CN107394162A - A kind of electrode material that lithium ion battery is prepared using sludge and its preparation method and application - Google Patents

A kind of electrode material that lithium ion battery is prepared using sludge and its preparation method and application Download PDF

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Publication number
CN107394162A
CN107394162A CN201710613715.8A CN201710613715A CN107394162A CN 107394162 A CN107394162 A CN 107394162A CN 201710613715 A CN201710613715 A CN 201710613715A CN 107394162 A CN107394162 A CN 107394162A
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China
Prior art keywords
sludge
lithium ion
electrode material
ion battery
prepared
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CN201710613715.8A
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Chinese (zh)
Inventor
张利锋
神克超
贺文杰
刘毅
郭守武
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Priority to CN201710613715.8A priority Critical patent/CN107394162A/en
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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
    • H01M4/362—Composites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a kind of method that lithium ion battery is prepared using sludge.Comprise the following steps that：Wet mud is dried for 1~2 hour at 120 DEG C, the sludge of drying is calcined a few hours at a certain temperature, then mixed according to a certain percentage with graphite, ball milling 5~15 hours.Product is prepared into lithium ion battery as electrode material and tests its performance.The main component of product is silica and graphite, in irregular particle shape pattern.The preparation method is simple to operate, and reaction condition is general, and cost is low, can be directly used for industrial-scale production, and processing for sludge and using providing theoretical foundation and practical experience.

