CN118263484A - Method and system for detecting electrolyte stable state of all-vanadium redox flow battery - Google Patents
Method and system for detecting electrolyte stable state of all-vanadium redox flow battery Download PDFInfo
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 453
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000008859 change Effects 0.000 claims abstract description 31
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 16
- 238000012546 transfer Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 8
- 230000033228 biological regulation Effects 0.000 claims description 7
- 229910001456 vanadium ion Inorganic materials 0.000 abstract description 14
- 230000003204 osmotic effect Effects 0.000 abstract description 4
- 238000011161 development Methods 0.000 description 9
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- 230000008569 process Effects 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 238000005562 fading Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 2
- 239000003011 anion exchange membrane Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000003014 ion exchange membrane Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002000 Electrolyte additive Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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Abstract
The invention relates to the field of all-vanadium redox flow batteries, and discloses a method and a system for detecting the stable state of electrolyte of an all-vanadium redox flow battery, wherein the method comprises the following steps: operating a primary battery system; collecting the volume, concentration and valence state data of the positive and negative electrolyte of the primary battery after 20 charge-discharge cycles are finished; calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte of the primary battery; judging the stable state of the electrolyte of the primary battery; stopping detection when the electrolyte of the primary battery is in a stable state, otherwise, adjusting the electrolyte, and performing a circulation test after adjustment; and recording the steady state parameters, and ending the test. According to the invention, the stable state of the electrolyte under different working conditions can be detected, and in the stable state, the shuttle speed of vanadium ions in different valence states, the total shuttle amount of the vanadium ions caused by the osmotic pressure difference and the hydraulic pressure difference of the electrolyte are in dynamic balance.
Description
Technical Field
The invention relates to the field of all-vanadium redox flow batteries, in particular to a method and a system for detecting the stable state of electrolyte of an all-vanadium redox flow battery.
Background
The positive and negative electrolyte in the all-vanadium redox flow battery are separated by a proton exchange membrane, however, the form and the speed of the transmembrane diffusion of vanadium ions in different valence states are different, so that the total amount of the vanadium ions in the positive and negative electrolyte is unbalanced, the capacity of the battery is attenuated, and the service life and the maintenance cost of the battery are influenced. Therefore, the research on an electrolyte preparation scheme with a higher stable state has important significance for further improving the performance of the all-vanadium redox flow battery.
At present, the prior art mainly enhances the stability of the electrolyte of the all-vanadium redox flow battery and slows down the capacity fading through electrolyte additives, membrane modification, structural design optimization and operation parameter regulation and control. The Chinese patent publication No. CN117638177A discloses a negative electrode electrolyte suitable for an all-vanadium redox flow battery, and the low-temperature stability and the electrode reaction activity at low temperature of the negative electrode electrolyte can be respectively improved by adopting mixed acid and additive, so that the high-efficiency operation of the all-vanadium redox flow battery at low temperature is realized. The chinese patent publication No. CN114744253B discloses a method for inhibiting capacity fade and on-line capacity recovery of an all-vanadium redox flow battery, which adopts a membrane that allows electrolyte of the all-vanadium redox flow battery to flow from positive electrode to negative electrode, for example: the PBI-based ion exchange membrane or other anion exchange membranes or porous membranes are connected in a pipeline outside the battery or are mixed with Nafion series proton exchange membranes in a galvanic pile for use, and the purposes of inhibiting the capacity attenuation and recovering the capacity of the all-vanadium redox flow battery are realized by adjusting the proportion of the PBI-based ion exchange membrane or other anion exchange membranes or the porous membranes to the Nafion series membranes. The Chinese patent publication No. CN112768721B discloses a composite serpentine flow channel structure and an all-vanadium redox flow battery containing the same, wherein a reserved electrode compression space is designed, electrolyte is guided to flow into the reserved compression electrode space through the composite serpentine flow channel and then flows into a porous electrode, so that the electrolyte is distributed more uniformly, the overpotential is reduced, and the performance of the battery is improved. The Chinese patent publication No. CN115472883A discloses a design method and application of an electrolyte of an all-vanadium redox flow battery with high capacity retention rate, and the average valence state of the electrolyte is improved to enable the anode liquid to generate excessive VO 2 + in the primary charging process, The defect of VO 2 + available to the positive electrode caused by the diffusion of V 2+ to the positive electrode to consume the VO 2 + is avoided, meanwhile, the accumulation of unavailable V 2+ in the negative electrode liquid is reduced, and the capacity retention rate of the all-vanadium redox flow battery is greatly improved. Although these methods can achieve a certain effect, they inevitably have problems of long development period, influence on battery performance, increase in cost, poor adaptability, and unchanged net migration of the electrolyte. The Chinese patent publication No. CN108091914A discloses a method for slowing down capacity fading of an all-vanadium redox flow battery and an ion permeability testing device, wherein the concentration ratio of positive and negative vanadium ions in the all-vanadium redox flow battery is controlled to be inversely proportional to the dynamic permeation speed ratio of positive and negative vanadium ions in an all-vanadium redox flow battery system, so that the capacity fading problem of the battery is relieved, and the utilization rate of electrolyte is improved. Although the problem of permeation of vanadium ions of positive and negative electrodes is involved, the shuttle speed of vanadium ions in different valence states is only used as a reference, and water shuttle and the change of the shuttle speed of the vanadium ions caused by osmotic pressure in the battery operation process are not considered, so that the electrolyte cannot keep a stable state for a long time in the use process, and meanwhile, the battery system for different working conditions is not strong in general applicability.
