CN101609128B - Method for testing comprehensive valence of electrolyte of vanadium redox battery and device therefor - Google Patents
Method for testing comprehensive valence of electrolyte of vanadium redox battery and device therefor Download PDFInfo
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- CN101609128B CN101609128B CN2009100895275A CN200910089527A CN101609128B CN 101609128 B CN101609128 B CN 101609128B CN 2009100895275 A CN2009100895275 A CN 2009100895275A CN 200910089527 A CN200910089527 A CN 200910089527A CN 101609128 B CN101609128 B CN 101609128B
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Abstract
The invention discloses a method for testing comprehensive valence of electrolyte of a vanadium redox battery, comprising the steps: a) acquiring the mutation time of electric potential of the electrolyte of the vanadium redox battery, and the mutation time including first mutation time t1 of the electric potential of positive pole electrolyte and second mutation time t2 of the electric potential of negative pole electrolyte; b) obtaining the comprehensive valence a of the electrolyte according to the formula I*(FMV/nI)= (t2-t1)/(2a-7) by utilizing the first mutation time t1 and the second mutation time t2; wherein a is the comprehensive valence of the electrolyte, M is total vanadium concentration of the electrolyte with the unit of mol/L, V is the canning volume of the electrolyte with the unit of L, n is the number of single batteries of the vanadium redox battery, I is the charging current of the vanadium redox battery with the unit of A, and F is Faraday constant. According to the method, the comprehensive valence of the electrolyte of the vanadium redox battery can accurately tested in an online way.
Description
Technical field
The present invention relates to vanadium cell, be specifically related to test the method and apparatus of comprehensive valence state of the electrolytic solution of vanadium cell.
Background technology
Vanadium cell, its full name are vanadium redox battery (Vanadium RedoxBattery is abbreviated as VRB).As a kind of environmental protection accumulator, the manufacturing of vanadium cell, use and discarded process does not all produce objectionable impurities.Because the vanadium cell charging rapidly, energy transformation ratio is high, can prepare the MW class electric battery, and electric energy can high-powerly be provided for a long time, and therefore important use is all arranged in a lot of fields.
The preparation process of typical vanadium cell may further comprise the steps: earlier vanadic sulfate (IV), vanadic sulfate (III), sulfuric acid and water are mixed with V electrolyte in proportion, then electrolytic solution and suitable electrode material, conducting membrane material, battery container, electrolytic solution storage tank and electrolyte delivery system are formed vanadium cell jointly.The typical electrolytic solution that in vanadium cell, uses contains the potpourri that 50% state of oxidation is formed for+4 vanadium ion for+3 vanadium ion and 50% state of oxidation, and this electrolytic solution is divided into two equal parts usually as anodal electrolytic solution and negative pole electrolytic solution.The comprehensive valence state of term electrolytic solution is meant the mean value of the valence state of all vanadium ions in the electrolyte of vanadium redox battery, and the comprehensive valence state of typical vanadium cell electrolysis is 3.5 valencys.
In the vanadium cell operational process, in positive pole, the negative pole generation electron exchange of vanadium cell, the anodal valence state of electrolytic solution or negative pole valence state are along with the time changes, and the comprehensive valence state of electrolytic solution is constant in theory, remains 3.5 valencys.Yet the vanadium cell of actual motion can the situation that comprehensive valence state departs from 3.5 valencys may occur when long-play.For example, when take place to reveal on vanadium cell liquid road, the vanadium ion of the oxygen of air has got into liquid road rear oxidation divalent or 3 valencys can make the comprehensive valence state of electrolytic solution be higher than 3.5 valencys, and this moment, the balance of electrolytic solution was destroyed, and influenced the usability of vanadium cell.Therefore, when vanadium cell moves, need in time to grasp the situation of change of the comprehensive valence state of electrolyte of vanadium redox battery.
U.S. Pat 20050164075 disclosed technology are to utilize the theory of the state consistency of electrolyte of vanadium redox battery in each Battery pack; Beyond power supply vanadium cell heap; Increase by one group and be specifically designed to the battery that detects vanadium cell open-circuit voltage (OCV); Let electrolytic solution flow through vanadium cell heap and test battery simultaneously, the open-circuit voltage that obtains through test battery is judged the state-of-charge (SOC) of electrolyte of vanadium redox battery.
