CN107621453A - The detection method of lead ion content in a kind of power type lead accumulator dividing plate - Google Patents
The detection method of lead ion content in a kind of power type lead accumulator dividing plate Download PDFInfo
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Abstract
The present invention relates to Lead-acid Battery Technology field, disclose a kind of detection method of lead ion content in power type lead accumulator dividing plate, the inventive method terminates the plumbum ion concentration in the electric power storage pool surface free acid solution for taking out the sour charging stage by detecting chemical conversion, and the content of lead ion in power type lead accumulator dividing plate is calculated.The inventive method is simple to operation, experimental result is stable, battery structure need not be destroyed during measurement, it is i.e. detectable in the preparatory phase of battery, battery separator thickness is adjusted by data result, or change technique to reduce because dividing plate dendrite penetrates caused by ion concentration is too high the problem of, the qualification rate of battery can be improved, the production cost of enterprise is reduced, suitable for industrial production and practical application, solves Pb in Electrolyte of Plumbic Acerbic High Battery2+Ion concentration can not accurate and effective detection the problem of, filled up the Pb of electrolyte in cell manufacturing process2+Technological gap in ion concentration detection.
Description
Technical field
The present invention relates to lead ion in Lead-acid Battery Technology field, more particularly to a kind of power type lead accumulator dividing plate to contain
The detection method of amount.
Background technology
Lead-acid accumulator is a kind of stable performance, safe charge power supply, the capacity of analysis inside battery electric discharge and
Terminal voltage level is extremely important to improving battery life.Lead-acid battery both positive and negative polarity reagentia mechanism is dissolving-PRECIPITATION MECHANISM, is put
Electric process：PbO2It is dissolved into electrolyte and generates Pb4+, Pb4+Ion generates Pb in the presence of extraneous electronics2+Ion, lead ion
With SO4Ionic crystal generates PbSO4.Charging process：Solid-state PbSO in both positive and negative polarity4Be dissolved as lead ion in the electrolytic solution, lead from
Son positive pole in the presence of extraneous electronics generates Pb4+Ion, Pb4+Ionic crystal is into PbO2, negative pole generation Pb.
During whole battery use, lead ion is most important intermediate product, but lead ion and SO4Ion exists
Electrolyte is H2SO4Battery in easily crystallize into PbSO4, sulfuric acid lead dendritic crystal meeting penetrating clapboard, cause battery short circuit to fail.Battery
In stability of the dividing plate in sulfuric acid directly affect life-span of battery, and clapboard aperture unreasonable structure can cause lead dendritic crystal
Growth, and then cause the increase of battery short circuit risk, battery service life reduction.Lead dendritic crystal growth causes battery short circuit, does not also have
Suppress positive active material and occur the effect expanded in deep discharge cyclic process, so as to cause battery premature failure.Lead dendritic crystal
Caused possible cause is the Pb in dividing plate2+Too high levels, the efficiency for charge-discharge of battery is have impact on, therefore in lead accumulator dividing plate
The detection of lead ion content is extremely important.
The Chinese patent of Application No. 201510019071.0 discloses lead (II) ion in a kind of battery liquid
Detection method, dissected by battery, collect the liquid in dividing plate, the lead ion content in Atomic Absorption Spectrometry amount solution and
Total plumbum ion concentration these steps are calculated, can accurately know the concentration of lead ion in dividing plate, the machine to studying battery short circuit
Reason provides important foundation.But the method can only detect the battery prepared, and battery must be dissected, such as
Fruit can just detect the content of lead ion in dividing plate in the preparatory phase of battery, then battery can be adjusted in time, improve
The product quality and qualification rate of battery, reduce cost.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides lead ion content in a kind of power type lead accumulator dividing plate
It detection method, can detect in battery chemical conversion end in the sour charging stage is taken out, be that one kind is accurate, intuitively, quickly determine
The method of testing of lead ion content in inside battery acid solution.
The present invention concrete technical scheme be：The method includes the steps of：
1) configuration standard solution：The Pb that theoretical content according to lead ion in battery electrolyte calculates2+Concentration prepare it is more
The Pb of individual gradient concentration2+Standard liquid；
2) standard curve is done：The Pb of various concentrations is tested on Atomic Absorption Spectrometer2+The absorbance of standard liquid, according to
Concentration of standard solution and absorbance linear regression, obtain standard curve；
3) sample：It is quantitative to extract chemical conversion end in the electric power storage pool surface free acid solution for taking out the sour charging stage, as survey
Sample；
4) measure：Measure absorbance of the test specimens on Atomic Absorption Spectrometer；
5) calculate：Pb in test specimens is calculated according to the absorbance of test specimens and standard curve2+Concentration, further according to test specimens
Volume and electrolyte cumulative volume calculate electrolyte in Pb2+Content.
