CN107621453B - Method for detecting content of lead ions in power type lead storage battery separator - Google Patents
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Abstract
The invention relates to the technical field of lead-acid storage batteries, and discloses a method for detecting the content of lead ions in a power type lead storage battery separatorAnd calculating the lead ion concentration of the free acid solution on the surface of the storage battery in the acid charging stage to obtain the content of the lead ions in the power type lead storage battery separator. The method is simple and easy to operate, has stable experimental results, does not need to damage the battery structure during measurement, can detect the battery in the preparation stage of the battery, adjusts the thickness of the battery separator through data results or changes the process to reduce the problem of dendritic crystal penetration of the separator caused by overhigh ion concentration, can improve the qualification rate of the battery, reduces the production cost of enterprises, is suitable for industrial production and practical application, and solves the problem of Pb in the electrolyte of the lead-acid storage battery2+The problem that the ion concentration can not be accurately and effectively detected is solved, and the Pb of the electrolyte in the battery preparation process is filled2+Technical blank in ion concentration detection.
Description
Technical Field
The invention relates to the technical field of lead-acid storage batteries, in particular to a method for detecting the content of lead ions in a power type lead storage battery separator.
Background
The lead-acid storage battery is a charging power supply with stable performance and high safety, and the analysis of the discharge capacity and terminal voltage level inside the battery is very important for prolonging the service life of the battery. The reaction mechanism of the positive electrode and the negative electrode of the lead-acid battery is a dissolution-precipitation mechanism, and the discharging process is as follows: PbO2Dissolved in the electrolyte to generate Pb4+，Pb4+The ions generate Pb under the action of external electrons2+Ions, lead ions and SO4Ion crystallization to produce PbSO4. And (3) charging process: solid PbSO in positive and negative electrodes4Lead ions are dissolved in the electrolyte, and the positive electrode of the lead ions generates Pb under the action of external electrons4+Ion, Pb4+Ion crystallization to PbO2The negative electrode generates Pb.
Lead ions are the most important intermediate product during the whole battery use process, but lead ions and SO4The ion in the electrolyte is H2SO4Is easy to crystallize into PbSO4The lead sulfate dendrites can penetrate the separator, causing short circuit failure of the battery. The stability of the separator in the battery in sulfuric acid directly affects the service life of the battery, and the improper pore diameter structure of the separator can lead to the growth of lead dendrites, so that the risk of battery short circuit is increased, and the service life of the battery is shortened. The lead dendrite growth causes a short circuit of the battery and also does not play a role in inhibiting the positive active material from swelling during a deep discharge cycle, thereby causing premature failure of the battery. A possible cause of lead dendrite generation is Pb in the separator2+The content is too high, which affects the charging and discharging efficiency of the battery, so the detection of the content of lead ions in the lead storage battery separator is very important.
The Chinese patent with the application number of 201510019071.0 discloses a method for detecting divalent lead ions in a storage battery electrolyte, which can accurately know the concentration of lead ions in a partition plate through the steps of battery dissection, collection of liquid in the partition plate, measurement of the content of lead ions in a solution by an atomic absorption spectrometry and calculation of the total lead ion concentration, and provides an important basis for researching the short circuit mechanism of a battery. However, the method can only detect the prepared battery, and the battery must be dissected, if the content of the lead ions in the partition plate can be detected in the preparation stage of the battery, the battery can be adjusted in time, the product quality and the qualification rate of the battery are improved, and the cost is reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for detecting the content of lead ions in a power type lead storage battery separator, which can detect the content of the lead ions in acid liquor in a battery accurately, visually and quickly when the formation of the storage battery is finished and the storage battery is in an acid pumping and charging stage.
The specific technical scheme of the invention is as follows: the method comprises the following steps:
1) preparing a standard solution: calculated Pb according to the theoretical content of lead ions in the electrolyte of the battery2+Concentration of (2) preparing Pb of multiple gradient concentrations2+A standard solution;
2) making a standard curve: testing different concentrations of Pb on atomic absorption spectrometer2+Performing linear regression on the absorbance of the standard solution according to the concentration of the standard solution and the absorbance to obtain a standard curve;
3) sampling: quantitatively extracting a free acid solution on the surface of the storage battery in the acid-extracting and charging stage after the formation is finished, namely obtaining a test sample;
4) measurement: measuring the absorbance of the measured sample on an atomic absorption spectrometer;
5) and (3) calculating: calculating Pb in the test sample according to the absorbance of the test sample and the standard curve2+And then calculating Pb in the electrolyte according to the volume of the test sample and the total volume of the electrolyte2+The content of (a).