The disclosed technology of Chinese patent CN1502141A is the production of electrolytic solution, has wherein mentioned the technology of recovering electrolyte balance, and the technology of recovering electrolyte balance is with asymmetric electrolytic tank, consumable anode, the electrolytic solution electrolytic reduction in the negative electrode is arrived the valence state that needs.
In the prior art; The method of measuring the comprehensive valence state of vanadium cell generally is employed in vanadium cell and can takes a sample and adopt potentiometric titration to measure then; Yet this sampling method can not satisfy the requirement of vanadium cell being carried out online detection, and sampling also can accelerate to destroy the balance of electrolyte of vanadium redox battery.
Therefore, need a kind ofly can be timely and accurately the comprehensive valence state of electrolyte of vanadium redox battery to be carried out on-line detection method.
Summary of the invention
The technical matters that the present invention solves is to provide a kind of method and apparatus that timely and accurately the comprehensive valence state of electrolyte of vanadium redox battery is carried out on-line testing.
For solving the problems of the technologies described above, the present invention provides the method for testing of the comprehensive valence state of a kind of electrolyte of vanadium redox battery, comprises step:
A) mutation time of the electrolytic solution current potential of acquisition vanadium cell, said mutation time comprises first mutation time t1 of anodal electrolytic solution current potential and the second mutation time t2 of negative pole electrolytic solution current potential;
B) utilize the said first mutation time t1 and the second mutation time t2 to obtain the comprehensive valence state a of electrolytic solution according to formula I:
Among the formula I: a is the comprehensive valence state of electrolytic solution; M is the electrolytic solution total V density, and unit is mol/L; V is the canned volume of electrolytic solution, and unit is L; N is the monocell number of vanadium cell, and unit is individual; I is the charging current of vanadium cell, and unit is A; F is a Faraday constant.
Preferably, the mutation time of said battery electrolyte current potential be the vanadium cell initial charge or when recharging behind the deep discharge mutation time of the current potential of electrolytic solution.
Preferably, also comprise step before the step a):
Measure the cycle potentials of electrolyte of vanadium redox battery;
Preferably, the mutation time of the electrolytic solution current potential of the vanadium cell of test described in the step a) is specially:
A1) gather the electrolyte of vanadium redox battery potential data;
A2) obtain the mutation time of electrolyte of vanadium redox battery current potential according to said potential data.
If said cycle potentials value and standard electric place value produce deviation, vanadium cell is carried out recharging behind the deep discharge.
The present invention also provides a kind of potential testing device that in the described method of testing of above arbitrary technical scheme, uses, and comprises first electrode pair, first pot that is connected with said first electrode pair that are connected on the anodal electrolytic solution of vanadium cell, is connected second electrode pair on the vanadium redox battery negative pole electrolyte, second pot that is connected with said second electrode pair.
Preferably, said first electrode pair and second electrode pair are the electrode pair of mereurous sulfate contrast electrode and platinum electrode composition.
The present invention provides the method for testing of the comprehensive valence state of a kind of electrolyte of vanadium redox battery.According to method provided by the invention, measure the mutation time of anodal electrolytic solution and negative pole electrolytic solution earlier, can confirm the comprehensive valence state of electrolytic solution according to the mutation time difference of this positive pole electrolytic solution current potential and negative pole electrolytic solution current potential then.Compared with prior art, method provided by the invention can not influence under the normal situation about using of vanadium cell, and the comprehensive valence state of online definite vanadium cell is confirmed the equilibrium state of electrolyte of vanadium redox battery, thereby determines vanadium cell is carried out electrolysis or other processing.
In a kind of preferred scheme; Method provided by the invention is tested the cycle potentials of vanadium cell earlier; If cycle potentials value and standard electric place value produce deviation, explain that then electrolyte balance is destroyed, carry out deep discharge to vanadium cell and recharge this moment; The comprehensive valence state of on-line measurement electrolyte of vanadium redox battery then is to carry out electrolysis or other processing to vanadium cell.
