CN106654263A - Preparation method of Prussian blue based sodium ion battery positive electrode material - Google Patents

Preparation method of Prussian blue based sodium ion battery positive electrode material Download PDF

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Publication number
CN106654263A
CN106654263A CN201611255163.XA CN201611255163A CN106654263A CN 106654263 A CN106654263 A CN 106654263A CN 201611255163 A CN201611255163 A CN 201611255163A CN 106654263 A CN106654263 A CN 106654263A
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Prior art keywords
prussian blue
sodium
ion battery
battery positive
ferrox
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CN201611255163.XA
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Chinese (zh)
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王海燕
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东莞市佳乾新材料科技有限公司
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Priority to CN201611255163.XA priority Critical patent/CN106654263A/en
Publication of CN106654263A publication Critical patent/CN106654263A/en

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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
    • H01M4/58Selection 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C3/00Cyanogen; Compounds thereof
    • C01C3/08Simple or complex cyanides of metals
    • C01C3/12Simple or complex iron cyanides
    • 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
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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 invention discloses a preparation method of a Prussian blue based sodium ion battery positive electrode material. The preparation method takes ferrous oxalate and sodium oxalate as raw materials, and makes the raw materials react with sodium ferrocyanide; a reaction speed can be slower and the production speed of a Prussian blue mono-crystal becomes slow, so that the aim of reducing defects in a Prussian blue crystal is realized. A sodium ion battery positive electrode prepared from the Prussian blue crystal can still keep good stability after being subjected to a plurality of times of charge-discharge cycles, and the service life is long. The method is simple in preparation process, easy to implement and suitable for large-scale production.

Description

A kind of preparation method of Prussian blue base sodium-ion battery positive material

Technical field

The present invention relates to field of batteries, more particularly to a kind of preparation side of Prussian blue base sodium-ion battery positive material Method.

Background technology

With the fast development of extensive intelligent grid, and the popularization and application of electric automobile, lithium resource cannot meet lithium The great demand of ion battery, the energy storage technology for developing alternative lithium ion battery is extremely necessary.Sodium reserves in the earth's crust are rich Richness, it is widely distributed, belong to congenerss with lithium, it is a kind of battery raw material of feasible replacement lithium.But sodium atom amount is bigger than lithium, Standard electrochemical potential is lower than lithium, and current sodium-ion battery energy density is also difficult to be compared favourably with lithium ion battery, and it is right to still need to Sodium-ion battery system is studied.

Sodium-ion battery is made up of positive pole, negative pole, electrolyte and barrier film etc.:The usual employing of positive and negative electrode material can be embedded in/ The active material of deintercalation sodium ion, electrolyte is then made up of sodium ion conducting salt and organic solvent.The active matter of positive and negative electrode material Matter is electrochemically reacted, and determines the fundamental characteristics of this electrode, is the core component of sodium-ion battery, and the performance of battery is played Important function.The at present research with regard to sodium ion positive electrode be concentrated mainly on transition metal oxide, polyanionic compound, Six cyanogen metallic compounds or organic-based material etc..Wherein Prussian blue (KFe [Fe (CN)6]) there is three-dimensional open architecture, have It is a kind of typical transition metal iron cyanide beneficial to the transmission and storage of alkali metal ion.It is Prussian blue in water system battery The electrochemical behavior of excellent K and Na is shown, its excellent chemical property shows good in large-scale energy storage device Good application prospect.

Chinese patent CN201510097071.2 discloses a kind of sodium-ion battery richness sodium positive electrode and preparation method thereof With a kind of sodium-ion battery, the method comprising the steps of:(1) under agitation, it is nickel salt solution, cobalt salt solution, manganese salt is molten Liquid, oxalate solution and sodium salt solution mixing, the condition of the mixing causes Ni2+, Co2+, Mn2+ and Na+ in mixed solution Total mole number is 0.8~1 with the ratio of the molal quantity of oxalate denominationby:1;(2) in a sealed meter environment, above-mentioned mixed solution is carried out Hydro-thermal reaction, then cooled down, solid-liquid separation, washing, drying, obtain presoma;(3) presoma is forged under air atmosphere Burn, obtain sodium-ion battery richness sodium positive electrode.The sodium-ion battery richness sodium positive electrode that the inventive method is prepared can The high power capacity discharge and recharge of sodium-ion battery is realized, and makes sodium-ion battery that there is excellent cyclical stability.