Description

A kind of electrode material that lithium ion battery is prepared using sludge and preparation method thereof and Using
【Technical field】
The invention belongs to inorganic micro Nano material preparation field, more particularly to a kind of prepare lithium ion battery using sludge Electrode material and its preparation method and application.
【Background technology】
Lithium ion battery is a kind of new electrochmical power source, and because it has, energy density is big, cycle performance is excellent, memoryless Effect, security performance be high, the advantage such as environment-friendly, receives the favor of people.For lithium ion battery, electrode material is shadow The key factor of battery performance and cost is rung, important component of the negative material as lithium battery, becomes research work The research emphasis of person.At present, commercialized lithium cell cathode material is mainly based on graphite.Graphite electrode material is although with good Good cycle performance, but relatively low theoretical specific capacity (372mAh/g) constrains the realization of commercialization lithium battery high-energy-density； Meanwhile graphite is a kind of non-renewable resources, immoderate use will necessarily cause the exhaustion of resource.
In order to better meet commercialized requirement, scientific research personnel is researching and developing the negative material of ultra-high capacity.Such as Chinese patent CN201310435744.1 discloses a kind of lithium ion battery silicon/silica carbon graphite composite negative pole material, and this is special Profit has invented a kind of silicon/silica carbon graphite composite negative pole material using graphite as framework material；Chinese patent CN201310554493.9 discloses lithium ion battery anode active material and preparation method thereof and lithium ion battery, the invention Potassium permanganate, hydrogen chloride and polyvinylpyrrolidone is used to prepare manganese dioxide nano pipe after hydro-thermal for raw material；China Patent CN201310007838.9 discloses a kind of preparation method of silicon dioxide/ carbon composite negative electrode material for lithium ion battery, should Method prepares porous silica by sol-gel process and atmosphere pressure desiccation, next carries out carbon bag to silica Cover and be thermally treated resulting in target product.Above-mentioned invention requires high there is complex process, experimental facilities, prepares cost height, pollution The problems such as environment, it is unfavorable for commercialized application.
Municipal sludge is a kind of very big solid waste of harmfulness.During municipal sewage treatment, the dirt in sewage Dye thing is enriched with, concentrates and be transferred in sludge, forms municipal sludge.The conventional method of China's processing sludge mainly have burning, Fill, arrange the methods of extra large, but these methods can produce secondary pollution.It has been investigated that the main component of sludge is titanium dioxide Silicon and organic matter, silica are a kind of lithium cell cathode materials.The present invention use sludge and graphite as raw material, through calcining- The method of ball milling prepares a kind of electrode material of lithium battery.This method is simple to operate, and reaction condition is general, and cost is low, can be direct For industrial-scale production.
【The content of the invention】
The shortcomings that it is an object of the invention to overcome above-mentioned prior art, there is provided one kind prepares lithium ion battery using sludge Electrode material and its preparation method and application.Preparation method technique provided by the invention is simple, reaction condition is general, is produced into This is low, can mass produce.
To reach above-mentioned purpose, the present invention is achieved using following technical scheme：
A kind of method for the electrode material that lithium ion battery is prepared using sludge, is comprised the following steps：
1) wet mud is dried；
2) sludge of drying is calcined into 2~6h at a temperature of 400~600 DEG C；
3) after burnt sludge is mixed with graphite, abundant ball milling, the electrode material for preparing lithium ion battery is obtained Material.
Further improve of the invention is：
In step 1), wet mud is carried out at 120 DEG C, drying time 1-2h.
In step 2), calcination atmosphere is air or argon gas.
Sludge is with graphite according to 20:The mass ratio mixing of (1~5).
Ball-milling Time is 5~15h.
A kind of electrode material, electrode material are granular silica, a diameter of 300~500nm.
A kind of electrode material prepared using sludge is used for the application for preparing lithium ion battery.
Compared with prior art, the invention has the advantages that：
The present invention is raw material using sludge and graphite, and a kind of lithium ion battery anode material has been synthesized by the method for calcining-ball milling Material.The traditional treatment method of sludge mainly includes burning, landfill etc., and these methods are not often thorough there is handling, and can cause Secondary pollution.It is relatively expensive and traditional lithium cell negative pole material synthetic method needs to use the industrial chemicals of high-purity, work Skill is cumbersome, yield is relatively low in building-up process in addition, is not suitable for industrialized production.Compared to the former, the invention has raw material Wide material sources, cost are low, building-up process is simple to operation, equipment is simple, can industrialized production the advantages that, can effectively solve Pollution of the sludge to environment, realize the purpose of waste reclamation.
【Brief description of the drawings】
Fig. 1 is the scanning electron microscope (SEM) photograph for preparing product；
Fig. 2 is the XRD for preparing product；
Fig. 3 is the cycle performance figure for preparing product.
【Embodiment】
It is further described with reference to the accompanying drawings and examples and prepares the method for lithium ion battery, product using sludge The sign of microstructure and performance.
Embodiment 1：
1) wet mud is dried 1 hour at 120 DEG C；
2) sludge of drying is calcined 2 hours at 400 DEG C；
3) by burnt sludge and graphite according to 16:1 mass ratio mixing, ball milling 5 hours；
4) product that ball milling is crossed is prepared into lithium ion battery as electrode material and tests its performance.
Embodiment 2：
1) wet mud is dried 2 hours at 120 DEG C；
2) sludge of drying is calcined 6 hours at 400 DEG C；
3) by burnt sludge and graphite according to 16:1 mass ratio mixing, ball milling 5 hours；
4) product that ball milling is crossed is prepared into lithium ion battery as electrode material and tests its performance.
Embodiment 3：
1) wet mud is dried 1 hour at 120 DEG C；
2) sludge of drying is calcined 4 hours at 500 DEG C；
3) by burnt sludge and graphite according to 16:1 mass ratio mixing, ball milling 5 hours；
4) product that ball milling is crossed is prepared into lithium ion battery as electrode material and tests its performance.
Embodiment 4：
1) wet mud is dried 2 hours at 120 DEG C；
2) sludge of drying is calcined 2 hours at 600 DEG C；
3) by burnt sludge and graphite according to 16:1 mass ratio mixing, ball milling 5 hours；
4) product that ball milling is crossed is prepared into lithium ion battery as electrode material and tests its performance.
Embodiment 5：
1) wet mud is dried 1 hour at 120 DEG C；
2) sludge of drying is calcined 5 hours at 500 DEG C；
3) by burnt sludge and graphite according to 16:3 mass ratio mixing, ball milling 5 hours；
4) product that ball milling is crossed is prepared into lithium ion battery as electrode material and tests its performance.
The test result of the present embodiment is as illustrated, Fig. 1 is sweeping using the lithium ion battery electrode material of sludge preparation Electron microscope picture is retouched, wherein obtained material is particle of the diameter in 300~500nm.Fig. 2 is the XRD after sludge calcining Figure, the product as can be seen from the figure prepared is silica.Fig. 3 is the current density of the electrode material prepared in 1A/g Under cycle performance figure, the material as can be seen from the figure prepared has good cycle performance.
The technological thought of above content only to illustrate the invention, it is impossible to protection scope of the present invention is limited with this, it is every to press According to technological thought proposed by the present invention, any change done on the basis of technical scheme, claims of the present invention is each fallen within Protection domain within.

