CN109546163A - A kind of method of modifying of organic flow battery graphite felt electrode - Google Patents

A kind of method of modifying of organic flow battery graphite felt electrode Download PDF

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Publication number
CN109546163A
CN109546163A CN201811356141.1A CN201811356141A CN109546163A CN 109546163 A CN109546163 A CN 109546163A CN 201811356141 A CN201811356141 A CN 201811356141A CN 109546163 A CN109546163 A CN 109546163A
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graphite felt
flow battery
graphite
modifying
organic
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CN109546163B (en
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张庶
罗金宏
李恩竹
张树人
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University of Electronic Science and Technology of China
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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
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8817—Treatment of supports before application of the catalytic active composition
    • 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
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • 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
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to the organic battery technologies in electrochemical energy storage field, are related to a kind of method of manganese dioxide modification graphite felt electrode being produced on a large scale, specially a kind of method of modifying of organic flow battery graphite felt electrode.The present invention is first handled graphite felt with ultrasound-nitration mixture, to increase the surface area of graphite fibre, increases the reaction site of graphite electrode, and graphite fibre surface has no obvious fracture；Secondly, its electrochemical reaction catalytic activity of the surface enhanced of graphite fibre is grown in using manganese dioxide, to improve battery capacity and energy efficiency.Operation of the present invention is simple and easy, is produced on a large scale, and application cost is low, provides a kind of electrode material processing approach of performance significant increase for the preparation of organic flow battery.