Description of drawings
Fig. 1 is vanadium cell provided by the invention and potential testing device syndeton synoptic diagram;
Fig. 2 is a potential test device synoptic diagram provided by the invention;
Current potential-time plot that the vanadium cell that Fig. 3 a records for the present invention records when passing through initial charge;
Current potential-time plot during normal charge and discharge of vanadium cell that Fig. 3 b records for the present invention;
Current potential-time plot that the vanadium cell that Fig. 3 c records for the present invention records when recharging through deep discharge.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
See also Fig. 1, be vanadium cell of the present invention, potential testing device syndeton synoptic diagram.The vanadium cell group comprises that number is a n monocell, and n wherein gets positive integer, and for the size of n, the present invention does not have special restriction.
This vanadium cell group also comprises the negative pole jar R1 and anodal jar R2 that electrolytic solution is provided to vanadium cell; Negative pole jar R1 is communicated with through negative pole pipeline L1 with the negative pole of a said n monocell, and the negative pole pipeline is provided with the first ebullator P1 of circular electrolyte and measures the first potential test device C1 of negative pole electrolytic solution current potential; Anodal jar R2 is communicated with through anodal pipeline L2 with the positive pole of the monocell of said n parallel connection, and anodal pipeline is provided with the second ebullator P2 of circular electrolyte and measures the second potential test device C2 of anodal electrolytic solution current potential.
Two potential test device C1, C2 have identical structure.Please be potential testing device structural representation provided by the invention simultaneously referring to Fig. 2.This potential testing device C comprises the electrode pair that is connected among the electrolyte of vanadium redox battery pipeline L, and said electrode pair can be electrode pair that can the potential electrode current potential well known to those skilled in the art, is preferably mereurous sulfate and platinum electrode is right.
In this embodiment; Electrode pair among the potential testing device C is made up of a mereurous sulfate contrast electrode 11a and a platinum electrode 11b; Mereurous sulfate contrast electrode 11a and platinum electrode 11b are provided with the sealing plug 12 that is used for fixing electrode pair, and the other end of mereurous sulfate contrast electrode 11a and platinum electrode 11b is connected with negative pole with the positive pole of ORP (redox) potential test appearance 13 respectively.Wherein, can to select concentration be the sulfuric acid solution of 0.1mol/L～7mol/L to the conducting solution of mereurous sulfate contrast electrode.
After vanadium cell circulation normal operation a period of time; Because the generation of situation such as long-time use of battery or gas leakage inevitably can cause the comprehensive valence state of electrolytic solution to change, and promptly departs from 3.5 original valencys; The electrolyte of vanadium redox battery valence state possibly be higher than 3.5 valencys, also possibly be lower than 3.5 valencys.Therefore the present invention carries out electrolysis comprehensive valence state is returned to the electrolytic solution valence state adjusting gear of 3.5 valencys to it also providing on the vanadium cell when the comprehensive valence state of electrolytic solution departs from 3.5 valencys.
According to the present invention, be assembled into vanadium cell behind the preparation electrolyte of vanadium redox battery, this moment, the comprehensive valence state of electrolyte of vanadium redox battery was 3.5 valencys, vanadium cell voltage is 0 volt basically.When vanadium cell is carried out first charge and discharge; Be connected the first anodal potential testing device C1 of vanadium cell and the second potential testing device C2 that is connected the vanadium cell negative pole potential data through computer acquisition positive and negative electrode electrolytic solution respectively; Obtain the positive and negative electrode potential curve; And this curve mapped to the time, obtain first mutation time t1 of anodal current potential and the second mutation time t2 of negative pole current potential respectively.The monocell that the potential jump time according to the invention is meant vanadium cell voltage during less than the situation of 0.5V when charging to WV, the bust time of the time that jumps of anodal electrolytic solution current potential or negative pole electrolytic solution current potential.
The first mutation time t1 and the second mutation time t2 substitution formula I are obtained the comprehensive valence state a of electrolytic solution:
Among the formula I: a is the comprehensive valence state of electrolytic solution; M is the electrolytic solution total V density, and unit can be mol/L; V is the canned volume of electrolytic solution, and unit can be for rising L; N is the monocell number of vanadium cell, and unit can be for individual; I is the charging current of vanadium cell, and unit can be ampere (A); F is a Faraday constant, and this Faraday constant F can get 26.8 ampere-hours; The unit of the first mutation time t1 and the second mutation time t2 can for hour.Because when vanadium cell discharged for the first time, first mutation time and second mutation time were equal basically, so the comprehensive valence state of vanadium cell is 3.5 valencys basically.