Claims (7)

  1. A kind of 1. method for the electrode material that lithium ion battery is prepared using sludge, it is characterised in that comprise the following steps：
    1) wet mud is dried；
    2) sludge of drying is calcined into 2~6h at a temperature of 400~600 DEG C；
    3) after burnt sludge is mixed with graphite, abundant ball milling, the electrode material for preparing lithium ion battery is obtained.
  2. 2. the method for the electrode material according to claim 1 that lithium ion battery is prepared using sludge, it is characterised in that step It is rapid 1) in, wet mud is carried out at 120 DEG C, drying time 1-2h.
  3. 3. the method for the electrode material according to claim 1 that lithium ion battery is prepared using sludge, it is characterised in that step It is rapid 2) in, calcination atmosphere is air or argon gas.
  4. 4. the method for the electrode material according to claim 1 that lithium ion battery is prepared using sludge, it is characterised in that dirty Mud is with graphite according to 20:The mass ratio mixing of (1~5).
  5. 5. the method for the electrode material that lithium ion battery is prepared using sludge according to claim 1 or 4, its feature are existed In Ball-milling Time is 5~15h.
  6. 6. a kind of electrode material prepared using claim 1-5 any one methods described, it is characterised in that electrode material is Granular silica, a diameter of 300~500nm.
  7. 7. application of claim 6 electrode material in lithium ion battery is prepared.
CN201710613715.8A 2017-07-25 2017-07-25 A kind of electrode material that lithium ion battery is prepared using sludge and its preparation method and application Pending CN107394162A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110311145A (en) * 2019-07-01 2019-10-08 江苏乾景新能源产业技术研究院有限公司 A method of fuel-cell catalyst is prepared using sludge

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106058190A (en) * 2016-07-19 2016-10-26 天津师范大学 Preparation method for high-capacity anode material for lithium ion battery
CN106207161A (en) * 2015-05-06 2016-12-07 南开大学 Negative material and preparation method and with the lithium rechargeable battery of this negative material
CN106920966A (en) * 2017-04-12 2017-07-04 同济大学 A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106207161A (en) * 2015-05-06 2016-12-07 南开大学 Negative material and preparation method and with the lithium rechargeable battery of this negative material
CN106058190A (en) * 2016-07-19 2016-10-26 天津师范大学 Preparation method for high-capacity anode material for lithium ion battery
CN106920966A (en) * 2017-04-12 2017-07-04 同济大学 A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
邹金龙: "《污泥的材料化利用技术与原理 第1版》", 31 May 2015 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110311145A (en) * 2019-07-01 2019-10-08 江苏乾景新能源产业技术研究院有限公司 A method of fuel-cell catalyst is prepared using sludge
CN110311145B (en) * 2019-07-01 2021-06-18 江苏乾景新能源产业技术研究院有限公司 Method for preparing fuel cell catalyst by adopting sludge

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