CN109088063A - A kind of lithium ion battery material and preparation method thereof - Google Patents

A kind of lithium ion battery material and preparation method thereof Download PDF

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Publication number
CN109088063A
CN109088063A CN201810926167.9A CN201810926167A CN109088063A CN 109088063 A CN109088063 A CN 109088063A CN 201810926167 A CN201810926167 A CN 201810926167A CN 109088063 A CN109088063 A CN 109088063A
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added
ion battery
lithium ion
nano
dispersion fluid
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崔晓迪
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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
    • 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
    • H01M4/58—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a kind of lithium ion battery materials, it is composed of the following raw materials by weight: lithium hydroxide 50-80, ferrous ammonium phosphate 80-100, 2- mercapto benzimidazole 1-2, nano dispersion fluid 30-40, thiophene 15-20, dibenzoyl peroxide 0.3-0.4, the present invention uses phosphorus trichloride mixed with nano-silicon dioxide first, again with triethanolamine blending reaction, effectively improve the surface-active of silica, the present invention is using thiophene as monomer, using nano dispersion fluid as reaction dissolvent, pass through polymerization, realize effective combination of nano silica and polythiophene, to improve sintering stability, improve the electric conductivity of finished-product material.

Description

A kind of lithium ion battery material and preparation method thereof
Technical field
The invention belongs to battery material fields, and in particular to a kind of lithium ion battery material and preparation method thereof.
Background technique
Lithium-ion-power cell is generally acknowledged most potential on-vehicle battery both at home and abroad at present, mainly by positive electrode, negative The part such as pole material, diaphragm, electrolyte forms；Wherein, positive electrode is the important component of lithium ion battery, and is determined The key factor of performance of lithium ion battery；Therefore, from the aspect of resource, environmental protection and security performance, lithium ion battery is found Ideal electrode active material is still international energy material worker primary problem to be solved；
Current commercialized anode material for lithium-ion batteries mainly has cobalt acid lithium, LiMn2O4
And LiFePO4；Cobalt acid lithium is the positive electrode for being now widely used for small-scale lithium ion cell, but since cobalt is toxic, money Source reserves are limited expensive, and the battery security that assembles as positive electrode of cobalt acid lithium material and thermal stability are bad, Oxygen can be generated under high temperature, can not meet the technical requirements of power battery；LiMn2O4 is although cheap, environmentally friendly, safety, multiplying power It performance and has a safety feature, but its theoretical capacity is not high, it is poor to be recycled performance, thermal stability and high-temperature behavior, is answering Greatest problem in is that cycle performance is bad, especially under high temperature, when Manganic ion and big multiplying power discharging in material The divalent manganesetion that particle surface is formed finally destroys the structure of LiMn2O4 so that the dissolution of material in the electrolytic solution is obvious, Also reduce the cycle performance of material；
Therefore, find that a kind of conductive stability is good, hair of the superior lithium-ion-power cell material of comprehensive performance for modernization It opens up particularly significant.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of lithium ion battery material and its systems Preparation Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of lithium ion battery material, it is composed of the following raw materials by weight:
Lithium hydroxide 50-80, ferrous ammonium phosphate 80-100,2- mercapto benzimidazole 1-2, nano dispersion fluid 30-40, thiophene 15-20, dibenzoyl peroxide 0.3-0.4.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano silica 10-17, phosphorus trichloride 3-4, triethanolamine 2-5, Sucrose acetoisobutyrate 0.1-0.2.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) phosphorus trichloride is taken, is added in the deionized water of 50-67 times of its weight, stirs evenly, nano silica is added, Increasing temperature is 55-60 DEG C, insulated and stirred 20-30 minutes, Sucrose acetoisobutyrate is added, stirs evenly, obtains ester solution；
(2) triethanolamine is taken, is added in above-mentioned ester solution, insulated and stirred 1-2 hours at 90-96 DEG C, is cooled to room temperature, i.e., Obtain the nano dispersion fluid.
A kind of preparation method of lithium ion battery material, comprising the following steps:
(1) dibenzoyl peroxide is taken, is added in the dehydrated alcohol of 10-14 times of its weight, stirs evenly, it is molten to obtain initiator Liquid；