The content of the invention

It is an object of the invention to provide a kind of preparation method of Prussian blue base sodium-ion battery positive material, party's legal system Standby Prussian blue defect is little, good cycling stability, so as to the positive electrode capacity dimension for preparing holds efficiency high, long service life.

For achieving the above object, the present invention is employed the following technical solutions:

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 120- The speed stirring of 300rpm, after completion of dropping, continues to stir 36-48h, and blue precipitate is obtained, by its deionized water centrifugation After cleaning repeatedly, using absolute ethanol washing 2-3 time, afterwards evacuation is dried, prepared Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 200-450rpm rotational speeds, after obtained powder is dried, is scattered in dehydrated alcohol In, after Deca binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

Preferably, the use mol ratio of the Ferrox. and Disodium oxalate. is 1-2:1;Ferrox. and surfactant Use quality amount is than position 1.5-2:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.2-2.5.

Preferably, the surfactant is P123, fatty alcohol-polyoxyethylene ether, sodium stearoyl lactate or dodecyl sulfur One kind in sour sodium.

Preferably, the ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, and 1mm's waits mass mixing thing.

Preferably, the process of lapping persistent period be 10-12h, during every half an hour convert direction of rotation.

Preferably, the conductive agent is the one kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.

Preferably, described adhesive is in polyvinylidene fluoride, polrvinyl chloride polyvinyl alcohol or Carboxymethyl cellulose sodium It is a kind of.

Preferably, in the step (2), the input amount of each component is Prussian blue 65-80 parts, conductive agent 15-25 parts, two Zirconium oxide abrasive ball 80-105 parts, binding agent 5-10 parts.

The invention has the advantages that, Ferrox. and Disodium oxalate. are adopted for raw material, react with sodium ferrocyanide, can So that response speed is slower so that the speed of production of Prussian blue monocrystalline is slack-off, so as to reduce Prussian blue crystal In defect purpose.The sodium-ion battery positive pole prepared by the Prussian blue crystal, remains to after multiple charge and discharge cycles Keep good stability, long service life.And the method preparation process is simple, easily with enforcement, it is adapted to large-scale production.

Specific embodiment

In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution The present invention is released, any restriction will not be constituted to the present invention.

Embodiment 1

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 120rpm's Speed stir, after completion of dropping, continue stir 36h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 2 times, afterwards evacuation is dried, and is obtained Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 200rpm rotational speeds, after obtained powder is dried, and in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

The use mol ratio of Ferrox. and Disodium oxalate. is 1:1;The use quality amount ratio of Ferrox. and surfactant Position 1.5:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.2.Surfactant is P123, fatty alcohol polyoxy second One kind in alkene ether, sodium stearoyl lactate or sodium lauryl sulphate.Ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, 1mm's waits mass mixing thing.The process of lapping persistent period be 10-12h, during every half an hour convert direction of rotation.It is conductive Agent is the one kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.Binding agent is polyvinylidene fluoride, polychlorostyrene second One kind in alkene polyvinyl alcohol or Carboxymethyl cellulose sodium.In step (2), the input amount of each component is Prussian blue 65 parts, is led 15 parts of electric agent, 80 parts of zirconium dioxide mill ball, 5 parts of binding agent.

