CN106848242A - A kind of organic lithium storage materials of high power capacity and its application - Google Patents

A kind of organic lithium storage materials of high power capacity and its application Download PDF

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Publication number
CN106848242A
CN106848242A CN201710106184.3A CN201710106184A CN106848242A CN 106848242 A CN106848242 A CN 106848242A CN 201710106184 A CN201710106184 A CN 201710106184A CN 106848242 A CN106848242 A CN 106848242A
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storage materials
power capacity
lithium storage
organic
organic lithium
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CN106848242B (en
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王艳
郑洪河
曲群婷
吴永德
朱国斌
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Suzhou Huaying New Energy Materials Technology Co.,Ltd.
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Suzhou University
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/364Composites as mixtures
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/60Selection of substances as active materials, active masses, active liquids of organic compounds
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The present invention relates to a kind of organic lithium storage materials of high power capacity, it is selected from one or more mixture of composition in organic acid and its salt with butene dioic acid conjugation bond structure.From one or more mixture of composition in organic acid and its salt with butene dioic acid conjugation bond structure, storage lithium so can be carried out using conversion of the conjugated double bond on molecule space, lithium ion may be stored not only on carboxylic group, it is also possible to change by the chemical bond in carboxyl site, reversibly forms Li2O is stored among electrode micropore;The activity storage lithium site of this material is more, and a molecule with butene dioic acid structure can store 8 ~ 12 lithium ions.