After the vanadium cell primary charging; Vanadium cell gets into the cycle charge discharge electric process; This moment, the first potential testing device C1 and the second potential testing device C2 noted the potential curve of positive electrode electrolytic solution and the cycle potentials curve of negative electrode electrolytic solution respectively, and this curve was mapped to the time.When battery has just circulated charge and discharge, can think that the electrolyte of vanadium redox battery valence state does not change, still be 3.5 valencys.Therefore get before the above-mentioned vanadium cell positive and negative electrode current potential in a charge and discharge cycle of cycle potentials curve several times as the standard value of positive and negative electrode current potential SOC (State of charge state-of-charge) tabulation, should show as criteria table to vanadium cell.
When vanadium cell carries out normal charge and discharge, utilize the interval to remain between 10%～90% SOC, promptly the electrolytic solution utilization factor is 80%.Battery because service condition like the generation of situation such as gas leakage, behind the oxygen entering liquid-way system, can make the vanadium ion valence state in the electrolytic solution change, causes the comprehensive valence state of electrolytic solution to depart from 3.5 valencys through after repeatedly recycling, and destroys the balance of electrolytic solution.Because two potential testing device C1, C2 can continue to write down circulate electrolyte current potential situation; Therefore this cycle potentials and criteria table are compared; Depart from the standard value of the cycle potentials in the form if find cycle potentials; Think that then electrolyte balance is destroyed, the comprehensive valence state of electrolytic solution has departed from 3.5 valencys.For example the minimum value of negative pole current potential and the standard value of negative pole potential minimum are compared, compare with the maximal value and the peaked standard value of anodal current potential of anodal current potential simultaneously.If the minimum value of negative pole current potential is greater than the standard value of the minimum value of negative pole current potential; And the maximal value of anodal current potential approximates the peaked standard value of anodal current potential; Explain that electrolyte balance destroys; And the comprehensive valence state that is electrolytic solution is lower than 3.5 valencys, and this moment, the SOC of vanadium cell will judge with anodal electrolytic solution current potential.If the minimum value of negative pole current potential approximates the standard value of negative pole potential minimum; And the maximal value of anodal current potential is less than the peaked standard value of anodal current potential; Explain that electrolyte balance destroys; And the comprehensive valence state that is electrolytic solution is higher than 3.5 valencys, and this moment, the SOC of vanadium cell will use negative pole electrolytic solution current potential to judge.
After confirming that through comparison cycle potentials and criteria table electrolyte balance is destroyed, vanadium cell is carried out deep discharge recharge, and write down the positive and negative electrode current potential, make potential curve.When vanadium cell is carried out deep discharge, can be with voltage deep discharge to the single battery voltage of monocell less than 1V, preferred, with voltage deep discharge to the single battery voltage of monocell less than 0.5V.
Vanadium cell passes through deep discharge, when recharging, writes down first mutation time t1 of anodal electrolytic solution current potential and the second mutation time t2 of negative pole electrolytic solution current potential, and first mutation time and the second mutation time substitution formula I are obtained the comprehensive valence state a of electrolytic solution.
The vanadium cell heap that adopts 5 monocell to form, electrode area 250cm
2, vanadium concentration is 1.5mol/L in the electrolytic solution, sulfate concentration 4mol/L in the electrolytic solution, and the valence state of chemically examining electrolytic solution with potentiometric titration is 3.5 valencys, the electrolytic solution volume is 6L altogether, the canned 3L electrolytic solution of anodal liquid storage, the canned 3L electrolytic solution of negative pole liquid storage.
With the sulfuric acid solution of canned 4mol/L in the mereurous sulfate contrast electrode, be assembled into electrode pair with the platinum electrode of 0.2mm diameter, and be connected on the potential test appearance, the potential test instrument is installed on the vanadium cell flow pipeline according to shown in Figure 2 according to assembling shown in Figure 1.