The lead-acid battery belongs to a dry-charged state in the preparation process, namely, the lead element exists in the forms of lead oxide, lead sulfate and basic lead sulfate. Only after the sulfuric acid electrolyte is injected and charged in the formation stage, the redox reaction occurs, and the lead ions exist in the electrolyte. It is not possible to measure the lead ion content of the electrolyte prior to the formation stage. The method adopts the liquid-enriched formation in the process of charging and discharging the battery formation, and the acid liquid is excessive in the process, so that the detection of taking out a small amount of acid liquid has no influence on the preparation of the battery. In the acid extraction and charging stage, the lead ion concentration in the partition board and the sulfuric acid solution on the surface of the cluster belong to the same solution system, so that the lead ion concentration of the partition board and the sulfuric acid solution on the surface of the cluster are related, but after the battery is prepared, whether the lead ion concentration in the partition board is related to the lead ion concentration of the acid solution in the acid extraction and charging process is not reported, the lead ion content in the electrolyte in the prepared battery finished product can be reflected by analyzing the partition board dendritic phenomenon of the lagging battery through a large number of experiments by considering the penetration of lead sulfate, and the higher the lead ion content is, the more serious the partition board dendritic phenomenon of the battery is.
Preferably, the gradient concentration Pb in the step 1) is2+The number of standard solutions is 12-18.
Preferably, the atomic absorption spectrometer in the step 2) and the step 4) is a graphite furnace atomic absorption spectrometer.
Preferably, the detection parameters of the atomic absorption spectrometer in the step 2) and the step 4) are as follows: the wavelength is 455.4nm, the slit width is 0.5nm, the lamp current is 10mA, the burner height is 8mm, and the temperature rise program is as follows: heating at 25-120 deg.C at a heating rate of 10 deg.C/s for 40 s; at the temperature of 120 ℃ and 1700 ℃, the heating rate is 10 ℃/s, and the temperature is kept for 30 s; 1700 ℃ and 2700 ℃, the temperature rise rate is 30 ℃/s, and the temperature is kept for 5 s; 2700 ℃ and 2800 ℃ with a temperature rise rate of 10 ℃/s for 5 s.
Preferably, Pb in the step 2)2+The mean concentration or the mean of two mean concentrations of the standard solution and the calculated Pb content of the solution2+The concentration deviation is not more than 5%.
Preferably, in the step 3), the number of samples is 6, and the sampling positions are the surfaces of 6 unit grid plates of the battery respectively.
Preferably, steps 3) to 5) are repeated, calculating Pb in a plurality of electrolytes calculated from the test samples2+The average value of the contents is the content of the lead ions in the separator of the power type lead storage battery.
Although the lead ion concentration and the sulfuric acid solution on the surface of the cluster belong to the same solution system, the internal structure of the battery where the solution is located is complex, so that the solution is difficult to be ensured to be uniform in the preparation process, a plurality of different cells are arranged in the battery, and the cells are not connected, so that a plurality of samples need to be averaged to ensure the accuracy of the result.
Preferably, the battery has Pb on the surfaces of six single-grid plates2+The smaller the standard deviation of the concentration, the smaller the Pb content of the battery2+The more uniform the distribution, if the standard deviation is greater than 5%, the battery is not qualified and needs to be adjusted.
Preferably, if the content of lead ions in the separator of the power lead storage battery is 0.1 to 5g/L, the battery is qualified, and if the content of lead ions in the separator of the power lead storage battery is not within this range, the battery needs to be adjusted.
In the electrolyte of the battery, the average content of lead ions is too high or the distribution of lead ions is not uniform, and the local content is too high, which may cause lead dendrite generation, thereby affecting the service life of the battery.
Preferably, Pb in the sample is measured in the step 5)2+Is within the concentration range of the standard solution.