(2) 2- mercapto benzimidazole, thiophene mixing are taken, is added in above-mentioned nano dispersion fluid, stirs evenly, be sent to reaction In kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and above-mentioned initiator solution is added, insulated and stirred 3-4 hours, discharges It is cooling, obtain polymer solution；
(3) lithium hydroxide, ferrous ammonium phosphate mixing are taken, is added in above-mentioned polymer solution, stirs evenly, be sent into sintering furnace In, it is passed through inert gas, is calcined 10-20 hours at 600-750 DEG C, discharging is cooling to get the lithium ion battery material.
Advantages of the present invention:
The present invention uses phosphorus trichloride mixed with nano-silicon dioxide first, then with triethanolamine blending reaction, effectively improve The surface-active of silica, the present invention is using thiophene as monomer, using nano dispersion fluid as reaction dissolvent, by polymerization, realizes Effective combination of nano silica and polythiophene improves the electric conductivity of finished-product material to improve sintering stability, It is strong as the electrode material electric conductivity height of lithium ion battery, stability, effectively improve the recyclable number of lithium ion battery.
Specific embodiment
Embodiment 1
A kind of lithium ion battery material, it is composed of the following raw materials by weight:
Lithium hydroxide 80, ferrous ammonium phosphate 100,2- mercapto benzimidazole 2, nano dispersion fluid 40, thiophene 20, diphenyl peroxide Formyl 0.4.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano silica 17, phosphorus trichloride 4, triethanolamine 5, Sucrose acetoisobutyrate 0.2.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) phosphorus trichloride is taken, is added in the deionized water of 67 times of its weight, stirs evenly, nano silica is added, is increased Temperature is 60 DEG C, insulated and stirred 30 minutes, Sucrose acetoisobutyrate is added, stirs evenly, obtains ester solution；
(2) triethanolamine is taken, is added in above-mentioned ester solution, insulated and stirred 2 hours at 96 DEG C are cooled to room temperature to get institute State nano dispersion fluid.
A kind of preparation method of lithium ion battery material, comprising the following steps:
(1) dibenzoyl peroxide is taken, is added in the dehydrated alcohol of 14 times of its weight, is stirred evenly, obtain initiator solution；
(2) 2- mercapto benzimidazole, thiophene mixing are taken, is added in above-mentioned nano dispersion fluid, stirs evenly, be sent to reaction In kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, and above-mentioned initiator solution is added, and insulated and stirred 4 hours, discharging cooled down, Obtain polymer solution；
(3) lithium hydroxide, ferrous ammonium phosphate mixing are taken, is added in above-mentioned polymer solution, stirs evenly, be sent into sintering furnace In, it is passed through inert gas, is calcined 20 hours at 750 DEG C, discharging is cooling to get the lithium ion battery material.
Embodiment 2
A kind of lithium ion battery material, it is composed of the following raw materials by weight:
Lithium hydroxide 50, ferrous ammonium phosphate 80,2- mercapto benzimidazole 1, nano dispersion fluid 30, thiophene 15, diphenyl peroxide Formyl 0.3.
The nano dispersion fluid is made of the raw material of following weight parts:
Nano silica 10, phosphorus trichloride 3, triethanolamine 2, Sucrose acetoisobutyrate 0.1.
The preparation method of the nano dispersion fluid, comprising the following steps:
(1) phosphorus trichloride is taken, is added in the deionized water of 50 times of its weight, stirs evenly, nano silica is added, is increased Temperature is 55 DEG C, insulated and stirred 20 minutes, Sucrose acetoisobutyrate is added, stirs evenly, obtains ester solution；
(2) triethanolamine is taken, is added in above-mentioned ester solution, insulated and stirred 1 hour at 90 DEG C is cooled to room temperature to get institute State nano dispersion fluid.
A kind of preparation method of lithium ion battery material, comprising the following steps:
(1) dibenzoyl peroxide is taken, is added in the dehydrated alcohol of 10 times of its weight, is stirred evenly, obtain initiator solution；
(2) 2- mercapto benzimidazole, thiophene mixing are taken, is added in above-mentioned nano dispersion fluid, stirs evenly, be sent to reaction In kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C, and above-mentioned initiator solution is added, and insulated and stirred 3 hours, discharging cooled down, Obtain polymer solution；
(3) lithium hydroxide, ferrous ammonium phosphate mixing are taken, is added in above-mentioned polymer solution, stirs evenly, be sent into sintering furnace In, it is passed through inert gas, is calcined 10 hours at 600 DEG C, discharging is cooling to get the lithium ion battery material.
Performance test:
The lithium ion battery material of embodiment 1；
Apparent density: 1.28 g/cm3；
Tap density: 2.35g/cm3；
Specific capacity (25 DEG C, 1C, vs li, mAh/g) 131.1；
Specific capacity (60 DEG C, 1C, vs li, mAh/g) 131.9.
The lithium ion battery material of embodiment 2；
Apparent density: 1.31 g/cm3；
Tap density: 2.41g/cm3；
Specific capacity (25 DEG C, 1C, vs li, mAh/g) 134.0；
Specific capacity (60 DEG C, 1C, vs li, mAh/g) 133.8.