Close first valve 1 and second valve 2, start vanadium cell and carry out first charging, discharge procedures, continuous current 17.5A charging, continuous current 17.5A discharge.After vanadium cell is accomplished a charging, discharge procedures; Adopt the measured potential data of computer recording potential testing device; And with these data and time mapping; Obtain the current potential-time plot shown in Fig. 3 a, the mutation time t1 that test obtains the current potential of anodal electrolytic solution is about 39.8 minutes, and the mutation time t2 that test obtains the current potential of negative pole electrolytic solution is 39.7 minutes; The comprehensive valence state of the electrolytic solution that calculates according to formula I is about 3.5 valencys, conforms to the valence state of potentiometric titration chemical examination electrolytic solution.
After primary charging, discharge procedures were accomplished, vanadium cell was proceeded the charge and discharge that circulate, during cycle charge-discharge; The utilization interval of SOC is remained between the 10%-90%, and being about to the electrolytic solution utilization factor is 80%, simultaneously through the computer recording cycle potentials; To the time mapping, shown in Fig. 3 b.
, vanadium cell during several charge and discharge, can think that electrolyte balance is through destroying before carrying out.Select second charge and discharge process, anodal current potential, negative pole current potential are made table as criteria table to SOC, as shown in table 1:
Table 1SOC and current potential standard value table
Annotate:
*: the current potential that battery records during by overdischarge;
*: the current potential that battery records when overcharging.
Vanadium cell through 1000 circulation charge and discharge after; The maximal value that measures negative pole electrolytic solution current potential is about-890mv; And the maximal value of anodal electrolytic solution current potential is about 510mv; Less than the peaked standard value 546mv of anodal electrolytic solution, promptly the SOC in the criteria table is 90% o'clock the peaked standard value of anodal electrolytic solution.At this moment, can confirm that electrolyte balance has taken place by destruction, and the comprehensive valence state of electrolytic solution is greater than 3.5 valencys.
Stop the charge and discharge process of vanadium cell; With the vanadium cell deep discharge; Deep discharge to vanadium cell voltage charges to vanadium cell behind the deep discharge less than 0.5V again, obtains the current potential-time plot shown in Fig. 3 c; And the mutation time t1 of current potential that test obtains anodal electrolytic solution is 38.5 minutes, and the mutation time t2 of the current potential of negative pole electrolytic solution is 81.5 minutes.With the comprehensive valence state that obtains electrolytic solution among t1 and the t2 substitution formula I is 3.63 valencys.To the electrolyte of vanadium redox battery sampling, the valence state of chemically examining electrolytic solution with potentiometric titration is 3.63 valencys, conforms to the valence state that adopts formula I to calculate.
More than the method for testing and the device of the comprehensive valence state of electrolyte of vanadium redox battery provided by the present invention carried out detailed introduction.Used concrete example among this paper principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (9)
1. the method for testing of the comprehensive valence state of electrolyte of vanadium redox battery comprises step:
A) mutation time of the electrolytic solution current potential of acquisition vanadium cell; The monocell that said mutation time comprises vanadium cell voltage less than the situation of 0.5V under when charging to WV, first mutation time t1 of anodal electrolytic solution current potential and the second mutation time t2 of negative pole electrolytic solution current potential;
B) utilize the said first mutation time t1 and the second mutation time t2 to obtain the comprehensive valence state a of electrolytic solution according to formula I:
Among the formula I: a is the comprehensive valence state of electrolytic solution; M is the electrolytic solution total V density, and unit is mol/L; V is the canned volume of electrolytic solution, and unit is L; N is the monocell number of vanadium cell, and unit is individual; I is the charging current of vanadium cell, and unit is A; F is a Faraday constant.
2. method of testing according to claim 1, the mutation time that it is characterized in that said electrolytic solution current potential be the vanadium cell initial charge or when recharging behind the deep discharge mutation time of electrolytic solution current potential.
3. method of testing according to claim 1 is characterized in that said step a) also comprises step before:
Measure the cycle potentials of electrolyte of vanadium redox battery;
If said cycle potentials value and standard electric place value produce deviation, vanadium cell is carried out recharging behind the deep discharge.