The invention provides a method and a system for detecting the stable state of electrolyte of an all-vanadium redox flow battery to solve the problems.
Disclosure of Invention
The invention aims to provide a method and a system for detecting the stable state of electrolyte of an all-vanadium redox flow battery, which are used for detecting data of the positive and negative electrode electrolyte in the stable state under different working conditions and guiding the development of the electrolyte, so that the problems of long development period, poor performance, high cost, poor adaptability and faster capacity attenuation of the electrolyte are solved.
The application discloses a method for detecting the stable state of electrolyte of an all-vanadium redox flow battery, which comprises the following steps:
step S1: operating a primary battery system to perform charge and discharge cycles;
step S2: collecting positive electrolyte volume, negative electrolyte volume, positive electrolyte concentration, negative electrolyte concentration, positive electrolyte valence state and negative electrolyte valence state data of the primary battery after 20 charge-discharge cycles are finished;
Step S3: calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte of the primary battery;
step S4: judging the stable state of the electrolyte of the primary battery;
Step S5: stopping detection when the primary battery electrolyte is in a stable state; otherwise, electrolyte is adjusted, and the steps S1-S4 are iterated after adjustment;
Step S6: and recording the steady state parameters, and ending the test.
Preferably, the working conditions of the charge-discharge cycle in step S1 are as follows: the voltage range of the single cell is 0.6-1.7V, the current density is 20-300 mA/cm 2, the initial electrolyte concentration is 1.0-3.0 mol/L, and the average valence state of the initial electrolyte is 3.5.
Preferably, in step S3, the calculation formula for calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte of the primary battery is as follows:
;
;
;
Wherein: -a rate of change of volume, The volume of the positive electrolyte of the primary battery,The initial volume of the primary battery positive electrolyte,-A rate of change of the concentration,The concentration of the positive electrolyte of the primary battery,The initial concentration of the first-stage battery positive electrolyte,The average valence state of the electrolyte of the primary battery,-The volume of the first-stage battery negative electrode electrolyte,The concentration of the negative electrolyte of the primary battery,The valence state of the positive electrolyte of the primary battery,-The valence state of the negative electrolyte of the primary battery.
Preferably, the judging method for judging the stable state of the electrolyte of the primary battery in the step S4 is as follows: when the volume change rate is 1% or less, the concentration change rate is 1% or less, and the average valence state is 3.49 or more and 3.51 or less, the electrolyte is in a stable state.
Preferably, the step of electrolyte adjustment in step S5 is:
step S51: determining initial barrel, target barrel, and volume of electrolyte transfer
；
Wherein: -electrolyte transfer volume;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery positive electrolyte barrel, and the electrolyte transfer target barrel is a first-stage battery negative electrolyte barrel;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery cathode electrolyte barrel, and the electrolyte transfer target barrel is a first-stage battery anode electrolyte barrel;
step S52: electrolyte transfer is carried out, and the volume extracted from the initial barrel for electrolyte transfer is The electrolyte of the electrolyte is fed into a secondary battery cathode electrolyte barrel;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows:
Wherein: -a charge level of the electric power, -The number of cores of the secondary cell stack;
step S54: and after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel into the electrolyte transfer target barrel.
Preferably, the steady state parameters in step S6 are: the volume of the positive electrode electrolyte, the concentration of the positive electrode electrolyte, the valence state of the positive electrode electrolyte, the volume of the negative electrode electrolyte, the concentration of the negative electrode electrolyte and the valence state of the negative electrode electrolyte of the primary battery.
A system for an all-vanadium redox flow battery electrolyte steady state detection method, comprising: the system comprises a primary battery system, a secondary battery system and an adjustment detection system, wherein the adjustment detection system is connected with the primary battery system and the secondary battery system through pipelines respectively.