Lead-acid battery battery in preparation process belongs to dry lotus state, i.e., form existing for lead element be lead oxide,
Lead sulfate, basic lead sulphate.Redox reaction can just only occur after chemical conversion stage injection sulfuric acid electrolyte and charging,
It can be present in the state of lead ion in electrolyte.Therefore it is that can not measure the lead ion content in electrolyte before the chemical conversion stage
's.Be melted into Battery formation charge and discharge process using pregnant solution type, during acid solution be excessive, therefore take out a small amount of acid
Preparation of the liquid detection on battery does not influence.Taking out the sour charging stage, sulfuric acid of the plumbum ion concentration in dividing plate with cluster surface
Solution is to belong to same solution system, therefore their plumbum ion concentration should have correlation, but battery is prepared and completed
Afterwards, whether the plumbum ion concentration in dividing plate with the plumbum ion concentration for taking out acid solution in sour charging process has correlation to have not been reported,
We consider penetrating for lead sulfate, by substantial amounts of experiment, experimental data card by analyzing the dividing plate dendrite phenomenon of behindhand battery
The concentration of lead ion can actually reflect in the finished battery after the completion of preparing in electrolyte in the sulfuric acid solution on bright cluster surface
Lead ion content, and the content of lead ion is higher, and the dividing plate dendrite phenomenon of battery is more serious.
Preferably, gradient concentration Pb in the step 1)2+The number of standard liquid is 12-18.
Preferably, the Atomic Absorption Spectrometer in the step 2) and step 4) is graphite furnace atomic absorption spectrophotometer.
Preferably, the detection parameters of the Atomic Absorption Spectrometer in the step 2) and step 4) are：Wavelength
455.4nm, slit width 0.5nm, lamp current 10mA, burner height 8mm, heating schedule are：25-120 DEG C, heating rate 10
DEG C/s, keep 40s；120-1700 DEG C, 10 DEG C/s of heating rate, keep 30s；1700-2700 DEG C, 30 DEG C/s of heating rate, protect
Hold 5s；2700-2800 DEG C, 10 DEG C/s of heating rate, keep 5s.
Preferably, the Pb in the step 2)2+The average value of the intermediate concentration of standard liquid or two intermediate concentrations with
The Pb that theoretical content calculates in solution2+Concentration deviation is not more than 5%.
Preferably, sampling number is 6 in the step 3), sample position is respectively 6 single lattice pole plate tables of battery
Face.
Preferably, repeat step 3) -5), calculate the Pb in multiple electrolyte being calculated by test specimens2+Content
The content of lead ion in average value, as power type lead accumulator dividing plate.
Although plumbum ion concentration is to belong to same solution system with the sulfuric acid solution on cluster surface, the electricity where solution
Pond internal structure is complicated, therefore it is difficult to ensure that solution is homogeneous in preparation process, and inside battery has multiple different single lattices,
It is unconnected between single lattice, it is therefore desirable to take multiple samples to average to ensure the accuracy of result.
Preferably, the Pb of six single lattice polar board surfaces of the battery2+The standard deviation of concentration is smaller, battery Pb2+Point
Cloth is more uniform, if standard deviation is more than 5%, the battery is unqualified, need to be adjusted.
Preferably, the content of lead ion is if 0.1-5g/L, then battery conjunction in the power type lead accumulator dividing plate
Lattice, if not in this range, the battery needs to adjust the content of lead ion in power type lead accumulator dividing plate.
In the electrolyte of battery, lead ion average content is too high or lead ion skewness, and local too high levels are all
Lead dendritic crystal generation is likely to result in, so as to influence battery life.
Preferably, Pb in test specimens in the step 5)2+Concentration in the concentration range of standard liquid.
It is compared with the prior art, the beneficial effects of the invention are as follows：The inventive method takes out acid by detecting to be melted into terminate to be in
The plumbum ion concentration of the electric power storage pool surface free acid solution of charging stage, is calculated lead ion in power type lead accumulator dividing plate
Content, the inventive method is simple to operation, and experimental result is stable, and result is identical with trend compared with prior art, but survey
Battery structure need not be destroyed during amount, i.e. detectable in the preparatory phase of battery, the preparation on battery does not influence, if going wrong
It can in time take measures, the methods of by the arrangement that adjusts dividing plate, make the lead ion content of battery up to standard, it is possible to increase battery
Qualification rate, reduce the production cost of enterprise.This method reliable results, has convincingness, suitable for work closer to actual production
Industry produces and practical application, solves Pb in Electrolyte of Plumbic Acerbic High Battery2+Ion concentration can not accurate and effective detection the problem of,
Battery separator thickness can be adjusted by data result, or change technique come reduce caused by ion concentration is too high every
The problem of plate dendrite penetrates, the Pb of electrolyte in cell manufacturing process is filled up2+Technological gap in ion concentration detection.