Compared with the prior art, the invention has the beneficial effects that: the method calculates the content of the lead ions in the power type lead storage battery separator by detecting the lead ion concentration of the free acid solution on the surface of the storage battery in the acid pumping and charging stage after the formation is finishedMeasures are taken, the lead ion content of the battery reaches the standard by adjusting the arrangement of the partition plates and other methods, the qualified rate of the battery can be improved, and the production cost of enterprises is reduced. The method is closer to the actual production, has reliable result and convincing power, is suitable for industrial production and practical application, and solves the problem of Pb in the electrolyte of the lead-acid storage battery2+The problem that the ion concentration cannot be accurately and effectively detected can be solved by adjusting the thickness of the battery separator through a data result or changing the process to reduce the problem of dendritic crystal penetration of the separator caused by overhigh ion concentration, and the Pb of the electrolyte in the battery preparation process is filled2+Technical blank in ion concentration detection.
Detailed Description
The present invention will be further described with reference to the following examples.
4 power type lead storage batteries with the same formula and preparation method are selected and numbered as 1, 2, … and 4 respectively, and the theoretical content of lead ions in the electrolyte is 0.1-5 g/L.
Example 1
Making a standard curve: calculated Pb according to the formula of the battery and the theoretical content of lead ions in the electrolyte2+Concentration of (2) to prepare Pb with 18 concentration gradients2+The concentrations of the standard solutions are 0.5g/L, 0.7g/L, 0.9g/L, 1.1g/L, … and 4.1g/L respectively. Testing Pb with different concentrations on graphite furnace atomic absorption spectrometer2+And (5) linearly regressing the absorbance of the standard solution according to the concentration and the absorbance of the standard solution to obtain a standard curve.
Sample measurement: selecting a No. 1 battery, respectively extracting 6 free acid solutions on the surfaces of 6 single grid polar plates of the storage battery with the formation completed in the acid extraction charging stage, wherein the sampling amount is 1mL, and measuring the absorbance on an atomic absorption spectrometer. And calculating the content of lead ions in the electrolyte according to the total volume and the sampling volume of the electrolyte. The average of the lead ion contents of the 6 samples was calculated.
Example 2
Making a standard curve: calculated Pb according to the formula of the battery and the theoretical content of lead ions in the electrolyte2+Concentration of (2) to prepare Pb with 12 concentration gradients2+The standard solution is used for preparing a standard solution,the concentrations are 0.2g/L, 0.5g/L, 0.8g/L, 1.1g/L, …, 3.8g/L, respectively. Testing Pb with different concentrations on graphite furnace atomic absorption spectrometer2+And (5) linearly regressing the absorbance of the standard solution according to the concentration and the absorbance of the standard solution to obtain a standard curve.
The sample measurement method was the same as in example 1.
Example 3
Making a standard curve: calculated Pb according to the formula of the battery and the theoretical content of lead ions in the electrolyte2+Concentration of (2) to prepare Pb with 15 concentration gradients2+The concentrations of the standard solutions are 0.3g/L, 0.4g/L, 0.5g/L, … and 1.8g/L respectively. Testing Pb with different concentrations on graphite furnace atomic absorption spectrometer2+And (5) linearly regressing the absorbance of the standard solution according to the concentration and the absorbance of the standard solution to obtain a standard curve.
The sample measurement method was the same as in example 1.
Examples 4 to 6
The batteries of No. 2 to No. 4 are respectively selected, and the manufacturing and sample measuring methods of the other standard curves are the same as those of the example 1.
Comparative examples 1 to 4
Respectively selecting batteries No. 1-4, dissecting the batteries, weighing a sulfuric acid AGM separator of each battery according to a certain weight, wherein the weight is W1, soaking and washing the separator by pure water until each part of the separator is neutral, collecting all soaked and washed liquids, quantifying the liquids into a fixed volume by using a quantitative bottle, wherein the volume is V1, measuring the liquids by adopting an atomic absorption spectrometry method, wherein the content of the obtained lead ions is Q1, drying and weighing the washed separator according to a weight of W2, and the concentration of the lead ions in the electrolyte of the separator is C (Q1 x V1)/(W1-W2).
TABLE 1 lead ion concentration according to different standard curves
| Example 1 | Example 2 | Example 3 | |
| Average lead ion content | 0.745g/L | 0.761g/L | 0.753g/L |
From table 1 we can see that different standard curves are used, provided that within the scope of the invention the measured lead ion content is within 2%.