Preferably, the primary battery system includes at least: a primary battery stack, a primary battery positive electrode pump, a primary battery positive electrode electrolyte barrel, a primary battery negative electrode pump and a primary battery negative electrode electrolyte barrel;
The primary battery pile is respectively connected with a primary battery positive electrode pump, a primary battery negative electrode pump, a primary battery positive electrode electrolyte barrel and a primary battery negative electrode electrolyte barrel through pipelines;
Two ends of the primary battery positive electrode pump are respectively connected with the primary battery pile and the primary battery positive electrode electrolyte barrel through pipelines;
The primary battery positive electrode electrolyte barrel is respectively connected with the primary battery pile, the primary battery positive electrode pump and the adjustment detection system through pipelines; a primary battery positive electrolyte level detector is arranged in the primary battery positive electrolyte barrel;
Two ends of the primary battery cathode pump are respectively connected with the primary battery pile and the primary battery cathode electrolyte barrel through pipelines;
The primary battery cathode electrolyte barrel is respectively connected with the primary battery pile, the primary battery cathode pump and the adjustment detection system through pipelines; and a primary battery negative electrolyte liquid level detector is arranged in the primary battery negative electrolyte barrel.
Preferably, the secondary battery system includes at least: a secondary battery stack, a secondary battery positive electrode pump, a secondary battery positive electrode electrolyte barrel, a secondary battery negative electrode pump and a secondary battery negative electrode electrolyte barrel;
The secondary battery pile is respectively connected with the secondary battery positive electrode pump, the secondary battery negative electrode pump, the secondary battery positive electrode electrolyte barrel and the secondary battery negative electrode electrolyte barrel through pipelines;
Two ends of the secondary battery positive electrode pump are respectively connected with the secondary battery pile and the secondary battery positive electrode electrolyte barrel through pipelines;
The secondary battery positive electrode electrolyte barrel is respectively connected with the secondary battery pile and the secondary battery positive electrode pump through pipelines;
Two ends of the secondary battery cathode pump are respectively connected with the secondary battery pile and the secondary battery cathode electrolyte barrel through pipelines;
And the secondary battery cathode electrolyte barrel is connected with the secondary battery pile, the secondary battery cathode pump and the adjustment detection system through pipelines respectively.
Preferably, the adjustment detection system comprises at least: a multi-channel valve, an ultraviolet absorption detector, a standard electrolyte barrel, an electrolyte distributing pump and a waste liquid barrel;
The multi-channel valve is respectively connected with the primary battery positive electrolyte barrel, the primary battery negative electrolyte barrel, the secondary battery negative electrolyte barrel, the ultraviolet absorption detector, the standard electrolyte barrel, the electrolyte distribution pump and the waste liquid barrel through pipelines;
the ultraviolet absorption detector is connected with the multichannel valve through a pipeline;
The standard electrolyte barrel is connected with the multi-channel valve through a pipeline;
the electrolyte distribution pump is connected with the multichannel valve through a pipeline;
The waste liquid barrel is connected with the multi-channel valve through a pipeline.
The invention has the beneficial effects that:
1. According to the invention, the collocation of the concentration and the volume of the positive and negative electrolyte is optimally regulated, so that the stable state of the electrolyte under different working conditions is detected, and the total quantity of vanadium ions shuttled by vanadium ion shuttles in different valence states, osmotic pressure difference and hydraulic pressure difference in the state is dynamically balanced, so that the capacity attenuation speed is slowed down.
2. The invention can rapidly and accurately detect the stable state parameters of the positive and negative electrolyte under different working conditions, provides guidance for developing the high-stability electrolyte formula, shortens the development period, reduces the development workload, improves the development efficiency and saves the resources.
Drawings
FIG. 1 is a flow chart of a method for detecting the electrolyte stability of an all-vanadium redox flow battery according to the present invention;
fig. 2 is a schematic diagram of an electrolyte steady state detection system of an all-vanadium redox flow battery of the present invention.
1. A primary cell stack; 2. a primary battery positive electrode pump; 3. a primary battery negative electrode pump; 4. an anode electrolyte barrel of the primary battery; 5. a first-stage battery negative electrode electrolyte barrel; 6. a primary battery positive electrolyte level detector; 7. a primary battery negative electrolyte level detector; 8. a multi-channel valve; 9. an ultraviolet absorption detector; 10. a standard electrolyte tank; 11. an electrolyte dispensing pump; 12. a waste liquid barrel; 13. a secondary cell stack; 14. a secondary battery positive electrode pump; 15. a secondary battery negative electrode pump; 16. a secondary battery positive electrode electrolyte barrel; 17. and a secondary battery cathode electrolyte barrel.
