CN104241651A - Method for preparing sulphur-supported porous carbon lithium battery electrode material by using waste polyurethane plastic - Google Patents
Method for preparing sulphur-supported porous carbon lithium battery electrode material by using waste polyurethane plastic Download PDFInfo
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- CN104241651A CN104241651A CN201410445255.9A CN201410445255A CN104241651A CN 104241651 A CN104241651 A CN 104241651A CN 201410445255 A CN201410445255 A CN 201410445255A CN 104241651 A CN104241651 A CN 104241651A
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- H01M4/00—Electrodes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The invention discloses a method for preparing a sulphur-supported porous carbon lithium battery electrode material by using waste polyurethane plastic. The method comprises the following steps: with sublimed sulphur, potassium carbonate and waste polyurethane as raw materials, performing high-temperature heat treatment on the raw materials in a muffle furnace to prepare porous carbon, and performing hot melting and mechanical dispersing to prepare the sulphur-supported porous carbon lithium battery electrode material active substance. The method is characterized in that elemental sulphur is calcined and melted to enter the pores of porous carbon, electrode material slurry is prepared through a mechanical dispersing method, and finally drying by a vacuum drying oven is carried out to obtain the sulphur-supported porous carbon composite electrode material. Through an electrochemical test, the novel sulphur-supported porous carbon composite electrode material is high in cyclic stability, remarkable in rate performance and simple to prepare, is prepared from cheap raw materials, and has a commercial potential; in addition, test conditions are mild.
Description
Technical field
The present invention relates to a kind of method that the electrode material of lithium battery of porous carbon sulfur loaded prepared by waste polyurethane plastics, belong to lithium ion power battery electrode technical field of material.
Background technology
Along with the development of society, the environmental consciousness of people is more and more stronger, and electric automobile (EV) receives increasing concern as a kind of vehicles of new green power.Lithium ion battery as its power becomes hot technology equally, and in order to adapt to the needs of electric motor car, it is high that preparation has specific capacity, and energy density is large, and the electrode material of good cycle becomes the key of Development of Electric Vehicles technology.The theoretical specific capacity (1675 mAh/g) of its superelevation of thioneine and theoretical specific energy density (2500 KW/kg) most probable become the lithium ion battery as electric car power supply of future generation.And element sulphur itself has two large defects as electrode material.First sulphur simple substance itself is neither electronic conductor neither ion conductor, and it two is that sulphur can form polysulfide and be dissolved in the electrolyte of battery in the process of discharge and recharge.This directly results in the problems such as the cycle life of lithium-sulfur cell, coulombic efficiency be low.The commercialization of what these problems were serious hinder lithium-sulfur cell.In order to limit this drawback, general other as carbon nanotube encapsulation (J. Power Sources 2012,202,394-339.), coated (the J. Mater. Chem. A 2013 of carbon, 1,6602-6608.), the technology such as coated, the doping (Nat. Commun. 2011,2,325.) of nucleocapsid or template lambda limiting process, macromolecule layer limits the dissolving of polysulfide.Although above method can both suppress the dissolving of polysulfide to a certain extent, improve the cycle performance of electrode material, because its preparation method is complicated, experiment condition harshness all fails to realize commercially producing on a large scale.
Porous carbon is black powder or granular amorphous carbon, it is a kind of artificial material with carbon element with highly developed pore structure and very high surface areas, its physicochemical properties are stablized, acid and alkali-resistance, can stand that water is wet, high temperature and high pressure, water insoluble and organic solvent, using after losing efficacy and can regenerate, is a kind of recycling economy material.It is widely used in the fields such as industry, agricultural, national defence, traffic, medical and health, environmental protection.The industrial development of ammonia ester is very fast, the consumption figure of polyurethane doubles substantially for every ten years in the world, meanwhile, a large amount of discarded object is created in the manufacture and usage process of polyurethane, polyurethane material is as a kind of important high polymer, and its reasonable recycling will have great Social benefit and economic benefit.Discarded polyurethane plastics is prepared into there is micropore and mesoporous porous carbon materials, and be used on lithium-sulfur cell, can sulphur be consolidated and the dissolving of the polysulfide that inhibit sulphur to produce in charge and discharge process.The combination electrode material of the porous carbon sulfur loaded of this kind of method acquisition has good stable circulation performance and high rate performance after tested, has given full play of the characteristic of the height ratio capacity of sulphur.
