CN110729504B - Method and system for reducing oxidation speed of electrode of flow battery - Google Patents

Method and system for reducing oxidation speed of electrode of flow battery Download PDF

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CN110729504B
CN110729504B CN201810783095.7A CN201810783095A CN110729504B CN 110729504 B CN110729504 B CN 110729504B CN 201810783095 A CN201810783095 A CN 201810783095A CN 110729504 B CN110729504 B CN 110729504B
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高新亮
张华民
邹毅
王晓丽
张涛
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Dalian Rongke Power Co Ltd
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    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
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Abstract

A method and a system for reducing the oxidation speed of an electrode of a flow battery belong to the field of flow batteries, and aim to solve the problem of oxidation of the electrode of the flow battery, the technical key points are as follows: the method comprises the step of adding an organic reducing agent into the anode electrolyte solution, and has the effect of reducing the oxidation speed of the anode carbon felt electrode.

Description

Method and system for reducing oxidation speed of electrode of flow battery
Technical Field
The invention belongs to the field of flow batteries, and relates to a method and a system for reducing the oxidation speed of an electrode of a flow battery.
Background
The all-vanadium redox flow battery becomes a preferred scheme for large-scale energy storage due to the advantages of high safety, long service life, independent power capacity and convenience for large-scale production. However, the stability of long-term operation of each component device of a large-scale MW-grade vanadium battery project is a main factor for restricting the performance of the vanadium battery. The 10 kW-level electric pile relates to series-parallel connection of several electric piles, each electric pile comprises series connection of dozens of single batteries, so that the reduction of the performance of any one battery directly influences the normal use of the whole electric pile, and how to improve the tolerance of the single battery and further increase the stability of the single electric pile is the most basic ring for prolonging the service life of a large-scale system and reducing the maintenance cost.
The operation fault summary of the single cell stack for years shows that the most common irreversible symptoms of the kW-grade cell stack are mainly represented by irreversible and continuous increase of the voltage value of a single cell, and the main reasons are that the electrode is blocked by vanadium salt (positive and negative electrodes) and the electrode is oxidized and damaged (positive electrode) due to long-time operation of the cell stack. The reason of the highest frequency of the two is that the anode carbon felt electrode is oxidized and damaged, and the root cause of the electrode oxidation is as follows: during charging, when the concentration of the substrate to be reacted (e.g. V in the positive solution of a vanadium cell)4+) When the current drops to a certain degree, the excessive current takes a carbon felt electrode as a substrate, and the oxidation of the carbon felt electrode is accelerated. Due to the existence of the hydrogen evolution side reaction of the cathode solution of the all-vanadium flow battery: 2H++2V2+＝2V3++H2℃ @, the reaction belongs to the self-discharge reaction of the negative electrode, the continuous attenuation of the system discharge capacity caused by the long-term accumulation of the hydrogen evolution side reaction is one of the main reasons of the capacity attenuation of the all-vanadium redox flow battery, and simultaneously the reaction causes the V in the charging process of the positive electrode solution4+The concentration is further reduced, so that the oxidation of the anode electrode in the charging process is further intensified。
At present, the following two methods are mainly used to improve the problem of oxidation damage of the electrode:
the mixed acid system prevents the carbon felt electrode from oxidizing: a mixed acid all-vanadium battery system which uses a mixed acid of hydrochloric acid (8mol/L) and sulfuric acid (1mol/L) as a supporting electrolyte, due to the presence of a large amount of hydrochloric acid in the electrolyte, so that Cl in the positive electrode solution-1Is easy to be oxidized to be separated out of the solution, which is an inherent side reaction of the mixed acid vanadium battery system, and Cl is easy to be separated out when the positive electrode solution has high SOC due to the existence of chlorine separation reaction-1Continuously lose electrons, thereby being used as a substrate and a 4-valent vanadium ion (V)4+) Are oxidized together, thereby avoiding the accelerated oxidation of the carbon felt by current when the valence-4 vanadium is insufficient, and the Cl is utilized2Side reactions are precipitated to protect the electrodes.
The method for increasing the flow rate at the end of charging comprises the following steps: in the early report, the method of increasing the flow rate of the electrolyte at the charging end is adopted to reduce the phenomenon of difficult charging caused by the increase of concentration polarization at the charging end, so as to slow down the oxidation of the electrode, however, the method has little effect on protecting the electrode and has no substantial effect.
Disclosure of Invention
In order to solve the problem of electrode oxidation resistance of the flow battery, the invention provides the following technical scheme: a method for reducing the oxidation speed of an electrode of a flow battery comprises the step of adding an organic reducing agent into a positive electrolyte solution.