Embodiment 2

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 300rpm's Speed stir, after completion of dropping, continue stir 48h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 3 times, afterwards evacuation is dried, and is obtained Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 450rpm rotational speeds, after obtained powder is dried, and in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

The use mol ratio of Ferrox. and Disodium oxalate. is 2:1;The use quality amount ratio of Ferrox. and surfactant Position 2:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.5.Surfactant is P123, aliphatic alcohol polyethenoxy One kind in ether, sodium stearoyl lactate or sodium lauryl sulphate.Ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, 1mm's waits mass mixing thing.The process of lapping persistent period be 12h, during every half an hour convert direction of rotation.Conductive agent is One kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.Binding agent is polyvinylidene fluoride, polrvinyl chloride gathers One kind in vinyl alcohol or Carboxymethyl cellulose sodium.In step (2), the input amount of each component is Prussian blue 80 parts, conductive agent 25 parts, 105 parts of zirconium dioxide mill ball, 10 parts of binding agent.

Embodiment 3

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 200rpm's Speed stir, after completion of dropping, continue stir 40h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 2 times, afterwards evacuation is dried, and is obtained Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 350rpm rotational speeds, after obtained powder is dried, and in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

The use mol ratio of Ferrox. and Disodium oxalate. is 1:1;The use quality amount ratio of Ferrox. and surfactant Position 2:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.4.Surfactant is P123, aliphatic alcohol polyethenoxy One kind in ether, sodium stearoyl lactate or sodium lauryl sulphate.Ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, 1mm's waits mass mixing thing.The process of lapping persistent period be 11h, during every half an hour convert direction of rotation.Conductive agent is One kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.Binding agent is polyvinylidene fluoride, polrvinyl chloride gathers One kind in vinyl alcohol or Carboxymethyl cellulose sodium.In step (2), the input amount of each component is Prussian blue 70 parts, conductive agent 20 parts, 90 parts of zirconium dioxide mill ball, 8 parts of binding agent.Embodiment 4

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 200rpm's Speed stir, after completion of dropping, continue stir 40h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 3 times, afterwards evacuation is dried, and is obtained Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 350rpm rotational speeds, after obtained powder is dried, and in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

The use mol ratio of Ferrox. and Disodium oxalate. is 2:1;The use quality amount ratio of Ferrox. and surfactant Position 1.5:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.2.Surfactant is P123, fatty alcohol polyoxy second One kind in alkene ether, sodium stearoyl lactate or sodium lauryl sulphate.Ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, 1mm's waits mass mixing thing.The process of lapping persistent period be 12h, during every half an hour convert direction of rotation.Conductive agent is One kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.Binding agent is polyvinylidene fluoride, polrvinyl chloride gathers One kind in vinyl alcohol or Carboxymethyl cellulose sodium.In step (2), the input amount of each component is Prussian blue 70 parts, conductive agent 22 parts, 95 parts of zirconium dioxide mill ball, 7 parts of binding agent.

Embodiment 5

A kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:

(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is equal It is even, and after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with 180rpm's Speed stir, after completion of dropping, continue stir 45h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 2 times, afterwards evacuation is dried, and is obtained Prussian blue;

(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionization Water, adds zirconium dioxide mill ball, with 350rpm rotational speeds, after obtained powder is dried, and in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.

The use mol ratio of Ferrox. and Disodium oxalate. is 1:1;The use quality amount ratio of Ferrox. and surfactant Position 1.8:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.4.Surfactant is P123, fatty alcohol polyoxy second One kind in alkene ether, sodium stearoyl lactate or sodium lauryl sulphate.Ball milling pearl is zirconium oxide spheroidal graphite pearl, and diameter is respectively 2mm, 1mm's waits mass mixing thing.The process of lapping persistent period be 12h, during every half an hour convert direction of rotation.Conductive agent is One kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.Binding agent is polyvinylidene fluoride, polrvinyl chloride gathers One kind in vinyl alcohol or Carboxymethyl cellulose sodium.In step (2), the input amount of each component is Prussian blue 65 parts, conductive agent 18 parts, 95 parts of zirconium dioxide mill ball, 6 parts of binding agent.