4. according to each described method of testing of claim 1 to 3, it is characterized in that the mutation time that obtains the electrolytic solution current potential of vanadium cell described in the step a) is specially:
A1) gather the electrolyte of vanadium redox battery potential data;
A2) obtain the mutation time of electrolyte of vanadium redox battery current potential according to said potential data.
5. proving installation that is used to test the comprehensive valence state of electrolyte of vanadium redox battery; Comprise first electrode pair, first pot that is connected with said first electrode pair that are connected on the anodal electrolytic solution of vanadium cell, be connected second electrode pair on the vanadium redox battery negative pole electrolyte, with second pot that said second electrode pair is connected, the comprehensive valence state of wherein said test electrolyte of vanadium redox battery comprises step:
A) mutation time of the electrolytic solution current potential of acquisition vanadium cell; The monocell that said mutation time comprises vanadium cell voltage less than the situation of 0.5V under when charging to WV, first mutation time t1 of anodal electrolytic solution current potential and the second mutation time t2 of negative pole electrolytic solution current potential;
B) utilize the said first mutation time t1 and the second mutation time t2 to obtain the comprehensive valence state a of electrolytic solution according to formula I:
Among the formula I: a is the comprehensive valence state of electrolytic solution; M is the electrolytic solution total V density, and unit is mol/L; V is the canned volume of electrolytic solution, and unit is L; N is the monocell number of vanadium cell, and unit is individual; I is the charging current of vanadium cell, and unit is A; F is a Faraday constant.
6. proving installation according to claim 5 is characterized in that said first electrode pair and second electrode pair are the electrode pair of mereurous sulfate contrast electrode and platinum electrode composition.
7. according to claim 5 or 6 described proving installations, the mutation time that it is characterized in that said electrolytic solution current potential be the vanadium cell initial charge or when recharging behind the deep discharge mutation time of electrolytic solution current potential.
8. according to claim 5 or 6 described proving installations, it is characterized in that said step a) also comprises step before:
Measure the cycle potentials of electrolyte of vanadium redox battery;
If said cycle potentials value and standard electric place value produce deviation, vanadium cell is carried out recharging behind the deep discharge.
9. according to claim 5 or 6 described proving installations, it is characterized in that the mutation time that obtains the electrolytic solution current potential of vanadium cell described in the step a) is specially:
A1) gather the electrolyte of vanadium redox battery potential data;
A2) obtain the mutation time of electrolyte of vanadium redox battery current potential according to said potential data.
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| JP2016524789A (en) * | 2013-05-16 | 2016-08-18 | ハイドラレドックス テクノロジーズ ホールディングス リミテッド | Estimating the charge state of the positive electrolyte solution in a working redox flow battery cell without a reference electrode |
| CN104656030B (en) * | 2015-02-02 | 2018-04-27 | 王金全 | A kind of method of suitable flow battery SOC-OCV calibration curves |
| CN107631990B (en) * | 2017-09-08 | 2020-03-10 | 中国科学院过程工程研究所 | Method for representing apparent valence of vanadium in vanadium sodium fluorophosphate |
| CN109546186B (en) * | 2017-09-28 | 2021-11-09 | 大连融科储能技术发展有限公司 | SOC detection device and method for detecting state of electrolyte in flow battery and flow battery system with SOC detection device |
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| CN113820610B (en) * | 2021-09-21 | 2024-01-12 | 湖南钒谷新能源技术有限公司 | Method and system for detecting health state of mixed liquid of all-vanadium redox flow battery |
| CN116387583B (en) * | 2023-06-06 | 2023-09-19 | 北京普能世纪科技有限公司 | All-vanadium redox flow battery capacity recovery method |
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| CN110416648A (en) * | 2018-04-17 | 2019-11-05 | 大连融科储能装备有限公司 | The test method of single battery flow in flow battery module |
| CN110416648B (en) * | 2018-04-17 | 2021-03-02 | 大连融科储能装备有限公司 | Method for testing flow of single battery in flow battery module |
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Address after: 100084 Beijing city Haidian District Shuangqing Road research building block B Room 102 Patentee after: Beijing Puneng Century Technology Co., Ltd. Address before: 100084 Room 102, building B, comprehensive research building, Tsinghua University, Beijing, Haidian District Patentee before: Beijing Puneng Century Technology Co., Ltd. |
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