Description

A kind of organic lithium storage materials of high power capacity and its application
Technical field
The invention belongs to battery or electrode material for super capacitor field, it is related to a kind of lithium storage materials, and in particular to a kind of High power capacity, high power and long-life organic lithium storage materials and its application.
Background technology
With the development of power vehicle and scale energy storage technology, high power capacity, high power and long-life batteries and capacitor Have become most promising chemical energy storage power supply.Active material is lithium ion battery, sodium-ion battery, ultracapacitor Deng the key and core of chemical energy storage device.Traditional inorganic lithium storage materials a lot, and are widely used, so And, inorganic lithium storage materials are limited by factors such as stoichiometric proportions, and lithium storage content is limited;Moreover, inorganic lithium storage materials The fragility of itself is big, and obvious bulk effect is enough to cause the structure and surface hair of material during Lithium-ion embeding and abjection Raw to change, silicium cathode and metal oxide negative material are particularly evident, and these all largely govern inorganic storage lithium material The further development and scale application of material.By contrast, organic material has elasticity and pliability well, storage lithium process Bulk effect is small, and is the one of development high specific energy of future generation, long-life batteries and capacitor with green and reproducible feature Individual important development direction.
Organic lithium storage materials and the electrochmical power source based on this kind of material have environment-friendly, renewable, processability good With the low feature of price, people are caused in recent years and is more and more paid close attention to.However, so far, organic lithium storage materials are mostly Show that lithium storage content is low, high-rate charge-discharge capability difference and the short property of cycle life, such as, pyrene -4,5,9,10 tetrones are only There is the specific capacity of 275mAh/g, and capacity is reduced to 120mAh/g after 20 circulations;Naphthoquinones has the specific capacity of 190mAh/g, Capability retention after 100 circulations is less than 40%;Anthraquinone has the specific capacity of 250mAh/g, capacity reduction after 100 circulations To 30mAh/g;2- vinyl -4,8- dihydrobenzos-[1,2-b:4,5-b ']-Dithiophene -4,8- diketone organic materials have The specific capacity of 225mAh/g, capacity is reduced to 50mAh/g after 25 circulations.Above-mentioned organic lithium storage materials cycle performance difference it is main Reason is relevant with its dissolubility in organic carbonate ester solvent, and it is that electrode capacity declines rapidly that dissolving causes the loss of active material The major reason moved back, in order to solve this problem, people improve the molecular weight of material by means such as molecule aggregation, grafting, with Phase reduces its dissolubility in organic solvent, but organic molecule polymerization can cause its avtive spot to reduce even disappearance, The molecular weight of material is greatly increased simultaneously, thus causes the further decline of the specific capacity of material.Moreover, organic storage lithium material Material is poor due to the poorly conductive of itself, the high-rate charge-discharge capability of material, and the charge-discharge magnification of many experimental studies all can only It is confined between 0.1~1C, the requirement apart from industry application differs greatly.As can be seen here, lithium storage content is low, high rate performance and follow Ring poor performance is the key and bottleneck of the further development of the organic lithium storage materials of restriction and scale application.
The content of the invention
The invention aims to overcome the deficiencies in the prior art and to provide a kind of high power capacity, high power and long-life organic Lithium storage materials.
To reach above-mentioned purpose, the technical solution adopted by the present invention is:A kind of organic lithium storage materials of high power capacity, it be selected from One or more mixture of composition in organic acid and its salt with butene dioic acid conjugation bond structure.
Optimally, the organic acid includes maleic acid and fumaric acid, and the acylate includes maleic acid lithium, maleic acid Sodium, maleic acid iron, maleic acid cobalt, maleic acid aluminium, maleic acid nickel, maleic acid copper, calcium maleate, fumaric acid lithium, fumaric acid sodium, richness Horse acid iron, fumaric acid cobalt, fumaric acid aluminium, fumaric acid nickel, fumaric acid copper and calcium fumarate.Rear shape more preferably compound with cation Into the organic composite salt being almost not dissolved in organic carbonate solvent, such as maleic acid cobalt, fumaric acid nickel, fumaric acid aluminium.
A further object of the present invention is to provide a kind of application of the above-mentioned organic lithium storage materials of high power capacity, and it is used as electrode Active material.
Optimally, the preparation of the electrode is comprised the following steps:
A the organic lithium storage materials of the high power capacity and binding agent, conductive agent are carried out being mixed and made into electrode by () in dispersant Slurry;The mass ratio of the organic lithium storage materials of high power capacity, binding agent and conductive agent is 4~6:3~5:1;
B be coated with the electrode slurry on a current collector by (), suppressed after drying, cut, further drying.
Further, the binding agent is selected from Kynoar, sodium carboxymethylcellulose, Sodium Polyacrylate and alginic acid One or more mixture of composition in sodium;The conductive agent is in acetylene black, conductive carbon black, Graphene and CNT One or more mixture of composition;The dispersant is 1-METHYLPYRROLIDONE, N,N-dimethylformamide or water.
Further, in step (b), the pressure of the compacting is 1~3MPa/cm2
Further, in step (b), the temperature of the drying is 100~170 DEG C.
Optimally, the electrode can be used for the electrochemical devices such as lithium ion battery, sodium-ion battery or ultracapacitor.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art:High power capacity of the present invention has Machine lithium storage materials, from one or more mixing of composition in organic acid and its salt with butene dioic acid conjugation bond structure Thing, so can carry out storage lithium using conversion of the conjugated double bond on molecule space, and lithium ion may be stored not only in carboxyl base In group, it is also possible to changed by the chemical bond in carboxyl site, reversibly form Li2O is stored among electrode micropore;This material Activity storage lithium site it is many, a molecule with butene dioic acid structure can store 8~12 lithium ions.After tested, material Reversible lithium storage capacity be up to more than 1500mAh/g, the level than current material less than 300mAh/g improves 4~5 times, realizes The technical field significant technological break-through.The dissolubility of this kind of organic acid and its slaine in carbonate solvent is small, especially It is the organic composite salt formed after compound by bivalent cation, is not almost dissolved in organic carbonate ester solvent;It is prior It is, this organic lithium storage materials elastic properties of materials and good toughness, almost without obvious volume during Lithium-ion embeding and abjection Effect, therefore, material has excellent electrochemical cycle stability, circulates 500 times without obvious capacity attenuation;Optimization electrode group Cheng Hou, reversible capacity of the material under the conditions of 100C breaches traditional 0.1~1C multiplying powers limitation still above 570mAh/g, It is a kind of organic lithium storage materials with high power nature.This organic lithium storage materials have reproducible feature, abundance, Price is low, it is significant that the cost and cost of electrochmical power source will be reduced to future, is the following high specific energy of development, high power, longevity The important selection of life and low cost electrochmical power source.