Detailed Description
The present invention will be further described in detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Referring to fig. 1, a method for detecting the electrolyte stability of an all-vanadium redox flow battery comprises the following steps:
Step S1: setting working conditions of a primary battery system, and setting a single-core voltage range: 0.6-1.7V, current density: 20-300 mA/cm 2, and initial electrolyte concentration: 1.0-3.0 mol/L of initial electrolyte volume: 0.5-50L of initial electrolyte average valence state: 3.5, operating the primary battery system to perform charge and discharge circulation;
Step S2: after 20 charge-discharge cycles are finished, detecting the concentration and valence state of electrolyte by adopting an ultraviolet absorption detector 9, mixing the electrolyte to be detected with standard electrolyte with known concentration and valence state, enabling the valence state of the mixed electrolyte to be 3.2-3.8, recording the mixing volume ratio, testing the concentration and valence state of the mixed electrolyte, and calculating the concentration and valence state of the electrolyte to be detected, wherein the calculation formula is as follows:
;
;
Wherein: -the concentration of the electrolyte to be measured, -Mixing the concentration of the electrolyte solution,The initial volume of the standard electrolyte solution is chosen,Mixing the volume ratio of the electrolyte to be tested and the standard electrolyte in the electrolyte,-The concentration of the electrolyte to be measured,-Mixing the concentration of the electrolyte solution,-Standard electrolyte initial volume;
Further detecting the positive electrode electrolyte concentration, the positive electrode electrolyte valence state, the negative electrode electrolyte concentration and the negative electrode electrolyte valence state of the primary battery, and detecting the positive electrode electrolyte volume and the negative electrode electrolyte volume by adopting a liquid level sensor;
Step S3: calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte, wherein the calculation formula is as follows:
;
;
;
Wherein: -a rate of change of volume, The volume of the positive electrolyte of the primary battery,The initial volume of the primary battery positive electrolyte,-A rate of change of the concentration,The concentration of the positive electrolyte of the primary battery,The initial concentration of the first-stage battery positive electrolyte,The average valence state of the electrolyte of the primary battery,-The volume of the first-stage battery negative electrode electrolyte,The concentration of the negative electrolyte of the primary battery,The valence state of the positive electrolyte of the primary battery,-The valence state of the first-order battery negative electrode electrolyte;
Step S4: judging the stable state of the electrolyte of the primary battery, and when the volume change rate is less than or equal to 1%, the concentration change rate is less than or equal to 1% and the average valence state are satisfied at the same time When the electrolyte is more than or equal to 3.49 and less than or equal to 3.51, the electrolyte is in a stable state;
Step S5: stopping detection when the primary battery electrolyte is in a stable state; otherwise, electrolyte is regulated, and the regulation steps are as follows:
step S51: determining initial barrel, target barrel, and volume of electrolyte transfer
;
Wherein: -electrolyte transfer volume;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery anode electrolyte barrel 4, and the target barrel is a first-stage battery cathode electrolyte barrel 5;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery cathode electrolyte barrel 5, and the target barrel is a first-stage battery anode electrolyte barrel 4;
Step S52: electrolyte is transferred, and electrolyte with the volume of father V is extracted from an electrolyte transferring initial barrel and is sent into a secondary battery cathode electrolyte barrel 17;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows:
Wherein: -a charge level of the electric power, -Number of secondary cell stack cores;
step S54: after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel 17 into an electrolyte transfer target barrel;
Iterative steps S1-S4 after adjustment;
step S6: recording the volume of the positive electrode electrolyte, the concentration of the positive electrode electrolyte, the valence state of the positive electrode electrolyte, the volume of the negative electrode electrolyte, the concentration of the negative electrode electrolyte and the valence state of the negative electrode electrolyte of the primary battery system in a stable state, and ending the test.
Example 1: referring to fig. 2, an electrolyte steady state detection system of an all-vanadium redox flow battery comprises: the system comprises a primary battery system, a secondary battery system and an adjustment detection system. Connecting the primary battery pile 1 with a primary battery positive electrode pump 2 and a primary battery positive electrode electrolyte barrel 4 by adopting a PE pipeline to form a positive electrode electrolyte loop; the primary battery pile 1 is connected with the primary battery cathode pump 3 and the primary battery cathode electrolyte barrel 5 by adopting PE pipelines to form a cathode electrolyte loop; the primary battery positive electrolyte liquid level detector 6 and the primary battery negative electrolyte liquid level detector 7 are respectively arranged at a position 10cm above the liquid level in the primary battery positive electrolyte barrel 4 and the primary battery negative electrolyte barrel 5; the multi-channel valve 8 is respectively connected with the first-stage battery positive electrode electrolyte barrel 4, the first-stage battery negative electrode electrolyte barrel 5, the ultraviolet absorption detector 9, the standard electrolyte barrel 10, the electrolyte distribution pump 11, the waste liquid barrel 12 and the second-stage battery negative electrode electrolyte barrel 17 by adopting PE pipelines, the electrolyte distribution pump 11 pumps and injects electrolyte, and the multi-channel valve 8 controls the start and stop of each channel to realize the in and out of the electrolyte among all the components; the number of the electric cores of the secondary battery stack 13 is 5, and the secondary battery stack 13 is connected with a secondary battery positive electrode pump 14 and a secondary battery positive electrode electrolyte barrel 16 by adopting PE pipelines to form a positive electrode electrolyte loop; the secondary battery stack 13 is connected with the secondary battery cathode pump 15 and the secondary battery cathode electrolyte barrel 17 by PE pipelines to form a cathode electrolyte loop.
