1.In charge and discharge process, lithium ion is generated from metal lithium electrode, is diffused by electrolyte
Sulfur electrode, electronics are flowed from external circuit, and final discharging product Li is generated at cathode2S.However, the technology of lithium-sulfur cell hinders
Hinder and limit its application, for example cycle period is short, the content of sulfur loaded is low.Reason mainly has the following: (1) due in sun
Polysulfide intermediate product is generated in pole and cathode, and complicated the Nomenclature Composition and Structure of Complexes variation is generated during forming polysulfide,
Easily dissolution causes capacitance loss to polysulfide in the electrolytic solution, and the cyclical stability of electrode is poor；(2) sulphur and discharging product Li2S
With ion and electronic isolation, the electric conductivity of material is reduced.(3) polysulfide moves in circles between the anode and the cathode,
The loss of active material is caused, coulombic efficiency is lower, and surface of metal electrode is passivated, and generates insulation product Li2S/Li2S2。
(4) loss of metal lithium electrode is prevented mainly due to the passivation on surface and the formation (SEI film) of unstable solid-liquid interphase
The long-range cyclical stability of lithium-sulfur cell.
In recent years, largely studies have shown that the above problem can be negative by introducing sulphur-carbon, sulphur-polymer composites
The methods of pole, novel battery system, stable lithium an- ode are realized.Result of study specifically includes that (1) introduces new battery composition
Material and structure (cathode, binder, electrolyte and anode).(2) mechanism study of Li-S redox chemistry reaction.(3) exist
Conducting base (such as: carbon, polymer, metal) is introduced in sulfur electrode.This method can promote the electric conductivity of material to a certain degree,
But its energy density can also reduce.Research for novel electrode structure, main includes using sulphur-carbon, sulphur-polymer nanocomposite
Composite material, the storage of porous polysulfide, porous current collector, binder, self-supporting combination electrode, cathode and separator interlayer
Away from, polysulfide cathode, surface covering separator, polysulfide cathode, sandwich cathode construction, lithium metal protection and Li2S is living
Change.Based on the studies above, the development and application of the following lithium-sulfur cell still have extensive prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation process is simple, raw material is easy to get, and is able to ascend its chemical property
The preparation method of lithium-sulfur cell cathode biology carbon material.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) it is dried after taking dandelion 2-8g to wash, obtains product A；
2) 100mL water is added in product A, the concentrated acid of 10-60mL is then added thereto, being stirred with glass bar makes it sufficiently
Reaction, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1-5mL concentrated sulfuric acid is added in product C, 45-49mL water is placed in hydrothermal reaction kettle at 160-180 DEG C, reaction
8-30h obtains solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 5-10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 0-10h, is obtained
Product F；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) by product G with sulphur powder with (1-9): the mass ratio of (9-1) mixes, grinding obtain mixture H；
9) mixture H is laid in white alumina porcelain boat, is placed in the tube furnace of argon atmosphere from room temperature with 5-10
DEG C/heating rate of min is warming up to 155-165 DEG C, reaction 12-24h obtains lithium-sulfur cell cathode biology carbon material.
It states step 1) and adopts and be washed with distilled water.
The concentrated acid for stating step 2) is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with volume ratio 6:2:2.
Stating step 2) mixing time is 10-30min.
The step 6,9) argon gas flow velocity are 60-100sccm.
The present invention is using dandelion as biomass material, using first mixed acid pre-soaking, before rear hydro-thermal method preparation biological carbon
Object is driven, activation time is controlled in later period activation, regulation obtains being suitable for the biological carbon material for storing up sulphur, is applied to lithium sulphur electricity
Pond promotes its chemical property.
The beneficial effects of the present invention are embodied in:
1) present invention is using first mixed acid pre-soaking, and the mode of rear hydro-thermal process handles biological carbon matrix precursor, and then at heat
Reason obtains biological carbon material.Biomass exocuticle organic aldehyde, oxidation of ketones are obtained carboxyl structure by acid soak, so hydro-thermal process
Biomass endepidermis is further etched on this basis, and endepidermis lignin from biomass content is higher, thus needs high temperature height
Pressure could homogeneous reaction.