Further, the step of adding an organic reducing agent includes adding a weak organic reducing agent to the positive electrode electrolyte solution at intervals.
Further, the concentration of the weak organic reducing agent added into the positive electrolyte solution is detected, and when the concentration of the weak organic reducing agent in the positive electrolyte solution is lower than a threshold value, the weak organic reducing agent is supplemented; the interval between the two additions of the weak organic reducing agent is the time interval.
Furthermore, the time interval of adding the weak organic reducing agent in the positive electrolyte solution is 40-60 charge-discharge cycle periods of the flow battery.
Further, the step of adding the organic reducing agent comprises the step of adding a strong organic reducing agent to the positive electrode electrolyte at the end of charging of the flow battery in one charge-discharge cycle.
Further, in the last stage of charging of the positive electrolyte in the charge-discharge cycle of the flow battery, when the SOC of the positive electrolyte is greater than 85% and the average valence states of the positive electrolyte and the negative electrolyte are greater than or equal to 3.6, a strong organic reducing agent is added into the positive electrolyte in the last stage of charging until the SOC of the positive electrolyte is less than 75%.
Further, the method also comprises the step of leading the negative electrolyte into a part of the positive electrolyte storage tank by a guide pump.
Further, at the last stage of charging of the positive electrolyte in the charge-discharge cycle of the flow battery, when the SOC of the positive electrolyte is greater than 85% and the average valence states of the positive electrolyte and the negative electrolyte are less than 3.6, a part of the negative electrolyte is led into the positive electrolyte storage tank by the guide pump until the SOC of the positive electrolyte at the last stage of charging is less than 80%.
A system for reducing the oxidation speed of an electrode of a flow battery comprises a reducing agent adding device and a control device, wherein the control device controls the reducing agent adding device to add an organic reducing agent into a positive electrolyte solution.
Furthermore, the raw agent adding equipment is controlled by the control device to put the weak organic reducing agent into the flow battery every 40-60 charging and discharging cycle periods.
Further, the device also comprises a reducing agent detection device which detects the concentration of the weak organic reducing agent added into the positive electrolyte solution, and the control device controls the reducing agent adding device to supplement and add the weak organic reducing agent when the concentration of the weak organic reducing agent in the positive electrolyte solution is lower than a threshold value.
Further, the device also comprises an SOC monitoring device and an SOC monitoring device, wherein the SOC monitoring device is arranged below the liquid level of the positive electrolyte and is used for placing a reference electrode, the SOC monitoring device is used for monitoring the SOC of the positive electrolyte, the SOC exceeds the limit, then the SOC device sends a control signal to the control device, and the control device receives and drives the reducing agent adding equipment to add the strong organic reducing agent into the positive electrolyte.
Furthermore, the system also comprises a guide pump connected with the positive electrolyte storage tank and the negative electrolyte storage tank so as to lead a part of negative electrolyte into the positive electrolyte storage tank under the condition that the SOC of the electrolyte exceeds the limit.
Has the advantages that: adding a weak organic reducing agent into the electrolyte solution of the positive electrode at a time interval; and adding a strong organic reducing agent into the positive electrolyte at the last stage of charging of the positive electrolyte in each charge-discharge cycle of the flow battery. Namely, the organic reducing agent is selected to reduce the 5-valent vanadium (V) of the anode5+) Solution to 4V (V)4+) The solution can increase the concentration of a reaction substrate of the anode in the charging process, further reduce the oxidation speed of the anode carbon felt electrode, and can reduce the oxidation speed of the anode carbon felt electrode by using a two-stage addition mode, and start emergency measures during routine maintenance and SOC overrun, so that the oxidation speed of the anode carbon felt electrode is slower, and the mode is safer.
Detailed Description
In this embodiment, a method for reducing the oxidation rate of the electrode of the flow battery is to quickly determine the overall average valence state of the positive and negative electrolytes before the SOC of the positive electrolyte reaches 85%. When the overall average valence state is more than or equal to 3.6, specifically, when the SOC of the positive electrolyte is more than 85% at the final stage of charging, the method 1 is adopted to reduce the oxidation speed of the positive carbon felt electrode, namely a method for automatically adding a reducing agent; when the overall valence state is less than 3.6, specifically, when the SOC of the positive electrolyte is more than 80%, the method 2 is adopted to reduce the oxidation speed of the positive carbon felt electrode, and a part of the negative electrolyte is introduced into the positive electrode.