Research about lithium sulphur battery electrode material is more, and the dissolving of the conductivity and suppression polysulfide of improving sulphur by different control methods (the solid sulphur of porous mass, polymeric coating layer coating bag sulphur and doping three directions) is the key technology of lithium-sulfur cell.Wherein utilize the material of porous class to carry sulphur and just had relevant report as far back as 2009, Nazar etc. have inserted sulphur in a kind of ordered mesopore carbon (CMK-3), improve the cycle performance (Nat. Mater. 2009,8,500-506.) of sulphur with this.Chen etc. think that ordered mesoporous carbon material has the mesoporous of larger inner surface area, high porosity and suitable lithium ion conduction, are a kind of well sulfur-donors.They think that best sulfur content is 60%, and the first circle of the material that they prepare discharges 1138 mAh/g, can stable circulation 400 enclose (Electrochim. Acta. 2011,56,9549-9555.) under the current density of 6C.Wang etc. then employ the carrier of micropore-mesopore carbon as sulphur, and think that micropore can effectively keep electrolyte to limit the loss of sulphur, and the mesoporous conduction pathway as lithium ion is active material transmission lithium ion, this material can to circulate 800 (Phys. Chem. Chem. Phys. 2012 under the current density of 1.8 C in charge and discharge, 14,8703-8710).Li etc. are by carrying out activation processing with KOH to active carbon and this material being applied in lithium-sulfur cell as carrier, their experimental result shows when a year sulfur content is 64%, material has best chemical property to comprise the utilance of sulphur, specific discharge capacity and cyclical stability (J. Power Sources. 2013,240,598-605.).The glucose such as Gao carrys out synthetic microporous carbon ball as presoma, and pore diameter distribution is less than 1nm.This material has good cyclical stability, and 42 wt%'s carries sulfur content and the specific capacity (Energy Environ. Sci. 2010,3,1531 – 1537.) more than 900mAh/g.
In a word, seek a kind of porous, the carrier of conduction solves the effect and to improve the nonconducting characteristic of sulphur itself be design the key of lithium sulphur battery electrode material of shuttling back and forth of the generation of sulphur in charge and discharge process.
Summary of the invention
For the defect that prior art exists, the object of this invention is to provide a kind of method that the electrode material of lithium battery of porous carbon sulfur loaded prepared by waste polyurethane plastics, its preparation process includes hot melt and mechanical dispersion method; Specifically, allow elemental sulfur melting enter in the hole of this special porous carbon by calcining exactly, mechanical dispersion method prepares electrode material slurries, obtains the combination electrode material of porous carbon sulfur loaded eventually through vacuum drying chamber drying.
For achieving the above object, the present invention is achieved by the following technical solutions:
A method for the electrode material of lithium battery of porous carbon sulfur loaded prepared by waste polyurethane plastics, has following technical process and step:
A. waste polyurethane plastics pulverizer is pulverized, take 5-15g polyurethane plastics powder, pour into after fully mixing with the potassium carbonate powder of 15-45g in porcelain crucible, cover lid puts into Muffle furnace, temperature controlled at 500-1000 DEG C, the reaction time controls at 30-120min; The product obtained first is washed 10-20min with boiling water, then uses deionized water at normal temperature cyclic washing to neutral, put into oven drying 22-24h, obtained porous carbon materials;
B. get sublimed sulfur respectively, porous carbon prepared by step a, ball milling 30min-1h mixes, and puts into 155 DEG C, tube furnace calcining 12-14h, obtains the fine powder of black; The mass ratio of sulphur and porous carbon is 2.5:1-4:1;
C. get fine powder prepared by step b, conductive carbon black grinding 30min-1h mixes, wherein the mass ratio of porous carbon and conductive carbon is 1:1; Transferred in small beaker by mixture and add adhesive, abundant mix and blend 10min, obtains gluey black liquor; With high speed inner-rotary type beater dispersion slurries, each one minute repeats 5-10 time, obtains the gluey electrode slurry of black of homogeneous sulphur/porous carbon/conductive carbon;
D. be coated on uniformly by the black paste in step c on the metallic aluminium collector handled well in advance, be placed in vacuum drying oven dry, it is 60-80 DEG C that temperature arranges scope, drying time 20-24h; The electrode material of lithium battery of final obtained porous carbon sulfur loaded.
Adhesive in described step c is that Kynoar (PVDF) is dissolved in 1-METHYLPYRROLIDONE (NMP); The mass ratio of electrode material and adhesive is 8:1-9:1.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant advantage:
The electrode material of lithium battery of porous carbon sulfur loaded prepared by the present invention through the known good cycling stability of electro-chemical test, preparation method is simple, experiment condition is gentle, raw material are cheap, have business-like may and be applied to pure electric automobile.
Accompanying drawing explanation
X-ray diffraction (XRD) collection of illustrative plates of the electrode material of lithium battery of Fig. 1 porous carbon sulfur loaded.
