CN109546148A - A kind of method that chestnut peel prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material - Google Patents
A kind of method that chestnut peel prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material Download PDFInfo
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Abstract
A kind of method that chestnut peel prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, chestnut peel is added to the water, neutral filtering is diluted to 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material.The present invention is using chestnut peel 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 chestnut peel prepare it is porous not
The method of the spherical biological carbon lithium-sulfur cell negative electrode material of rule.
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, the biological carbon material of obtained load sulphur
With environment friendly, and it is able to ascend the load capacity of sulphur, the chestnut peel for promoting lithium-sulfur cell capacity prepares porous irregular ball
The method of shape biological carbon lithium-sulfur cell negative electrode material.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) it is dried after taking 2-8g chestnut peel to wash, obtains product A；
2) 100mL water is added in product A, the mixing 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, it is negative that reaction 12-24h obtains porous irregular spherical biological carbon lithium-sulfur cell
Pole material.
The step 1), which is adopted, to be washed with distilled water.
The concentrated acid of the step 2) is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with the volume ratio of 3:4:3.
Step 2) the mixing time is 50-120min.
The step 6,9) argon gas flow velocity are 60-100sccm.
The present invention is using chestnut peel 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) chestnut peel is a kind of biomass castoff, may be used as biological carbon negative pole material sulfur loaded applied to lithium sulphur electricity
Pond.Glucide rich in chestnut peel, hydrolytic process can form porous irregular spherical particle, be able to ascend sulphur
Load capacity promotes lithium-sulfur cell capacity.
4) 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.
5) 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 that the embodiment of the present invention 6 prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material.
Specific embodiment
Embodiment 1:
1) take 2g chestnut peel 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 3:4:3
With the total 10mL of concentrated nitric acid, stirring 50min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, wherein
Argon gas flow velocity is 60sccm.
Embodiment 2:
1) take 8g chestnut peel 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 3:4:3
With the total 60mL of concentrated nitric acid, stirring 120min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, wherein
Argon gas flow velocity is 100sccm.
Embodiment 3:
1) take 8g chestnut peel 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 3:4:3
With the total 60mL of concentrated nitric acid, stirring 70min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, wherein
Argon gas flow velocity is 100sccm.
Embodiment 4:
1) take 8g chestnut peel 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 3:4:3
With the total 60mL of concentrated nitric acid, stirring 100min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, wherein
Argon gas flow velocity is 100sccm.
Embodiment 5:
1) take 6g chestnut peel 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 3:4:3
With the total 45mL of concentrated nitric acid, stirring 115min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material for 24 hours, wherein
Argon gas flow velocity is 100sccm.
Embodiment 6:
1) take 4g chestnut peel 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 3:4:3
With the total 20mL of concentrated nitric acid, stirring 72min 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 porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, wherein
Argon gas flow velocity is 80sccm.
As seen from Figure 1, the chestnut peel obtained has porous irregular chondritic.The diameter of irregular spherical particle
For 40-50nm, the biggish specific surface area of nano-scale provides more spaces with the contact of electrolyte for the storage of sulphur.
Being incorporated as of nitric acid of the present invention introduces nitrogen-containing functional group in biological carbon, since nitrogen has electronegativity, compared to pure carbon
Material is stronger to the adsorptivity of sulphur；Concentrated sulfuric acid strong oxidizing property is stronger, can be carbonized in advance to chestnut peel, while introducing on surface
More oxygen atom, oxygen atom electronegativity is weaker with respect to nitrogen, but still can adsorb sulphur simple substance；Hydrochloric acid is easy to produce volatility gas
Body easily on chestnut peel surface and internal pore-creating, and introduces chlorine atom on surface.By controlling the concentration and additional proportion of acid,
A certain amount of nitrogen-atoms, oxygen atom and chlorine atom can be introduced, due to three under conditions of chestnut peel surface and internal pore-creating
The adsorption capacity of atom pair sulphur is different, and the ability for storing up sulphur is also different.
Claims (5)
1. a kind of method that chestnut peel prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material, it is characterised in that:
1) it is dried after taking 2-8g chestnut peel 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 porous irregular spherical biological carbon lithium-sulfur cell cathode material
Material.
2. the side that chestnut peel according to claim 1 prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material
Method, it is characterised in that: the step 1), which is adopted, to be washed with distilled water.
3. the side that chestnut peel according to claim 1 prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material
Method, it is characterised in that: the concentrated acid of the step 2) is to be separately added into the concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid with the volume ratio of 3:4:3.
4. the side that chestnut peel according to claim 1 prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material
Method, it is characterised in that: the step 2) mixing time is 50-120min.
5. the side that chestnut peel according to claim 1 prepares porous irregular spherical biological carbon lithium-sulfur cell negative electrode material
Method, it is characterised in that: the step 6,9) argon gas flow velocity are 60-100sccm.
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| CN112662204A (en) * | 2020-12-23 | 2021-04-16 | 哈尔滨工业大学 | Preparation method of porous/hollow-like carbon black material for lithium-sulfur battery |
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| CN107697900A (en) * | 2017-09-13 | 2018-02-16 | 陕西科技大学 | The preparation method of the cellular sodium-ion battery carbon electrode material of one species |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112662204A (en) * | 2020-12-23 | 2021-04-16 | 哈尔滨工业大学 | Preparation method of porous/hollow-like carbon black material for lithium-sulfur battery |
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