Step S1: the first-stage battery positive electrode electrolyte barrel 4 and the first-stage battery negative electrode electrolyte barrel 5 are respectively internally provided with 0.5L of 1.7mol/L vanadium electrolyte, the initial average valence state is 3.5, the set current density is 100mA/cm 2, the single-core voltage range is 0.6-1.7V, and a first-stage battery system is operated to start testing.
Step S2: after 20 charge-discharge cycles are finished, collecting the volume, concentration and valence state of positive and negative electrolyte of the primary battery, wherein the volume of positive electrolyte of the primary battery is 0.566L, the volume of negative electrolyte of the primary battery is 0.434L, the concentration of positive electrolyte is 1.814mol/L, the valence state of positive electrolyte is 3.87, the concentration of negative electrolyte is 1.551mol/L and the valence state of negative electrolyte is 3.00;
step S3: calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte,
;
;
；
Step S4: judging the stable state of the electrolyte of the primary battery,；
Step S5: electrolyte is regulated, and the steps S1-S4 are iterated after regulation;
Step S51: determining an initial barrel, a target barrel, and a volume of electrolyte transfer:
；
The electrolyte transferring initial barrel is a first-stage battery positive electrode electrolyte barrel 4, the electrolyte transferring target barrel is a first-stage battery negative electrode electrolyte barrel 5, and the volume is 0.097L;
Step S52: electrolyte is transferred, and electrolyte with the volume of 0.097L is extracted from an initial electrolyte transferring barrel and is sent into a secondary battery cathode electrolyte barrel 17;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows:
step S54: after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel 17 into an electrolyte transfer target barrel;
iterating step S1-step S4.
For the first iteration, the volume of the positive electrode electrolyte of the primary battery is 0.513L, the volume of the negative electrode electrolyte of the primary battery is 0.487L, the concentration of the positive electrode electrolyte is 1.897mol/L, the valence state of the positive electrode electrolyte is 3.87, the concentration of the negative electrode electrolyte is 1.492mol/L and the valence state of the negative electrode electrolyte is 3.05. Calculated to obtainContinuing to iterate the steps S1-S4 if the stable state judgment condition is not met;
The second iteration, the first-stage battery positive electrode electrolyte volume is 0.467L, the negative electrode electrolyte volume is 0.533L, the positive electrode electrolyte concentration 1.934mol/L, the positive electrode electrolyte valence state is 3.88, the negative electrode electrolyte concentration is 1.495mol/L and the negative electrode electrolyte valence state is 3.10. Calculated to obtain Continuing to iterate the steps S1-S4 if the stable state judgment condition is not met;
The third iteration, the positive electrode electrolyte volume of the primary battery is 0.459L, the negative electrode electrolyte volume is 0.541L, the positive electrode electrolyte concentration is 1.963mol/L, the positive electrode electrolyte valence state is 3.91, the negative electrode electrolyte concentration is 1.477mol/L and the negative electrode electrolyte valence state is 3.06. Calculated to obtain Continuing to iterate the steps S1-S4 if the stable state judgment condition is not met;
The fourth iteration, the primary battery positive electrode electrolyte volume is 0.442L, the negative electrode electrolyte volume is 0.558L, the positive electrode electrolyte concentration is 1.978mol/L, the positive electrode electrolyte valence state is 3.91, the negative electrode electrolyte concentration is 1.480mol/L and the negative electrode electrolyte valence state is 3.08. Calculated to obtain Continuing to iterate the steps S1-S4 if the stable state judgment condition is not met;
The fifth iteration, the primary battery positive electrode electrolyte volume is 0.431L, the negative electrode electrolyte volume is 0.569L, the positive electrode electrolyte concentration 1.980mol/L, the positive electrode electrolyte valence state is 3.93, the negative electrode electrolyte concentration 1.488mol/L and the negative electrode electrolyte valence state is 3.08. Calculated to obtain The iteration is stopped when the steady state judgment condition is met;
Step S6: recording steady state parameters: and (3) the volume of the positive electrolyte, the concentration of the positive electrolyte, the valence state of the positive electrolyte, the volume of the negative electrolyte, the concentration of the negative electrolyte and the valence state of the negative electrolyte are finished.
Example 2: the test system uses the same connection as in example 1.