2) synergistic effect of electrically conductive graphite is heat-treated and is added in tube furnace by hydrothermal product to be promoted in the present invention
The electric conductivity of material.Under the protection of inert gas, carboxylic acid molecules, which are decomposed, generates carbon dioxide generation hole, remaining carbon atom
Arrangement recombination forms carbon hexatomic ring, and structure is more orderly, and degree of graphitization is higher.At the same time, hydrothermal product surface is oxygen-containing
Functional group can promote the degree of graphitization and electric conductivity of material entirety with electrically conductive graphite stable bond.
3) in the soaking step of mixed acid of the present invention, the additional proportion and mixing time of mixed acid will affect acid to biomass
The degree of oxidation and etching degree of outer surface, and then influence the structure and post-processing mode of biological carbon in heat treatment process.
4) the carbon material supported sulphur of multilayer tubular biology has been made using dandelion as raw material in the present invention.Due to dandelion itself
With orderly tubular structure, and internal fiber cellulose content is abundant, is not easy to be destroyed in heat treatment process, tubular structure is in charge and discharge
Be conducive to the complete infiltration of electrolyte in electric process.
5) preparation process of the invention is relatively simple, and raw material is easy to get, and the biological carbon material of obtained load sulphur has environment friend
Good property.
6) skeleton of biological carbon of the invention as sulfur loaded, it is suppressed that polysulfide is in the electrolytic solution in charge and discharge process
Dissolution, while carburizing temperature and carrying the control of sulfur content and can change the electric conductivity of carbon material.
Detailed description of the invention
Fig. 1 is the SEM figure of lithium-sulfur cell cathode biology carbon material prepared by the embodiment of the present invention 2.
Specific embodiment
Embodiment 1:
1) take 2g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 10mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1mL concentrated sulfuric acid is added in product C, 49mL water is placed in hydrothermal reaction kettle at 160 DEG C, reacts 30h, obtain
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 5 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 10h, obtains product
F, wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 1:9, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains lithium-sulfur cell cathode biology carbon material, and wherein argon gas flow velocity is
60sccm。
Embodiment 2:
1) take 8g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere and obtains product F, and wherein argon gas flow velocity is
60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 7 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains lithium-sulfur cell cathode biology carbon material, and wherein argon gas flow velocity is
100sccm。
As shown in Figure 1, when carrying sulfur content is 60%, in the biological carbon pipe surface uniform load sulfur granules of nano-scale,
Acid soak and heat treatment do not damage the structure of biomass itself.
Embodiment 3:
1) take 8g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 8 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 2h, obtains product F,
Wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains lithium-sulfur cell cathode biology carbon material, and wherein argon gas flow velocity is
100sccm。
Embodiment 4:
1) take 8g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 60mL of concentrated nitric acid, stirring 10min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 180 DEG C, and reaction for 24 hours, obtains
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 6 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 5h, obtains product F,
Wherein argon gas flow velocity is 60sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 8:2, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 8 DEG C/
The heating rate of min is warming up to 155 DEG C, and reaction 12h obtains lithium-sulfur cell cathode biology carbon material, and wherein argon gas flow velocity is
100sccm。
Embodiment 5:
1) take 6g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 45mL of concentrated nitric acid, stirring 30min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 3mL concentrated sulfuric acid is added in product C, 47mL water is placed in hydrothermal reaction kettle at 160 DEG C, reacts 8h, obtain molten
Liquid D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 8h, obtains product
F, wherein argon gas flow velocity is 80sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 6:4, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5 DEG C/
The heating rate of min is warming up to 160 DEG C, and reaction obtains lithium-sulfur cell cathode biology carbon material for 24 hours, and wherein argon gas flow velocity is
100sccm。
Embodiment 6:
1) take 4g dandelion adopt be washed with distilled water after dry, obtain product A；