The average valence state calculation method of the electrolyte is as follows:
the vanadium ions in the vanadium battery system have four valence states, and for convenience of calculating, comparing and estimating the electrolyte unbalance degree of the system, the valence states of the anode system and the cathode system of the system are regarded as a whole to be subjected to weighted calculation.
The initial valence state of the finished electrolyte is 3.5, meaning 3 (V) in the electrolyte3+) And Vanadium (VO) in valence 42+) The concentration of the ions each accounted for 50% of the total vanadium concentration.
The specific calculation method of the average valence state of the electrolyte comprises the following steps:
Figure BDA0001733059560000051
wherein: i is the valence state of the vanadium ion, and the possible numerical values of i are 2, 3, 4 and 5;
Figure BDA0001733059560000052
-concentration of vanadium ions of valence i;
Figure BDA0001733059560000053
the volume of vanadium ions of valence i.
Through the above formula, the respective average valence states of the positive and negative electrolytes and the average valence state of the mixed positive and negative electrolytes can be calculated. The application significance is as follows: (1) knowing the capacity attenuation condition of the electrolyte and avoiding the damage of the valence state deviation of the electrolyte to the system; (2) the method is an important basis for leveling the electrolyte and calculating the consumption of the recovery agent to recover the system capacity.
Example (c):
the current electrolyte parameters and calculation results of the 2kW/1.5kWh system are as follows:
Figure BDA0001733059560000061
the data are directly acquired by a signal acquisition system and then calculated by a computer program to obtain the average valence states of the electrolyte of the positive electrode and the negative electrode.
The solution in this embodiment can solve the problem of electrode oxidation resistance of the flow battery, however, by testing the total valence state shift of the battery system, a professional instrument and an operator are required to be configured, and the maintenance cost is increased. At present, when the discharge capacity of a liquid flow system is attenuated to the required lower limit, the system capacity can be recovered by leveling the average valence state of the vanadium electrolyte of the system, but no matter a reducing agent is added or an online electrolysis method is adopted, the investment and the loss of manpower, material resources, equipment and system shutdown can be brought, the maintenance cost is high, for example, a 1MW/2MWh system is taken, the valence state of the system deviates from 30%, and the annual maintenance cost is close to 3 ten thousand yuan.
In order to solve the problem, in another embodiment, a method for reducing the oxidation rate of an electrode of a flow battery is an additive control method for resisting electrode oxidation, and is divided into two modes, namely a mode of adding a valence-state restoring agent and a mode of introducing an electrolyte, wherein the two modes can be used independently or in combination, and the specific method comprises the following steps:
adding a valence state restoring agent, namely adding a weak organic reducing agent and a strong organic reducing agent under a certain condition, wherein the weak organic reducing agent and the strong organic reducing agent can be used independently or in combination, and the weak organic reducing agent is added once at long time intervals (46-60 charging and discharging cycles) or when the concentration of the valence state restoring agent is lower than a corresponding threshold value of initial concentration; for strong organic reducing agents, the addition is made at the end of charge of each charge-discharge cycle at a certain SOC level and electrolyte valence.
The electrolyte introduction method is also performed under a certain condition, and mainly the SOC level and the electrolyte valence state are used as the conditions for judging whether or not to introduce.
The definition of the strong and weak organic reducing agents is as follows: when the reaction temperature is between 30 and 35 ℃, for any organic matter CxHyOz, when the oxide V is5+In proportion of total vanadium>90% and in the case of a large excess relative to the reducing agent, in the case of complete oxidative conversion of 1mol of its molecules to xmolCO2Required time of>96h, called weak organic reducing agent. Correspondingly, if 1mol of its molecule is completely oxidized to xmolCO2Required time of<And 8h, namely a strong organic reducing agent. The specified time point of taking 50 cycles as the supplement time point of the weak organic reducing agent in the system is the average V according to the charging and discharging process5+The concentration of the weak organic reducing agent is completely oxidized into CO according to a certain adding amount in the system2The number of charge-discharge cycles calculated.
The following table lists several common strong and weak organic reducing agents and lists the percent increase in carbon mat sheet resistance after 500 cycles by the addition of strong and weak organic reducing agents compared to a control without any reducing agent.