Transmission electron microscope (TEM) photo of the electrode material of lithium battery of Fig. 2 porous carbon sulfur loaded.
The cycle performance figure of the grading current discharge and recharge of the electrode material of lithium battery of Fig. 3 porous carbon sulfur loaded.
The cycle performance figure of small area analysis (0.1 C) discharge and recharge of the electrode material of lithium battery of Fig. 4 porous carbon sulfur loaded.
Embodiment
After now specific embodiments of the invention being described in.
The method of the electrode material of lithium battery of porous carbon sulfur loaded prepared by a kind of waste polyurethane plastics, there is following technical process and step: the waste polyurethane plastics got after 10 g pulverizing fully mix with 30 g potassium carbonate powder, put into porcelain crucible, after covering porcelain crucible lid, crucible is put into and be warmed up to 800 DEG C of Muffle furnaces in advance, porcelain crucible is taken out after reacting 60 min, solid in porcelain crucible is poured in preprepared boiling water, boils 10 min.Use Buchner funnel suction filtration again, the solid product obtained is spent repeatedly deionized water to neutral, put into oven drying 24 h.Finally the powder agate mortar of drying is ground to form homogeneous powder for subsequent use.
Get the sublimed sulfur of 6 g respectively, 1.5 g above-mentioned porous carbon ball milling 45 min mixes, put into the fine powder that 155 DEG C, tube furnace calcining, 12 h obtain black; Material 0.75 g of above-mentioned preparation, conductive carbon 0.15 g are ground 30 min and mix.Mixture is transferred in small beaker and adds 0.1 g and be dissolved in adhesive Kynoar (PVDF) in 1-METHYLPYRROLIDONE (NMP), abundant mix and blend 10 min, obtains gluey black liquor; With high speed inner-rotary type beater dispersion slurries, each one minute repeats 10 times, obtains the gluey slurry of black of homogeneous sulphur/porous carbon/conductive carbon.
Be coated on uniformly on the metallic aluminium collector handled well in advance by above-mentioned black paste, be placed in vacuum drying oven dry, temperature 80 DEG C, drying time 22, h, finally obtained the electrode material of lithium battery of porous carbon sulfur loaded.
the assembling of battery and test thereof
The above-mentioned electrode to be measured prepared is put into self-control stainless steel battery mould test.Using high purity lithium sheet as negative pole, polypropylene porous film (Celgard 2400) is barrier film, electrolyte is the trifluoromethanesulfonyl chloride LiTFSI of 1 mol/L and the mixed solution of 1,3-dioxolanes (DOL)/dimethyl ether (DME) (weight ratio is 1:1).Being assembled in the glove box being full of high-purity argon gas of battery is carried out.Measuring current density is 0.1C, 0.2C, 0.5C, 1C and 2C, and wherein 1C equals 1675 mA/g, and test voltage scope is 1-3 V.
As shown in Figure 1: the analysis showed that product is the composite material of sulphur load on porous carbon that degree of crystallinity is higher.Be illustrated in figure 2 its TEM photo: can find out porous carbon sulfur loaded composite material, porous carbon presents diaphanous film, and sulphur is evenly dispersed in the surfaces externally and internally of porous carbon.Be illustrated in figure 3 the ladder charging and discharging capacity performance map of porous carbon load S composite material front 60 circles under different current density.As can be seen from Figure 3, current density is 167mA/g(0.1C) time, first circle charging and discharging capacity is respectively 552mAh/g and 612mAh/g; Current density is 334mA/g(0.2C) time, charging and discharging capacity is respectively 355mAh/g and 427mAh/g; Current density is 835mA/g(0.5C) time, charging and discharging capacity is respectively 278mAh/g and 302mAh/g; Current density is 1670mA/g(1C) time, charging and discharging capacity is respectively 229mAh/g and 240mAh/g; Current density is 3340mA/g(2C) time, charging and discharging capacity remains on 192mAh/g and 202mAh/g respectively; Current density is 8350mA/g(5C) time, charging and discharging capacity remains on 124mAh/g and 130mAh/g respectively.As can be seen from Figure 4, battery charging and discharging capacity after small area analysis (0.1C) charge and discharge circulation 50 circle can both remain on ~ 400mAh/g.This material visible have certain stable circulation performance and good high rate performance, there are business-like potentiality.