Claims (3)

1. a kind of lithium ion battery material is made of the raw material of following weight parts:
Lithium hydroxide 50-80, ferrous ammonium phosphate 80-100,2- mercapto benzimidazole 1-2, nano dispersion fluid 30-40, thiophene 15-20, dibenzoyl peroxide 0.3-0.4, which is characterized in that the nano dispersion fluid is the raw material group by following weight parts At: nano silica 10-17, phosphorus trichloride 3-4, triethanolamine 2-5, Sucrose acetoisobutyrate 0.1-0.2.
2. a kind of lithium ion battery material according to claim 1, which is characterized in that the preparation of the nano dispersion fluid Method, comprising the following steps:
(1) phosphorus trichloride is taken, is added in the deionized water of 50-67 times of its weight, stirs evenly, nano silica is added, Increasing temperature is 55-60 DEG C, insulated and stirred 20-30 minutes, Sucrose acetoisobutyrate is added, stirs evenly, obtains ester solution；
(2) triethanolamine is taken, is added in above-mentioned ester solution, insulated and stirred 1-2 hours at 90-96 DEG C, is cooled to room temperature, i.e., Obtain the nano dispersion fluid.
3. a kind of preparation method of lithium ion battery material as described in claim 1, which comprises the following steps:
(1) dibenzoyl peroxide is taken, is added in the dehydrated alcohol of 10-14 times of its weight, stirs evenly, it is molten to obtain initiator Liquid；
(2) 2- mercapto benzimidazole, thiophene mixing are taken, is added in above-mentioned nano dispersion fluid, stirs evenly, be sent to reaction In kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and above-mentioned initiator solution is added, insulated and stirred 3-4 hours, discharges It is cooling, obtain polymer solution；
(3) lithium hydroxide, ferrous ammonium phosphate mixing are taken, is added in above-mentioned polymer solution, stirs evenly, be sent into sintering furnace In, it is passed through inert gas, is calcined 10-20 hours at 600-750 DEG C, discharging is cooling to get the lithium ion battery material.
CN201810926167.9A 2018-08-15 2018-08-15 A kind of lithium ion battery material and preparation method thereof Pending CN109088063A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112290023A (en) * 2020-10-21 2021-01-29 安徽清泉新能源科技集团有限责任公司 Polypyrrole-doped power battery material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1821065A (en) * 2006-03-20 2006-08-23 清华大学 Process for preparing high density spherical lithium ferric phosphate
CN101475157A (en) * 2009-01-21 2009-07-08 武汉大学 Preparation of lithium iron phosphate nano composite microsphere
CN108250437A (en) * 2018-01-23 2018-07-06 宿州市微腾知识产权运营有限公司 A kind of preparation method of Polypyrrole Conducting Materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1821065A (en) * 2006-03-20 2006-08-23 清华大学 Process for preparing high density spherical lithium ferric phosphate
CN101475157A (en) * 2009-01-21 2009-07-08 武汉大学 Preparation of lithium iron phosphate nano composite microsphere
CN108250437A (en) * 2018-01-23 2018-07-06 宿州市微腾知识产权运营有限公司 A kind of preparation method of Polypyrrole Conducting Materials

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112290023A (en) * 2020-10-21 2021-01-29 安徽清泉新能源科技集团有限责任公司 Polypyrrole-doped power battery material and preparation method thereof

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