Figure BDA0001733059560000071
The specific method for introducing the reducing agent and the electrolyte solution is as follows:
(1) adding an organic reducing agent with a fixed oxidation potential, namely a weak organic reducing agent, wherein for the addition of the weak organic reducing agent, two adding time judgment methods are provided, one method is 40-60, preferably, the addition is carried out once at intervals of 50 charge-discharge cycle periods, and the 50 charge-discharge cycle periods are generally just in the range that the concentration of the weak organic reducing agent is reduced from the initial concentration to the lower concentration and are suitable for the addition at the moment; a method for detecting the concentration of weak reducing agent added initially to judge if its concentration reaches threshold value includes such steps as adding the new weak reducing agent to the electrolyte at initial stage, adding the electrolyte to anode at the oxidation voltage of 1.4-1.6V, and adding substrate V when the electrolyte reaches 1.5V and the SOC is raised4+When the supply of electrons is not enough to consume the charging current, the reducing agent can be supplied to be oxidized before the carbon felt so as to protect the carbon felt. The weak reducing agent is present in the positive electrolyte and only acts rapidly in the high SOC stage to consume excess current, and when charging stops and the potential drops, the reaction automatically weakens and stops. The weak reducing agent is applied to a system with slower decay, and when the monitored amount of the weak reducing agent in the electrolyte drops below 0.001mol/L, the weak reducing agent is continuously replenished to 0.005 mol/L. Wherein, the initial adding concentration of the weak reducing agent is determined to be 0.005mol/L, and the thinking of the initial concentration determination is as follows:
1) and (4) the hydrogen evolution amount of each charge-discharge cycle when the flow battery system is in normal operation.
2) The operating frequency. For example, for a 5MW/10MWh system, the hydrogen evolution rate is 6LH for one charge-discharge cycle per day2/100Lsolution。The hydrogen evolution amount per 1MWh electrolyte per day is 60m3×6L×103360L. Folding deviceThe valence state deviation (increase) of the vanadium ions in the system is 3 x 10-4The valence is increased by about 0.03 in 3 months, namely the vanadium valence 5 is increased by 32.14mol, taking ethanol as an example, 1mol of ethanol can reduce 12mol of vanadium valence 5, 2.68mol of ethanol is needed every day, the time of 3 months is about 2.68X 90mol, and the total amount is about 300mol considering the comprehensive influence of other factors, namely 0.005mol/L ethanol is added in the solution initially.
(2) Adding a strong organic reducing agent, namely a rapid reducing agent, when the positive electrolyte is in a charging process and when the SOC of the positive electrolyte is more than 85 percent and the average valence state of the positive electrolyte and the negative electrolyte is more than or equal to 3.6, adding the strong organic reducing agent into the positive electrolyte at the last stage of charging until the SOC of the positive electrolyte is less than 75 percent. The flow battery system drives the reducing agent adding device through the control device to add the strong reducing agent to the positive electrode electrolyte, and the reducing agent begins to react with the positive electrode electrolyte5+Reaction takes place to provide substrate V4+To mitigate oxidation of the carbon felt, and the addition time and concentration are determined according to the operation mode and the total capacity of the flow battery system. And a positive electrode charging state monitoring device is matched, and sends a signal to a control device to drive the reducing agent adding equipment to add the strong reducing agent.
(3) And in the electrolyte introduction mode, in the charging process of each charge-discharge cycle, the SOC of the positive electrolyte is more than 85%, and the average valence state of the positive electrolyte and the negative electrolyte is less than 3.6, the negative electrolyte is introduced into a part of the positive electrolyte storage tank by the guide pump, and the negative electrolyte is stopped being continuously introduced into the positive electrolyte storage tank until the SOC of the positive electrolyte is less than 80%. V thus introduced from the negative electrode3+And V2+Will react with V in the positive electrolyte5+Generating a large number of V4+Available V at the end of charge of the positive electrode electrolyte4+The defect is greatly relieved, the oxidation speed of the positive carbon felt electrode is effectively reduced, and the system capacity of the flow battery can be improved.
In the embodiment, a system for reducing the oxidation speed of the electrode of the flow battery is further described, and the system comprises an SOC monitoring device, reducing agent adding equipment and a control device, wherein the SOC monitoring device is arranged below the liquid level of the positive electrolyte and is provided with a reference electrode, the SOC monitoring system is used for monitoring the SOC level of the positive electrolyte in each charging and discharging cycle, if the SOC level exceeds the limit, the SOC monitoring system sends out a control signal, the control device receives and drives the reducing agent adding equipment, and the strong organic reducing agent is added into the positive electrolyte in the last charging stage of the positive electrolyte of the flow battery. The system comprises a reducing agent detection device which detects the concentration of the weak organic reducing agent added into the positive electrolyte solution, and a control device controls the original agent adding device to add the weak organic reducing agent in a supplementing manner when the concentration of the weak organic reducing agent in the positive electrolyte solution is lower than a threshold value. In this case, it is preferable that the reducing agent addition means does not periodically add the weak organic reducing agent to the positive electrode electrolyte.