Step S1: the primary battery positive electrode electrolyte barrel 4 and the primary battery negative electrode electrolyte barrel 5 are respectively internally provided with 1.0mol/L vanadium electrolyte 3L, the initial average valence state is 3.5, the current density is set to be 20mA/cm 2, and the single-core voltage range is 0.6-1.7V. Operating the primary battery system and starting a test;
Step S2: after 20 charge-discharge cycles are finished, collecting the volume, concentration and valence state of positive and negative electrolyte of the primary battery, wherein the volume of positive electrolyte of the primary battery is 3.893L, the volume of negative electrolyte of the primary battery is 2.107L, the concentration of positive electrolyte is 1.053mol/L, the valence state of positive electrolyte is 3.80, the concentration of negative electrolyte is 0.902mol/L and the valence state of negative electrolyte is 3.05;
Step S3: calculating the volume change rate of the electrolyte Rate of change of concentrationAverage valence state，；
Step S4: judging the stable state of the electrolyte of the primary battery,；
Step S5: electrolyte is regulated, and the steps S1-S4 are iterated after regulation;
Step S51: determining an initial barrel, a target barrel, and a volume of electrolyte transfer:
；
；
the electrolyte transferring initial barrel is a first-stage battery anode electrolyte barrel 4, the electrolyte transferring target barrel is a first-stage battery cathode electrolyte barrel 5, and the volume is 1.044L;
Step S52: electrolyte is transferred, and the electrolyte with the volume of 1.044L is extracted from an initial electrolyte transferring barrel and is sent into a secondary battery cathode electrolyte barrel 17;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows: ；
step S54: after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel 17 into an electrolyte transfer target barrel;
Iterating the step S1 to the step S4;
After 7 iterations of the process,
，
Conforming to a steady state judgment condition, and stopping iteration;
Step S6: recording steady state parameters: and (3) the volume of the positive electrolyte, the concentration of the positive electrolyte, the valence state of the positive electrolyte, the volume of the negative electrolyte, the concentration of the negative electrolyte and the valence state of the negative electrolyte are finished.
Example 3: the test system uses the same connection as in example 1.
Step S1: 2.0mol/L vanadium electrolyte 30L is respectively filled in the first-stage battery positive electrode electrolyte barrel 4 and the first-stage battery negative electrode electrolyte barrel 5, the initial average valence state is 3.5, the current density is set to be 200mA/cm 2, the single-core voltage range is 0.6-1.7V, a first-stage battery system is operated, and the test is started;
Step S2: after 20 charge-discharge cycles are finished, collecting the volume, concentration and valence state of positive and negative electrolyte of the primary battery, wherein the volume of positive electrolyte of the primary battery is 30.43L, the volume of negative electrolyte of the primary battery is 29.57L, the concentration of positive electrolyte is 1.912mol/L, the valence state of positive electrolyte is 4.01, the concentration of negative electrolyte is 2.091mol/L and the valence state of negative electrolyte is 3.04;
Step S3: calculated to obtain
；
Step S4: judging the stable state of the electrolyte of the primary battery,
；
Step S5: electrolyte is regulated, and the steps S1-S4 are iterated after regulation;
Step S51: determining an initial barrel, a target barrel, and a volume of electrolyte transfer:
；
；
the electrolyte transferring initial barrel is a first-stage battery cathode electrolyte barrel 5, the electrolyte transferring target barrel is a first-stage battery anode electrolyte barrel 4, and the volume is 0.870L;
Step S52: electrolyte is transferred, and electrolyte with the volume of 0.870L is extracted from an initial electrolyte transferring barrel and is sent into a secondary battery cathode electrolyte barrel 17;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows: ；
step S54: after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel 17 into an electrolyte transfer target barrel;
Iterating the step S1 to the step S4;
After 3 iterations of the process,
，
Conforming to a steady state judgment condition, and stopping iteration;
Step S6: recording steady state parameters: and (3) the volume of the positive electrolyte, the concentration of the positive electrolyte, the valence state of the positive electrolyte, the volume of the negative electrolyte, the concentration of the negative electrolyte and the valence state of the negative electrolyte are finished.
Example 4: the test system uses the same connection as in example 1.
Step S1: the primary battery positive electrode electrolyte barrel 4 and the primary battery negative electrode electrolyte barrel 5 are respectively provided with 3.0mol/L vanadium electrolyte 50L, the initial average valence state is 3.5, the current density is 300mA/cm 2, the single-core voltage range is 0.6-1.7V, a primary battery system is operated, and the test is started;
Step S2: after 20 charge-discharge cycles are finished, collecting the volume, concentration and valence state of positive and negative electrolyte of the primary battery, wherein the volume of positive electrolyte of the primary battery is 54.35L, the volume of negative electrolyte of the primary battery is 45.65L, the concentration of positive electrolyte is 3.288mol/L, the valence state of positive electrolyte is 3.84, the concentration of negative electrolyte is 2.657mol/L and the valence state of negative electrolyte is 3.07;
step S3: calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte,
；
Step S4: judging the stable state of the electrolyte of the primary battery,
；
Step S5: electrolyte regulation is carried out;
Step S51: determining an initial barrel, a target barrel, and a volume of electrolyte transfer:
；
；
the electrolyte transferring initial barrel is a first-stage battery positive electrode electrolyte barrel 4, the electrolyte transferring target barrel is a first-stage battery negative electrode electrolyte barrel 5, and the volume is ；
Step S52: electrolyte is transferred, and electrolyte with the volume of 8.73L is extracted from an initial electrolyte transferring barrel and is sent into a secondary battery cathode electrolyte barrel 17;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows: ；
step S54: after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel 17 into an electrolyte transfer target barrel;
Iterating the step S1 to the step S4;
After 5 iterations of the process,
，
Conforming to a steady state judgment condition, and stopping iteration;
Step S6: recording steady state parameters: and (3) the volume of the positive electrolyte, the concentration of the positive electrolyte, the valence state of the positive electrolyte, the volume of the negative electrolyte, the concentration of the negative electrolyte and the valence state of the negative electrolyte are finished.