Embodiment
With reference to embodiment, the invention will be further described.
4 formulas and preparation method identical power type lead accumulator are chosen, respectively with 1,2 ..., 4 numberings, its electrolyte
The theoretical content of middle lead ion is 0.1-5g/L.
Embodiment 1
Make standard curve：According to battery formula, the Pb calculated according to the theoretical content of lead ion in electrolyte2+Concentration
Prepare the Pb of 18 concentration gradients2+Standard liquid, concentration are respectively 0.5g/L, 0.7g/L, 0.9g/L, 1.1g/L ..., 4.1g/
L.The Pb of various concentrations is tested on graphite furnace atomic absorption spectrophotometer2+The absorbance of standard liquid, according to concentration of standard solution
With absorbance linear regression, standard curve is obtained.
Sample measures：No. 1 battery is chosen, 6 chemical conversions is extracted respectively and terminates to be in 6 of the battery for taking out the sour charging stage
The free acid solution of single lattice polar board surface, amount of sampling 1mL, measure the absorbance on Atomic Absorption Spectrometer.According to electrolysis
The cumulative volume and sampling volume of liquid calculate the content of lead ion in electrolyte.Calculate the average value of 6 sample lead ion contents.
Embodiment 2
Make standard curve：According to battery formula, the Pb calculated according to the theoretical content of lead ion in electrolyte2+Concentration
Prepare the Pb of 12 concentration gradients2+Standard liquid, concentration are respectively 0.2g/L, 0.5g/L, 0.8g/L, 1.1g/L ..., 3.8g/
L.The Pb of various concentrations is tested on graphite furnace atomic absorption spectrophotometer2+The absorbance of standard liquid, according to concentration of standard solution
With absorbance linear regression, standard curve is obtained.
Sample measuring method is same as Example 1.
Embodiment 3
Make standard curve：According to battery formula, the Pb calculated according to the theoretical content of lead ion in electrolyte2+Concentration
Prepare the Pb of 15 concentration gradients2+Standard liquid, concentration are respectively 0.3g/L, 0.4g/L, 0.5g/L ..., 1.8g/L.In graphite
The Pb of various concentrations is tested on stove Atomic Absorption Spectrometer2+The absorbance of standard liquid, according to concentration of standard solution and absorbance
Linear regression, obtain standard curve.
Sample measuring method is same as Example 1.
Embodiment 4-6
2-4 batteries are chosen respectively, and the making of remaining standard curve and sample measuring method are same as Example 1.
Comparative example 1-4
1-4 batteries are chosen respectively, and battery is dissected, that determines weight power taking pond contains sulfuric acid AGM dividing plates, weight W1,
Using pure water soak and rinse dividing plate, until each position of dividing plate in neutrality, collect it is all immersion and flushing liquid and with determine
The volume of the quantification of fixation of measuring bottle, volume V1, using these liquid of Atomic Absorption Spectrometry amount, the content of gained lead ion
For Q1, the dividing plate rinsed well drying is weighed, weight W2, then in dividing plate electrolyte plumbum ion concentration be C=(Q1 × V1)/
(W1-W2)。
Plumbum ion concentration of the table 1. according to obtained by various criterion curve
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Average lead ion content | 0.745g/L | 0.761g/L | 0.753g/L |
According to table 1 we can see that using different standard curves, as long as within the scope of the invention, it is measured to obtain
Lead ion content error within 2%.
The different lead ion content measuring method contrast of table 2.