Brief description of the drawings
Accompanying drawing 1 is the SEM figures of maleic acid electrode slice in embodiment 1;
Accompanying drawing 2 is first three impulse electricity curve of maleic acid electrode in embodiment 1;
Accompanying drawing 3 is the rate charge-discharge property of maleic acid electrode in experimental example 1.
Accompanying drawing 4 is the long-term cycle performance of maleic acid electrode in experimental example 1.
Accompanying drawing 5 is the Li1S Strength Changes of maleic acid electrode XPS figures under different charging and discharging states in experimental example 1.
Specific embodiment
The organic lithium storage materials of high power capacity of the present invention, it is selected from the organic acid and its salt that bond structure is conjugated with butene dioic acid In one or more composition mixture;Wherein organic acid include maleic acid and fumaric acid, acylate include maleic acid lithium, Sodium maleate, maleic acid iron, maleic acid cobalt, maleic acid aluminium, maleic acid nickel, maleic acid copper, calcium maleate, fumaric acid lithium, rich horse Sour sodium, ferrous fumarate, fumaric acid cobalt, fumaric acid aluminium, fumaric acid nickel, fumaric acid copper and calcium fumarate.So can be using conjugation Conversion of the double bond on molecule space carries out storage lithium, and lithium ion may be stored not only on carboxylic group, it is also possible to by carboxyl The chemical bond change in site, reversibly forms Li2O is stored among electrode micropore;The activity storage lithium site of this material is more, and one The individual molecule with butene dioic acid structure can store 8~12 lithium ions.After tested, the reversible lithium storage capacity of material is up to More than 1500mAh/g, the level than current material less than 300mAh/g improves 4~5 times, realizes the technical field significant Technological break-through.The dissolubility of this kind of organic acid and its slaine in carbonate solvent is small, rear shape particularly compound with cation Into the organic composite salt (such as maleic acid cobalt, fumaric acid nickel, fumaric acid aluminium) being almost not dissolved in organic carbonate solvent;More Importantly, almost without obvious during this organic lithium storage materials elastic properties of materials and good toughness, Lithium-ion embeding and abjection Bulk effect, therefore, material has an excellent electrochemical cycle stability, and circulation 500 times is without obvious capacity attenuation;Optimization After electrode composition, reversible capacity of the material under the conditions of 100C breaches traditional 0.1~1C multiplying powers still above 570mAh/g Limitation, is a kind of organic lithium storage materials with high power nature.This organic lithium storage materials have reproducible feature, source Abundant, price is low, it is significant that the cost and cost of electrochmical power source will be reduced to future, be the following high specific energy of development, high power, Long-life and the important selection of low cost electrochmical power source.
The application of the above-mentioned organic lithium storage materials of high power capacity, it is used as the active material of electrode, can be used for lithium ion battery, sodium The electrochemical device such as ion battery or ultracapacitor.Specific preparation comprises the following steps:A () is by the organic storage lithium of the high power capacity Material carries out being mixed and made into electrode slurry with binding agent, conductive agent in dispersant;The organic lithium storage materials of high power capacity, bonding The mass ratio of agent and conductive agent is 4~6:3~5:1;B be coated with the electrode slurry on a current collector by (), carried out after drying Compacting, cutting, further drying.Thickness of electrode after drying is about 10 μm.The binding agent be selected from Kynoar, One or more mixture of composition in sodium carboxymethylcellulose (CMC), Sodium Polyacrylate (PAANa) and sodium alginate;Institute It is one or more mixture of composition in acetylene black, conductive carbon black, Graphene and CNT to state conductive agent;The dispersion Agent is 1-METHYLPYRROLIDONE, N,N-dimethylformamide or water.The pressure of the compacting is 1~3MPa/cm2.The drying Temperature be 100~170 DEG C.
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
Embodiment 1 provides a kind of application of the organic lithium storage materials of high power capacity, for making electrode of lithium cell, specially:
(a) by 5g maleic acids and 1g PVDF (commercially available), 4g acetylene blacks (commercially available) 20g 1-METHYLPYRROLIDONEs (NMP, It is commercially available) in be sufficiently mixed and be uniformly made electrode slurry;
B be coated on electrode slurry in copper foil current collector (commercially available) by (), 2MPa/cm is used after drying2Pressure pressed System, 10h is dried after cutting under 140 DEG C, vacuum condition;
The SEM figures of obtained maleic acid electrode slice are as shown in Figure 1, it can be seen that maleic acid bead and acetylene black conductor It is uniformly dispersed, and about 10 μm of thickness of electrode.
By prepared maleic acid electrode, according to existing battery production method:Using lithium metal as to electrode assembling into battery Charge-discharge test is carried out, its result is as shown in Figures 2 to 4.As seen from Figure 2, reversible capacity exceedes electrode first 1300mAh/g, the reversible capacity stabilization of electrode is in more than 1500mAh/g after 5 times circulate.The multiplying power of the electrode charge and times Rate discharge characteristics are shown in Fig. 3, it can be seen that this material not only has very excellent high-multiplying power discharge property, in 100C conditions Under the still reversible capacity with 570mAh/g, and with especially excellent high magnification charging quantity, (can be corresponded in 100C Charged under the conditions of super-large current 46.2A/g), and electrode will not be damaged, this property is all inorganic lithium storage materials Incomparable, show intentional power nature.By after 500 charge and discharge cycles, the capacity of electrode is not almost any Decay shows that this material has very excellent long-term charge and discharge cycles property (see Fig. 4).Fig. 5 is maleic acid electrode not With the Li1S Strength Changes of XPS figures under charging and discharging state, it can be seen that with the increase of electrode lithium-inserting amount, the intensity at Li1S peaks Gradually strengthen, the intensity at Li1S peaks is gradually reduced during de- lithium, illustrate that this material can be carried out by chemical bond change can Inverse embedding de- lithium, is a kind of high power capacity, high power and long-life organic lithium storage materials.
Embodiment 2-12
Embodiment 2-12 provides a kind of application of the organic lithium storage materials of high power capacity respectively, and it differs only in organic storage lithium material The species and quality of material, binding agent, conductive agent and dispersant, are specifically shown in Table 1;Electrode obtained in wherein insoluble ferrous fumarate Reversible capacity is lower slightly first, it may be possible to the reason for its electrochemical properties is more active.
The formula rate table of the organic lithium storage materials application of high power capacity in the embodiment 2-12 of table 1
The above embodiments merely illustrate the technical concept and features of the present invention, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention, all according to the present invention The equivalent change or modification that Spirit Essence is made, should all be included within the scope of the present invention.