Comparative example 1: adopts a conventional positive and negative electrolyte scheme: the volume and concentration are the same, and the valence state is 3.5.
Comparative example 2: adopts a conventional positive and negative electrolyte scheme: the volume and the concentration are the same, the positive electrode valence state is 4, and the negative electrode valence state is 3.
The positive and negative electrolytes prepared according to the positive and negative electrolyte parameter schemes detected in examples 1 to 4 were respectively subjected to charge and discharge tests under the conditions of examples 1 to 4 with the electrolytes of comparative examples 1 to 2, and the capacity retention rates after the 2 nd, 20 th, 50 th, 100 th and 200 th cycles were recorded, respectively, and the results are shown in table 1:
TABLE 1 electrolyte charge and discharge test results
As can be seen from table 1, the capacity retention rates of the 20 th cycle, the 50 th cycle, the 100 th cycle and the 200 th cycle show that the capacity fade rate of examples 1 to 4 is significantly lower than that of comparative examples 1 to 2, mainly due to the difference in volume between the positive and negative electrolytes in a stable state, the difference in liquid pressure and the difference in concentration caused by the difference in volume can affect the net shuttle amount of the diffusion of the positive and negative vanadium ions and water molecules across the membrane, thereby slowing down the rate of the capacity fade of the battery. Therefore, the invention detects the stable state of the electrolyte under different working conditions by optimally adjusting the concentration and volume of the positive and negative electrolytes, and the shuttle speed of vanadium ions in different valence states, the osmotic pressure difference and the total amount of vanadium ions caused by hydraulic pressure difference between the positive and negative electrolytes in the state realize dynamic balance, thereby slowing down the capacity attenuation speed; meanwhile, the invention can rapidly and accurately detect the stable state parameters of the positive and negative electrolyte under different working conditions, provides guidance for developing a customized electrolyte formula, shortens the development period, reduces the development workload, improves the development success rate and saves resources.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The method for detecting the steady state of the electrolyte of the all-vanadium redox flow battery is characterized by comprising the following steps of:
step S1: operating a primary battery system to perform charge and discharge cycles;
step S2: collecting positive electrolyte volume, negative electrolyte volume, positive electrolyte concentration, negative electrolyte concentration, positive electrolyte valence state and negative electrolyte valence state data of the primary battery after 20 charge-discharge cycles are finished;
Step S3: calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte of the primary battery;
step S4: judging the stable state of the electrolyte of the primary battery;
Step S5: stopping detection when the primary battery electrolyte is in a stable state; otherwise, electrolyte is adjusted, and the steps S1-S4 are iterated after adjustment;
Step S6: and recording the steady state parameters, and ending the test.
2. The method for detecting the stable state of the electrolyte of the all-vanadium redox flow battery according to claim 1, wherein the working conditions of the charge-discharge cycle in the step S1 are as follows: the voltage range of the single cell is 0.6-1.7V, the current density is 20-300 mA/cm 2, the initial electrolyte concentration is 1.0-3.0 mol/L, and the average valence state of the initial electrolyte is 3.5.
3. The method for detecting the steady state of the electrolyte of the all-vanadium redox flow battery according to claim 1, wherein the calculation formula for calculating the volume change rate, the concentration change rate and the average valence state of the electrolyte of the primary battery in the step S3 is as follows:
;
;
;
Wherein: -a rate of change of volume, The volume of the positive electrolyte of the primary battery,The initial volume of the primary battery positive electrolyte,-A rate of change of the concentration,The concentration of the positive electrolyte of the primary battery,The initial concentration of the first-stage battery positive electrolyte,The average valence state of the electrolyte of the primary battery,-The volume of the first-stage battery negative electrode electrolyte,The concentration of the negative electrolyte of the primary battery,The valence state of the positive electrolyte of the primary battery,-The valence state of the negative electrolyte of the primary battery.
4. The method for detecting the stable state of the electrolyte of the all-vanadium redox flow battery according to claim 1, wherein the judging method for judging the stable state of the electrolyte of the primary battery in the step S4 is as follows: when the volume change rate is 1% or less, the concentration change rate is 1% or less, and the average valence state is 3.49 or more and 3.51 or less, the electrolyte is in a stable state.