Claims (2)
1. prepare a method for the electrode material of lithium battery of porous carbon sulfur loaded with waste polyurethane plastics, it is characterized in that, there is following technical process and step:
A. waste polyurethane plastics pulverizer is pulverized, take 5-15g polyurethane plastics powder, pour into after fully mixing with the potassium carbonate powder of 15-45g in porcelain crucible, cover lid puts into Muffle furnace, temperature controlled at 500-1000 DEG C, the reaction time controls at 30-120min; The product obtained first is washed 10-20min with boiling water, then uses deionized water at normal temperature cyclic washing to neutral, put into oven drying 22-24h, obtained porous carbon materials;
B. get sublimed sulfur respectively, porous carbon prepared by step a, ball milling 30min-1h mixes, and puts into 155 DEG C, tube furnace calcining 12-14h, obtains the fine powder of black; The mass ratio of sulphur and porous carbon is 2.5:1-4:1;
C. get fine powder prepared by step b, conductive carbon black grinding 30min-1h mixes, wherein the mass ratio of porous carbon and conductive carbon is 1:1; Transferred in small beaker by mixture and add adhesive, abundant mix and blend 10min, obtains gluey black liquor; With high speed inner-rotary type beater dispersion slurries, each one minute repeats 5-10 time, obtains the gluey electrode slurry of black of homogeneous sulphur/porous carbon/conductive carbon;
D. be coated on uniformly by the black paste in step c on the metallic aluminium collector handled well in advance, be placed in vacuum drying oven dry, it is 60-80 DEG C that temperature arranges scope, drying time 20-24h; The electrode material of lithium battery of final obtained porous carbon sulfur loaded.
2. the method for the electrode material of lithium battery of porous carbon sulfur loaded prepared by waste polyurethane plastics according to claim 1, it is characterized in that, the adhesive in described step c is that Kynoar is dissolved in 1-METHYLPYRROLIDONE; The mass ratio of electrode material and adhesive is 8:1-9:1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104843673A (en) * | 2015-04-30 | 2015-08-19 | 昆明理工大学 | Porous carbon material preparing method |
| CN107140633A (en) * | 2017-07-10 | 2017-09-08 | 扬州大学 | A kind of preparation method and applications of the activated carbon with high specific surface area of biomass derived |
| CN111048782A (en) * | 2019-12-23 | 2020-04-21 | 北京理工大学重庆创新中心 | Preparation method and calcination temperature optimization method of nitrogen-doped conductive carbon material for lithium-sulfur battery |
| CN111357136A (en) * | 2017-11-03 | 2020-06-30 | 株式会社Lg化学 | Sulfur-carbon composite material and lithium-sulfur battery comprising same |
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| CN102163720A (en) * | 2011-02-12 | 2011-08-24 | 中南大学 | Lithium sulfide-porpous carbon compound positive material for lithium ion battery and preparation method thereof |
| CN103094535A (en) * | 2013-01-21 | 2013-05-08 | 北京化工大学 | Sulfur/carbon porous nano composite material and preparation method and application thereof |
| CN103236560A (en) * | 2013-04-16 | 2013-08-07 | 浙江大学 | Lithium-sulfur battery sulfur/carbon composite positive electrode material, preparation method and applications thereof |
| CN103754869A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing high-quality active carbon by adopting waste polyurethane foamed plastic |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102163720A (en) * | 2011-02-12 | 2011-08-24 | 中南大学 | Lithium sulfide-porpous carbon compound positive material for lithium ion battery and preparation method thereof |
| CN103094535A (en) * | 2013-01-21 | 2013-05-08 | 北京化工大学 | Sulfur/carbon porous nano composite material and preparation method and application thereof |
| CN103236560A (en) * | 2013-04-16 | 2013-08-07 | 浙江大学 | Lithium-sulfur battery sulfur/carbon composite positive electrode material, preparation method and applications thereof |
| CN103754869A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing high-quality active carbon by adopting waste polyurethane foamed plastic |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104843673A (en) * | 2015-04-30 | 2015-08-19 | 昆明理工大学 | Porous carbon material preparing method |
| CN107140633A (en) * | 2017-07-10 | 2017-09-08 | 扬州大学 | A kind of preparation method and applications of the activated carbon with high specific surface area of biomass derived |
| CN111357136A (en) * | 2017-11-03 | 2020-06-30 | 株式会社Lg化学 | Sulfur-carbon composite material and lithium-sulfur battery comprising same |
| CN111357136B (en) * | 2017-11-03 | 2022-09-06 | 株式会社Lg新能源 | Sulfur-carbon composite material and lithium-sulfur battery comprising same |
| US11611067B2 (en) | 2017-11-03 | 2023-03-21 | Lg Energy Solution, Ltd. | Sulfur-carbon composite and lithium-sulfur battery including same |
| CN111048782A (en) * | 2019-12-23 | 2020-04-21 | 北京理工大学重庆创新中心 | Preparation method and calcination temperature optimization method of nitrogen-doped conductive carbon material for lithium-sulfur battery |
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