Claims (8)

1. organic lithium storage materials of a kind of high power capacity, it is characterised in that:It is selected from the organic of butene dioic acid conjugation bond structure One or more mixture of composition in acid and its salt.
2. organic lithium storage materials of high power capacity according to claim 1, it is characterised in that:The organic acid include maleic acid and Fumaric acid, the acylate include maleic acid lithium, sodium maleate, maleic acid iron, maleic acid cobalt, maleic acid aluminium, maleic acid nickel, Maleic acid copper, calcium maleate, fumaric acid lithium, fumaric acid sodium, ferrous fumarate, fumaric acid cobalt, fumaric acid aluminium, fumaric acid nickel, rich horse Sour copper and calcium fumarate.
3. in claim 1 to 2 any organic lithium storage materials of high power capacity application, it is characterised in that:It is used as electrode Active material.
4. the application of the organic lithium storage materials of high power capacity according to claim 3, it is characterised in that the preparation of the electrode includes Following steps:
(a)The organic lithium storage materials of the high power capacity and binding agent, conductive agent are carried out being mixed and made into electrode slurry in dispersant; The mass ratio of the organic lithium storage materials of high power capacity, binding agent and conductive agent is 4 ~ 6:3~5:1;
(b)By electrode slurry coating on a current collector, suppressed after drying, cut, further drying.
5. the application of the organic lithium storage materials of high power capacity according to claim 4, it is characterised in that:The binding agent is selected from poly- One or more mixture of composition in vinylidene, sodium carboxymethylcellulose, Sodium Polyacrylate and sodium alginate;It is described to lead Electric agent is one or more mixture of composition in acetylene black, conductive carbon black, Graphene and CNT;The dispersant is 1-METHYLPYRROLIDONE, N,N-dimethylformamide or water.
6. the application of the organic lithium storage materials of high power capacity according to claim 4, it is characterised in that:Step(b)In, the compacting Pressure be 1 ~ 3 MPa/cm2
7. the application of the organic lithium storage materials of high power capacity according to claim 4, it is characterised in that:Step(b)In, the drying Temperature be 100 ~ 170 DEG C.
8. the application of the organic lithium storage materials of high power capacity according to claim 3, it is characterised in that:The electrode is used for lithium ion Battery, sodium-ion battery or ultracapacitor.
CN201710106184.3A 2017-02-27 2017-02-27 Application of high-capacity organic lithium storage material Active CN106848242B (en)

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CN102290562A (en) * 2010-06-21 2011-12-21 三星Sdi株式会社 Lithium battery and method of manufacturing same
CN105958011A (en) * 2011-06-29 2016-09-21 日东电工株式会社 Nonaqueous-electrolyte secondary battery and positive-electrode sheet therefor
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