5. The method for detecting the stable state of the electrolyte of the all-vanadium redox flow battery according to claim 1, wherein the step of adjusting the electrolyte in the step S5 is:
step S51: determining initial barrel, target barrel, and volume of electrolyte transfer
;
Wherein: -electrolyte transfer volume;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery positive electrolyte barrel, and the electrolyte transfer target barrel is a first-stage battery negative electrolyte barrel;
When (when) When the electrolyte is transferred, the initial barrel is a first-stage battery cathode electrolyte barrel, and the electrolyte transfer target barrel is a first-stage battery anode electrolyte barrel;
step S52: electrolyte transfer is carried out, and the volume extracted from the initial barrel for electrolyte transfer is The electrolyte of the electrolyte is fed into a secondary battery cathode electrolyte barrel;
Step S53: and (3) operating the secondary battery system to charge, wherein the charge electric quantity is as follows:
;
Wherein: -a charge level of the electric power, -Number of secondary cell stack cores;
step S54: and after the charging is finished, extracting the electrolyte in the secondary battery cathode electrolyte barrel into the electrolyte transfer target barrel.
6. The method for detecting the steady state of the electrolyte of the all-vanadium redox flow battery according to claim 1, wherein the steady state parameters in the step S6 are: the volume of the positive electrode electrolyte, the concentration of the positive electrode electrolyte, the valence state of the positive electrode electrolyte, the volume of the negative electrode electrolyte, the concentration of the negative electrode electrolyte and the valence state of the negative electrode electrolyte of the primary battery.
7. A system for implementing the all-vanadium redox flow battery electrolyte steady state detection method of any one of claims 1-6, comprising: the system comprises a primary battery system, a secondary battery system and an adjustment detection system, wherein the adjustment detection system is connected with the primary battery system and the secondary battery system through pipelines respectively.
8. The system of claim 7, wherein the primary battery system comprises at least: a primary battery stack, a primary battery positive electrode pump, a primary battery positive electrode electrolyte barrel, a primary battery negative electrode pump and a primary battery negative electrode electrolyte barrel;
The primary battery pile is respectively connected with a primary battery positive electrode pump, a primary battery negative electrode pump, a primary battery positive electrode electrolyte barrel and a primary battery negative electrode electrolyte barrel through pipelines;
Two ends of the primary battery positive electrode pump are respectively connected with the primary battery pile and the primary battery positive electrode electrolyte barrel through pipelines;
The primary battery positive electrode electrolyte barrel is respectively connected with the primary battery pile, the primary battery positive electrode pump and the adjustment detection system through pipelines; a primary battery positive electrolyte level detector is arranged in the primary battery positive electrolyte barrel;
Two ends of the primary battery cathode pump are respectively connected with the primary battery pile and the primary battery cathode electrolyte barrel through pipelines;
The primary battery cathode electrolyte barrel is respectively connected with the primary battery pile, the primary battery cathode pump and the adjustment detection system through pipelines; and a primary battery negative electrolyte liquid level detector is arranged in the primary battery negative electrolyte barrel.
9. The system of claim 8, wherein the secondary battery system comprises at least: a secondary battery stack, a secondary battery positive electrode pump, a secondary battery positive electrode electrolyte barrel, a secondary battery negative electrode pump and a secondary battery negative electrode electrolyte barrel;
The secondary battery pile is respectively connected with the secondary battery positive electrode pump, the secondary battery negative electrode pump, the secondary battery positive electrode electrolyte barrel and the secondary battery negative electrode electrolyte barrel through pipelines;
Two ends of the secondary battery positive electrode pump are respectively connected with the secondary battery pile and the secondary battery positive electrode electrolyte barrel through pipelines;
The secondary battery positive electrode electrolyte barrel is respectively connected with the secondary battery pile and the secondary battery positive electrode pump through pipelines;
Two ends of the secondary battery cathode pump are respectively connected with the secondary battery pile and the secondary battery cathode electrolyte barrel through pipelines;
And the secondary battery cathode electrolyte barrel is connected with the secondary battery pile, the secondary battery cathode pump and the adjustment detection system through pipelines respectively.
10. The system of claim 9, wherein the regulation detection system comprises at least: a multi-channel valve, an ultraviolet absorption detector, a standard electrolyte barrel, an electrolyte distributing pump and a waste liquid barrel;
The multi-channel valve is respectively connected with the primary battery positive electrolyte barrel, the primary battery negative electrolyte barrel, the secondary battery negative electrolyte barrel, the ultraviolet absorption detector, the standard electrolyte barrel, the electrolyte distribution pump and the waste liquid barrel through pipelines;
the ultraviolet absorption detector is connected with the multichannel valve through a pipeline;
The standard electrolyte barrel is connected with the multi-channel valve through a pipeline;
the electrolyte distribution pump is connected with the multichannel valve through a pipeline;
The waste liquid barrel is connected with the multi-channel valve through a pipeline.
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