Claims (8)

1. a kind of preparation method of Prussian blue base sodium-ion battery positive material, comprises the following steps:
(1) by after Ferrox. and Disodium oxalate. mix homogeneously, in solution and water, surfactant is added, ultrasonic agitation is uniform, and And after froth breaking, be added dropwise to ferrocyanide sodium water solution wherein using peristaltic pump, at ambient temperature, with the speed of 120-300rpm Degree stirring, after completion of dropping, continue stir 36-48h, be obtained blue precipitate, by its deionized water eccentric cleaning it is multiple after, Using absolute ethanol washing 2-3 time, afterwards evacuation is dried, and is obtained Prussian blue;
(2) after by obtained Prussian blue, conductive agent mixing, it is placed in marble and grinds in tank, and is added thereto to deionized water, plus Enter zirconium dioxide mill ball, with 200-450rpm rotational speeds, after obtained powder is dried, in being scattered in dehydrated alcohol, drop Plus after binding agent mix homogeneously, vacuum drying, after tabletting, as described positive electrode.
2. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute The use mol ratio for stating Ferrox. and Disodium oxalate. is 1-2:1;The use quality amount of Ferrox. and surfactant compares position 1.5-2:1;Ferrox. is 1 with the mol ratio that sodium ferrocyanide is used:2.2-2.5.
3. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute Surfactant is stated for P123, fatty alcohol-polyoxyethylene ether, the one kind in sodium stearoyl lactate or sodium lauryl sulphate.
4. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute It is zirconium oxide spheroidal graphite pearl to state ball milling pearl, and diameter is respectively 2mm, and 1mm's waits mass mixing thing.
5. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute The process of lapping persistent period is stated for 10-12h, during convert direction of rotation every half an hour.
6. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute Conductive agent is stated for the one kind in acetylene black, CNT, carbon nano-fiber or expanded graphite.
7. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute Binding agent is stated for the one kind in polyvinylidene fluoride, polrvinyl chloride polyvinyl alcohol or Carboxymethyl cellulose sodium.
8. the preparation method of Prussian blue base sodium-ion battery positive material according to claim 1, it is characterised in that:Institute In stating step (2), the input amount of each component is Prussian blue 65-80 parts, conductive agent 15-25 parts, zirconium dioxide mill ball 80- 105 parts, binding agent 5-10 parts.
CN201611255163.XA 2016-12-30 2016-12-30 Preparation method of Prussian blue based sodium ion battery positive electrode material CN106654263A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107331864A (en) * 2017-06-21 2017-11-07 浙江大学 A kind of cyano group positive electrode and its preparation method and application
CN108821310A (en) * 2018-05-25 2018-11-16 浙江大学 One white material in type Prussia and its preparation method and application
CN109637813A (en) * 2018-11-12 2019-04-16 华东师范大学 A kind of sunlight helps seawater battery and preparation method
CN109728295A (en) * 2017-10-30 2019-05-07 宁德时代新能源科技股份有限公司 Positive electrode active materials and preparation method thereof and sodium-ion battery

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CN103208628A (en) * 2013-04-12 2013-07-17 中国科学院化学研究所 Sodium-ion battery positive material and preparation method and application thereof
CN104282908A (en) * 2014-09-24 2015-01-14 张五星 Method for synthesizing high-sodium iron-based Prussian blue electrode material

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CN103208628A (en) * 2013-04-12 2013-07-17 中国科学院化学研究所 Sodium-ion battery positive material and preparation method and application thereof
CN104282908A (en) * 2014-09-24 2015-01-14 张五星 Method for synthesizing high-sodium iron-based Prussian blue electrode material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107331864A (en) * 2017-06-21 2017-11-07 浙江大学 A kind of cyano group positive electrode and its preparation method and application
CN107331864B (en) * 2017-06-21 2019-10-18 浙江大学 A kind of cyano positive electrode and its preparation method and application
CN109728295A (en) * 2017-10-30 2019-05-07 宁德时代新能源科技股份有限公司 Positive electrode active materials and preparation method thereof and sodium-ion battery
CN108821310A (en) * 2018-05-25 2018-11-16 浙江大学 One white material in type Prussia and its preparation method and application
CN108821310B (en) * 2018-05-25 2020-04-14 浙江大学 Prussian-like white material and preparation method and application thereof
CN109637813A (en) * 2018-11-12 2019-04-16 华东师范大学 A kind of sunlight helps seawater battery and preparation method

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