Description

A kind of method of modifying of organic flow battery graphite felt electrode
Technical field
The invention belongs to the organic battery technologies in electrochemical energy storage field, are related to a kind of titanium dioxide being produced on a large scale The method that manganese modifies graphite felt electrode, specially a kind of method of modifying of organic flow battery graphite felt electrode.
Background technique
With the rapid development of economy, the problems such as energy shortage increasingly sharpens, various countries researcher has been greatly facilitated to can The research of the renewable sources of energy.Since renewable energy has the problem of discontinuous, unstable, grid-connected hardly possible, cause its utilization rate low, abandons Wind abandons light rate height.Therefore needing to greatly develop can extensive energy storage technology matched with its.In various energy storage technologies, liquid stream Battery is greatly developed with its power and the mutually independent advantage of energy.
Organic flow battery is a kind of novel electric energy storing system, it be using different organic matter active substance solutions as Electrolyte in positive and negative fluid reservoir is transported in battery pile, through electrode by the energy-storage battery of positive and negative electrode material by external pump It is flowed back in fluid reservoir again after being reacted.Compared with other electrochemical energy storage cells, organic flow battery has extended cycle life, Maintenance cost is few, and cheap after organic electrolyte large-scale production, the response time is short, can modularization etc., especially organic liquid stream Cell electrolyte element is made of the high element of the crustal abundances such as carbon, hydrogen, oxygen, and scarcity is not present.
Graphite electrode possesses good corrosion resistance, and good electric conductivity, chemical stability, cost is relatively low, is ideal Electrode of liquid flow cell material.Currently used is PAN based graphite felt, and not only electric property is good, and is porous material Material has biggish specific surface area, can provide sufficient reaction site to react.
However, the chemical property of untreated graphite felt electrode is poor, therefore by being modified, improve graphite felt electrode It is most important to the electrocatalysis characteristic of positive and negative anodes reaction.Currently used major measure has 3: the surface functionalization of electrode； Deposited metal or transition metal oxide；The bulk doped of other elements.
Summary of the invention
For above-mentioned there are problem or deficiency, to improve graphite felt electro-chemical activity and as battery electrode when is entirely electric The capacity and energy efficiency in pond, the present invention provides a kind of method of modifying of organic flow battery graphite felt, mixed using ultrasound- After acid processing, manganese dioxide is grown on graphite fibre.
Technical solution is as follows:
Step 1 uses the nitration mixture of sulfuric acid and nitric acid composition to the graphite felt of 0.5mm-20mm thickness under ultrasound condition first It is impregnated, sulfuric acid concentration is 8-18.4mol/L in nitration mixture, and concentration of nitric acid 3-20mol/L, graphite felt is in progress nitration mixture processing Time be 1min-8h, holding temperature be 23-83 DEG C.
Graphite felt made from step 1 is rinsed to neutrality and is dried by step 2, is subsequently placed into liquor potassic permanganate and is infiltrated The gap of graphite felt is fully taken up to liquor potassic permanganate.
Saturated alkyl primary alconol is uniformly evaporated on the graphite felt fibres after step 2 infiltrates and carries out high temperature and moves back by step 3 Fire；When being annealed, heating temperature is 80-425 DEG C, soaking time 15min-5h；It takes out and is rinsed easily after the completion of annealing Molten substance is simultaneously dried for standby.
Further, the graphite felt is at the pre- place for being cleaned by ultrasonic and drying through deionized water, ultrapure water, alcohols or ketone The operation of step 1 is carried out after reason again.
Further, in the step 3 be saturated alkyl primary alcohol be methanol, ethyl alcohol, normal propyl alcohol, n-butanol, n-amyl alcohol and/or Ethylene glycol, using mixed alcohol Shi Kewei arbitrary proportion.
The present invention is first handled graphite felt with ultrasound-nitration mixture, to increase the surface area of graphite fibre, increases stone The reaction site of electrode ink, and graphite fibre surface has no obvious fracture；Secondly, being grown in graphite fibre using manganese dioxide Its electrochemical reaction catalytic activity of surface enhanced, to improve battery capacity and energy efficiency.
Operation of the present invention is simple and easy, is produced on a large scale, and application cost is low, and the preparation for organic flow battery provides A kind of electrode material processing approach of performance significant increase.
Detailed description of the invention
Fig. 1 is the discharge capacity and energy dose-effect that the graphite felt after embodiment 1 is modified is packed into organic flow battery circulation Rate test chart；
Fig. 2 is the discharge capacity and energy efficiency that unprocessed graphite felt is packed into organic flow battery circulation.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Step 1, ultrasound-nitration mixture handle graphite felt, are equipped with being placed in a thickness of the graphite felt of 4mm (2.5cm*2.5cm) The mixed acid solution of the 40mL concentrated sulfuric acid and concentrated nitric acidPolytetrafluoroethylcontainer container in, and be put into ultrasonic clear Washing machine heating water bath is to 80 DEG C, ultrasonic 10min.It is cooled to room temperature to it, graphite felt is rinsed to neutrality, and dried.
Step 2, the graphite felt for obtaining step 1 is put into 0.1mol/L liquor potassic permanganate is totally submerged it, places 12h Afterwards；Its surface residual solution is blotted in taking-up.
Graphite felt after step 2 infiltration is put into semiclosed container for evaporation by step 3, and dehydrated alcohol is evaporated to graphite On felt type product, at 60 DEG C, the time is for 24 hours for temperature control.Then high annealing, temperature 250 are carried out to gained graphite felt sample DEG C, keep the temperature 2h；Then it is dried for standby after rinsing readily soluble substance.
By graphite felt electrode prepared by embodiment and unprocessed graphite felt be respectively charged into organic quinones flow battery into Row test, test result are as shown in Figure 1, Figure 2.
The anode electrolyte electrochemically active molecules of organic quinones flow battery are formula A, formula B phenol compound or formula A With the oxidation product of formula B phenol compound；The electrolyte liquid electrochemically active molecules of organic quinones flow battery are formula C anthracene Quinones or its reduzate, and it is acid or neutral for adjusting positive and negative anodes electrolyte；
In formula,
R1、R2、R3、R4It is each independently selected from the following group: hydrogen (- H), sulfonic group (- SO3H), nitro (- NO2) or phosphate (- PO3H2)；
R5、R6、R7、R8It is each independently selected from the following group: hydrogen (- H), sulfonic group (- SO3H), nitro (- NO2) or phosphate (- PO3H2)；
R9、R10、R11、R12、R13、R14、R15、R16It is each independently selected from the following group: hydrogen (- H), sulfonic group (- SO3H), nitro (-NO2) or phosphate (- PO3H2)。
The preparation method of organic quinones fluid cell electrolyte is specific as follows: taking 1,2- phenol -3,5- shown in molecular formula D Disulfonic acid (BQDS) is formulated as the clear aqueous solution that concentration is 0.5mol/L, and the 1.1mL concentrated sulfuric acid is added under stiring, then will Positive fluid reservoir is added in solution.
9,10- anthraquinone-2-sulfonic acid (AQS) shown in molecular formula E is taken to be formulated as the clear aqueous solution that concentration is 0.5mol/L, And the 1.1mL concentrated sulfuric acid is added under stiring, cathode fluid reservoir then is added in solution.Organic flow battery is in 100mA/cm2's It is recycled under current density.
It is prepared from the test result of Fig. 1 and Fig. 2 as it can be seen that in the charge and discharge cycles of above-mentioned organic quinones flow battery Graphite felt electrode 12% has been respectively increased to reversible stored energy capacitance and charge and discharge cycles energy efficiency than unprocessed graphite felt With 10%, the performance of existing organic quinones flow battery is improved.