| Numbering | Plumbum ion concentration obtained by the inventive method | The standard deviation of 6 measurements | Plumbum ion concentration obtained by control methods |
| 1 | 0.74g/L | 3.40% | 0.85g/L |
| 2 | 0.89g/L | 7.84% | 0.92g/L |
| 3 | 5.68g/L | 2.79% | 5.90g/L |
| 4 | 7.71g/L | 5.58% | 7.22g/L |
Embodiment Isosorbide-5-Nitrae -6 and comparative example 1-4 measurement result are shown in Table 2.According to table 2 it will be seen that the inventive method
The lead ion content or conclusion that the lead ion content that measurement obtains obtains with prior art are basically identical, particularly dense in lead ion
When spending up to standard, the standard deviation of different single lattice lead ion contents, such as No. 2 batteries qualified in conventional method are also have detected,
In the detection of the inventive method, and it is unqualified, it need in time adjust, further improve the performance of battery.Therefore the inventive method is
The plumbum ion concentration measuring method higher than conventional method recall rate.Averaged in addition, the inventive method can be checked repeatedly,
The degree of accuracy of detection is improved, the process of detection liquid is prepared in conventional method needs soaking flushing dividing plate, it is difficult to not by artificial
Error caused by operation,
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；In the present invention
Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (10)
1. the detection method of lead ion content in a kind of power type lead accumulator dividing plate, it is characterised in that this method includes following
Step：
1）Configuration standard solution：The Pb that theoretical content according to lead ion in battery electrolyte calculates2+Concentration prepare multiple ladders
Spend the Pb of concentration2+Standard liquid；
2）Do standard curve：The Pb of various concentrations is tested on Atomic Absorption Spectrometer2+The absorbance of standard liquid, according to standard
Solution concentration and absorbance linear regression, obtain standard curve；
3）Sampling：It is quantitative to extract chemical conversion end in the electric power storage pool surface free acid solution for taking out the sour charging stage, as test specimens；
4）Measurement：Measure absorbance of the test specimens on Atomic Absorption Spectrometer；
5）Calculate：Pb in test specimens is calculated according to the absorbance of test specimens and standard curve2+Concentration, further according to the body of test specimens
Product and electrolyte cumulative volume calculate the Pb in electrolyte2+Content.
2. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 1, it is characterised in that institute
State step 1）Middle gradient concentration Pb2+The number of standard liquid is 12-18.
3. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 1, it is characterised in that institute
State step 2）With step 4）In Atomic Absorption Spectrometer be graphite furnace atomic absorption spectrophotometer.
4. the detection method of lead ion content, its feature exist in the power type lead accumulator dividing plate as described in claim 1 or 3
In the step 2）With step 4）In the detection parameters of Atomic Absorption Spectrometer be：Wavelength 455.4nm, slit width
0.5nm, lamp current 10mA, burner height 8mm, heating schedule are：25-120 DEG C, 10 DEG C/s of heating rate, keep 40s；
120-1700 DEG C, 10 DEG C/s of heating rate, keep 30s；1700-2700 DEG C, 30 DEG C/s of heating rate, keep 5s；2700-2800
DEG C, 10 DEG C/s of heating rate, keep 5s.
5. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 1, it is characterised in that institute
State step 2）In Pb2+Theoretical content calculates in the average value and solution of the intermediate concentration of standard liquid or two intermediate concentrations
Pb2+Concentration deviation is not more than 5%.
6. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 1, it is characterised in that institute
State step 3）Middle sampling number is 6, and sample position is respectively 6 single lattice polar board surfaces of battery.
7. the detection method of lead ion content, its feature exist in the power type lead accumulator dividing plate as described in claim 1 or 6
In repeat step 3）-5）, calculate the Pb in multiple electrolyte being calculated by test specimens2+The average value of content, as power
The content of lead ion in type lead accumulator dividing plate.
8. the detection method of lead ion content, its feature exist in the power type lead accumulator dividing plate as described in claim 1 or 6
In the Pb of six single lattice polar board surfaces of the battery2+The standard deviation of concentration is smaller, battery Pb2+Distribution is more uniform, if mark
Quasi- difference is more than 5%, then the battery is unqualified, need to be adjusted.
9. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 7, it is characterised in that institute
The content of lead ion in power type lead accumulator dividing plate is stated if 0.1-5g/L, then the battery is qualified, if power type lead accumulator
Not in this range, then the battery needs to adjust the content of lead ion in dividing plate.
10. the detection method of lead ion content in power type lead accumulator dividing plate as claimed in claim 1, it is characterised in that
The step 5）Pb in middle test specimens2+Concentration in the concentration range of standard liquid.
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| CN109060785A (en) * | 2018-06-21 | 2018-12-21 | 超威电源有限公司 | The test method of lead sulfate in a kind of lead storage battery separator paper |
| CN110715902A (en) * | 2019-08-29 | 2020-01-21 | 超威电源有限公司 | Method for detecting uniformity of positive lead paste of lead-acid storage battery |
| CN111307845A (en) * | 2018-12-25 | 2020-06-19 | 超威电源有限公司 | Sampling analysis method for polar plate formation stage |
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Address after: 313100 Zhejiang city of Huzhou province Changxing County pheasant emerging urban industrial park Applicant after: Chaowei Power Group Co., Ltd Address before: 313100 Zhejiang city of Huzhou province Changxing County pheasant emerging urban industrial park Applicant before: Chilwee Power Supply Co., Ltd. |
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