The system for reducing the oxidation speed of the electrode of the flow battery further comprises a guide pump, the guide pump is communicated with the positive electrolyte storage tank and the negative electrolyte storage tank, during the charging period of the positive electrolyte of each charging and discharging cycle of the flow battery, the SOC of the positive electrolyte is more than 85%, and the average valence of the positive electrolyte and the negative electrolyte is less than 3.6, the guide pump guides the negative electrolyte into one part of the positive electrolyte storage tank, and when the SOC of the positive electrolyte is less than 80%, the guide pump stops continuously guiding the negative electrolyte into the positive electrolyte storage tank.
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.

Claims (5)

1. A method for reducing the oxidation speed of an electrode of a flow battery is characterized by comprising the steps of adding a weak organic reducing agent into a positive electrolyte solution at certain time intervals and adding a strong organic reducing agent into the positive electrolyte at the last charging stage of one charge-discharge cycle of the flow battery; detecting the concentration of the weak organic reducing agent added into the positive electrolyte solution, and supplementing the weak organic reducing agent when the concentration of the weak organic reducing agent in the positive electrolyte solution is lower than a threshold value; the interval between the two times of adding the weak organic reducing agent is 40-60 charge-discharge cycle periods of the flow battery;
in the last stage of charging of the positive electrolyte in the charge-discharge cycle of the redox flow battery, when the SOC of the positive electrolyte is more than 85 percent and the average valence states of the positive electrolyte and the negative electrolyte are more than or equal to 3.6, adding a strong organic reducing agent into the positive electrolyte in the last stage of charging until the SOC of the positive electrolyte is less than 75 percent; when the SOC of the positive electrolyte is more than 85 percent and the average valence of the positive electrolyte and the negative electrolyte is less than 3.6, leading a part of the negative electrolyte into a positive electrolyte storage tank by a guide pump until the SOC at the last charging stage of the positive electrolyte is less than 80 percent; the specific calculation method of the average valence state of the electrolyte comprises the following steps:
Figure FDA0003151355640000011
wherein: i is the valence state of the vanadium ion, and the possible numerical values of i are 2, 3, 4 and 5;
Figure FDA0003151355640000012
-concentration of vanadium ions of valence i;
Figure FDA0003151355640000013
-volume of vanadium ions of valence i;
the definition of weak and strong organic reducing agents is as follows: the reaction temperature is between 30 and 35 ℃, and for any organic matter CxHyOz, the reaction temperature is in oxide V5+In proportion of total vanadium>90% and in excess with respect to the reducing agent, when 1mol of organic molecules are completely oxidized and converted into xmolCO2Required time of>96h, the organic matter is called weak organic reducing agent, and when 1mol of organic matter molecules are completely oxidized and converted into xmolCO2Required time of<For 8h, theOrganic substances are called strong organic reducing agents; the electrode is a carbon felt.
2. A system for implementing the method for reducing the oxidation rate of an electrode of a flow battery as recited in claim 1, comprising a reducing agent addition device, a control device, the control device controlling the reducing agent addition device to add an organic reducing agent to the positive electrolyte solution; the reducing agent adding equipment is controlled by the control device to put the weak organic reducing agent into the flow battery once every 40-60 charging and discharging cycle periods.
3. The system for reducing the oxidation rate of an electrode of a flow battery as recited in claim 2, further comprising a reducing agent detection device that detects a concentration of the weak organic reducing agent added to the positive electrolyte solution, and the control device controls the reducing agent addition device to add the weak organic reducing agent in addition when the concentration of the weak organic reducing agent in the positive electrolyte solution is below a threshold.
4. The system for reducing the oxidation rate of an electrode of a flow battery as recited in claim 2, further comprising an SOC monitoring device, the SOC monitoring device being disposed below the level of the positive electrolyte and the reference electrode being disposed, the SOC monitoring device being configured to monitor the SOC of the positive electrolyte, the SOC exceeding being determined, the SOC monitoring device sending a control signal to the control device, the control device receiving and driving the reductant adding device to add the strong organic reductant to the positive electrolyte.
5. The system for reducing the rate of oxidation of an electrode of a flow battery of claim 2, further comprising a diversion pump coupled to the positive and negative electrolyte reservoirs to enable a portion of the negative electrolyte to be directed into the positive electrolyte reservoir during an electrolyte SOC overrun condition.
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