Claims (3)

1. a kind of method of modifying of organic flow battery graphite felt, comprising the following steps:
Step 1 is carried out under ultrasound condition using graphite felt of the nitration mixture of sulfuric acid and nitric acid composition to 0.5mm-20mm thickness first Impregnate, sulfuric acid concentration is 8-18.4mol/L in nitration mixture, concentration of nitric acid 3-20mol/L, graphite felt carry out nitration mixture processing when Between be 1min-8h, holding temperature be 23-83 DEG C；
Graphite felt made from step 1 is rinsed to neutrality and is dried by step 2, be subsequently placed into liquor potassic permanganate infiltrate it is supreme Potassium manganate solution fully takes up the gap of graphite felt；
Saturated alkyl primary alconol is uniformly evaporated on the graphite felt fibres after step 2 infiltrates and carries out high annealing by step 3；? When being annealed, heating temperature is 80-425 DEG C, soaking time 15min-5h；It is taken out after the completion of annealing and rinses readily soluble substance And it is dried for standby.
2. the method for modifying of organic flow battery graphite felt as described in claim 1, it is characterised in that: the graphite felt is passing through Deionized water, ultrapure water, alcohols or ketone are cleaned by ultrasonic and carry out the operation of step 1 after the pretreatment dried again.
3. the method for modifying of organic flow battery graphite felt as described in claim 1, it is characterised in that: the step 3 is embezzled It is methanol, ethyl alcohol, normal propyl alcohol, n-butanol, n-amyl alcohol and/or ethylene glycol with alkyl primary alcohol.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110444771A (en) * 2019-08-12 2019-11-12 中盐金坛盐化有限责任公司 Organic water phase flow battery, electrode, method of modifying and redox flow battery energy storage system
CN110492055A (en) * 2019-08-12 2019-11-22 中盐金坛盐化有限责任公司 Modify method, electrode, battery and the energy-storage system of organic flow battery electrode
CN110492054A (en) * 2019-08-12 2019-11-22 中盐金坛盐化有限责任公司 Modify method, electrode, battery and the energy-storage system of organic flow battery electrode
CN111740126A (en) * 2020-07-03 2020-10-02 朱义奎 Chemical doping modification method for graphite felt electrode material of vanadium battery
CN112663329A (en) * 2020-12-23 2021-04-16 华东师范大学 Simple acid treatment method for graphite felt
CN113054204A (en) * 2021-03-17 2021-06-29 电子科技大学 Graphite felt electrode for alkaline organic flow battery and modification method
CN113054203A (en) * 2021-03-17 2021-06-29 电子科技大学 Graphite felt electrode for all-vanadium redox flow battery and modification method
CN115029720A (en) * 2022-06-30 2022-09-09 中化学朗正环保科技有限公司 Method for preparing modified graphite felt electrode

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110444771A (en) * 2019-08-12 2019-11-12 中盐金坛盐化有限责任公司 Organic water phase flow battery, electrode, method of modifying and redox flow battery energy storage system
CN110492055A (en) * 2019-08-12 2019-11-22 中盐金坛盐化有限责任公司 Modify method, electrode, battery and the energy-storage system of organic flow battery electrode
CN110492054A (en) * 2019-08-12 2019-11-22 中盐金坛盐化有限责任公司 Modify method, electrode, battery and the energy-storage system of organic flow battery electrode
CN110492055B (en) * 2019-08-12 2021-10-08 中盐金坛盐化有限责任公司 Method for modifying electrode for organic flow battery, electrode, battery and energy storage system
CN111740126A (en) * 2020-07-03 2020-10-02 朱义奎 Chemical doping modification method for graphite felt electrode material of vanadium battery
CN112663329A (en) * 2020-12-23 2021-04-16 华东师范大学 Simple acid treatment method for graphite felt
CN113054204A (en) * 2021-03-17 2021-06-29 电子科技大学 Graphite felt electrode for alkaline organic flow battery and modification method
CN113054203A (en) * 2021-03-17 2021-06-29 电子科技大学 Graphite felt electrode for all-vanadium redox flow battery and modification method
CN115029720A (en) * 2022-06-30 2022-09-09 中化学朗正环保科技有限公司 Method for preparing modified graphite felt electrode
CN115029720B (en) * 2022-06-30 2024-04-30 中化学朗正环保科技有限公司 Method for preparing modified graphite felt electrode

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