2) 100mL water is added in product A, the concentrated sulfuric acid, concentrated hydrochloric acid are then added thereto respectively with the volume ratio of 6:2:2
With the total 20mL of concentrated nitric acid, stirring 28min with glass bar reacts it sufficiently, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 5mL concentrated sulfuric acid is added in product C, 45mL water is placed in hydrothermal reaction kettle at 170 DEG C, reacts 10h, obtain
Solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon gas
1000 DEG C are warming up to the heating rate of 10 DEG C/min from room temperature in the tube furnace of atmosphere, in 1000 DEG C of reaction 8h, obtains product
F, wherein argon gas flow velocity is 100sccm；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) product G is mixed with sulphur powder with the mass ratio of 9:1, grinding obtains mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 10 DEG C/
The heating rate of min is warming up to 165 DEG C, and reaction 20h obtains lithium-sulfur cell cathode biology carbon material, and wherein argon gas flow velocity is
80sccm。
Claims (5)
1. a kind of preparation method of lithium-sulfur cell cathode biology carbon material, it is characterised in that:
1) it is dried after taking dandelion 2-8g to wash, obtains product A；
2) 100mL water is added in product A, the concentrated acid of 10-60mL is then added thereto, being stirred with glass bar keeps it sufficiently anti-
It answers, obtains solution B；
3) solution B is diluted to pH=7, filters, is dried to obtain product C；
4) the 1-5mL concentrated sulfuric acid is added in product C, 45-49mL water is placed in hydrothermal reaction kettle at 160-180 DEG C, reacts 8-
30h obtains solution D；
5) solution D is diluted to pH=7, filters, is dried to obtain product E；
6) product E is laid in white alumina porcelain boat, then uniform layer overlay electrically conductive graphite on it, is placed in argon atmosphere
Tube furnace in from room temperature be warming up to 1000 DEG C with the heating rate of 5-10 DEG C/min, in 1000 DEG C of reaction 0-10h, obtain product
F；
7) it by product F second alcohol and water repeated flushing, filters, drying obtains product G；
8) by product G with sulphur powder with (1-9): the mass ratio of (9-1) mixes, grinding obtain mixture H；
9) mixture H is laid in white alumina porcelain boat, be placed in the tube furnace of argon atmosphere from room temperature with 5-10 DEG C/
The heating rate of min is warming up to 155-165 DEG C, and reaction 12-24h obtains lithium-sulfur cell cathode biology carbon material.
2. the preparation method of lithium-sulfur cell cathode biology carbon material according to claim 1, it is characterised in that: the step
1) it adopts and is washed with distilled water.
3. the preparation method of lithium-sulfur cell cathode biology carbon material according to claim 1, it is characterised in that: the step
2) concentrated acid is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with volume ratio 6:2:2.
4. the preparation method of lithium-sulfur cell cathode biology carbon material according to claim 1, it is characterised in that: the step
2) mixing time is 10-30min.
5. the preparation method of lithium-sulfur cell cathode biology carbon material according to claim 1, it is characterised in that: the step
6,9) argon gas flow velocity be 60-100sccm.
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| CN110917232A (en) * | 2019-12-10 | 2020-03-27 | 苏州科技大学 | Method for applying medical natural product targeted medicine of dandelion extracted by hydrothermal method to mainly treat dermatitis allergy |
| CN111554934A (en) * | 2020-05-14 | 2020-08-18 | 陕西科技大学 | Biochar-loaded titanium dioxide for lithium-sulfur battery electrode and preparation method thereof |
| CN113087014A (en) * | 2021-03-31 | 2021-07-09 | 杭州艺深新材料有限公司 | Preparation method of carbon/selenium-doped titanium dioxide lithium-sulfur battery positive electrode material |
| KR20220007535A (en) * | 2020-07-10 | 2022-01-18 | 고려대학교 산학협력단 | Method for fabricating biochar based eledctrode and electrical energy storage device including the same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110917232A (en) * | 2019-12-10 | 2020-03-27 | 苏州科技大学 | Method for applying medical natural product targeted medicine of dandelion extracted by hydrothermal method to mainly treat dermatitis allergy |
| CN111554934A (en) * | 2020-05-14 | 2020-08-18 | 陕西科技大学 | Biochar-loaded titanium dioxide for lithium-sulfur battery electrode and preparation method thereof |
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| KR20220007535A (en) * | 2020-07-10 | 2022-01-18 | 고려대학교 산학협력단 | Method for fabricating biochar based eledctrode and electrical energy storage device including the same |
| CN113087014A (en) * | 2021-03-31 | 2021-07-09 | 杭州艺深新材料有限公司 | Preparation method of carbon/selenium-doped titanium dioxide lithium-sulfur battery positive electrode material |
| CN113087014B (en) * | 2021-03-31 | 2022-07-01 | 江西普瑞森新能源科技有限公司 | Preparation method of carbon/selenium-doped titanium dioxide lithium-sulfur battery positive electrode material |
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