TABLE 2 comparison of different lead ion content measurement methods
| Numbering | Concentration of lead ions obtained by the method of the invention | Standard deviation of 6 measurements | Concentration of lead ions obtained by the comparative method |
| 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 |
The measurement results of examples 1, 4 to 6 and comparative examples 1 to 4 are shown in Table 2. According to table 2, it can be seen that the lead ion content measured by the method of the present invention is substantially consistent with the lead ion content or conclusion obtained by the prior art, and particularly, when the lead ion concentration meets the standard, the standard deviation of the lead ion content of different cells is also detected, for example, the qualified battery No. 2 in the conventional method is not qualified in the detection of the method of the present invention, and needs to be adjusted in time, so as to further improve the performance of the battery. Therefore, the method is a method for measuring the lead ion concentration with higher detection rate than the traditional method. In addition, the method of the invention can carry out a plurality of times of examination and average value taking, improves the detection accuracy, and the traditional method needs to soak and wash the clapboard in the process of preparing the detection solution, is difficult to avoid errors caused by manual operation,
the raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for detecting the content of lead ions in a power type lead storage battery separator is characterized by comprising the following steps:
1) preparing a standard solution: calculated Pb according to the theoretical content of lead ions in the electrolyte of the battery2+Concentration of (2) preparing Pb of multiple gradient concentrations2+A standard solution;
2) making a standard curve: testing different concentrations of Pb on atomic absorption spectrometer2+Performing linear regression on the absorbance of the standard solution according to the concentration of the standard solution and the absorbance to obtain a standard curve;
3) sampling: quantitatively extracting a free acid solution on the surface of the storage battery in the acid-extracting and charging stage after the formation is finished, namely obtaining a test sample;
4) measurement: measuring the absorbance of the measured sample on an atomic absorption spectrometer;
5) and (3) calculating: calculating Pb in the test sample according to the absorbance of the test sample and the standard curve2+And then calculating Pb in the electrolyte according to the volume of the test sample and the total volume of the electrolyte2+The content of (a).
2. The method for detecting the content of lead ions in the separator of a power lead storage battery as set forth in claim 1, wherein the gradient concentration Pb in the step 1) is2+The number of standard solutions is 12-18.
3. The method for detecting the content of the lead ions in the power type lead storage battery separator as claimed in claim 1, wherein the atomic absorption spectrometer in the step 2) and the step 4) is a graphite furnace atomic absorption spectrometer.
4. The method for detecting the content of lead ions in the power type lead storage battery separator as claimed in claim 1 or 3, wherein the detection parameters of the atomic absorption spectrometer in the step 2) and the step 4) are as follows: wavelength 216.70nm, slit width 0.5nm, lamp current 10mA, burner height 8mm, the temperature-raising procedure is: heating at 25-120 deg.C at a heating rate of 10 deg.C/s for 40 s; at the temperature of 120 ℃ and 1700 ℃, the heating rate is 10 ℃/s, and the temperature is kept for 30 s; 1700 ℃ and 2700 ℃, the temperature rise rate is 30 ℃/s, and the temperature is kept for 5 s; 2700 ℃ and 2800 ℃ with a temperature rise rate of 10 ℃/s for 5 s.
5. The method for detecting the content of lead ions in the separator of a power lead storage battery according to claim 1, wherein the Pb in the step 2) is Pb2+The mean concentration or the mean of two mean concentrations of the standard solution and the calculated Pb content of the solution2+The concentration deviation is not more than 5%.
6. The method for detecting the content of lead ions in the separator of the power lead storage battery as claimed in claim 1, wherein the number of samples taken in the step 3) is 6, and the sampling positions are respectively the surfaces of 6 single-grid plates of the battery.
7. The method for detecting the content of lead ions in a separator for a power lead-acid battery as claimed in claim 1 or 6, wherein the steps 3) to 5) are repeated to calculate Pb in a plurality of electrolytes calculated from the test samples2+The average value of the contents is the content of the lead ions in the separator of the power type lead storage battery.
8. The method for detecting the content of lead ions in the separator of a power lead storage battery as claimed in claim 1 or 6, wherein the Pb on the surfaces of six unit grid plates of the battery2+The smaller the standard deviation of the concentration, the smaller the Pb content of the battery2+The more uniform the distribution, if the standard deviation is greater than 5%, the battery is not qualified and needs to be adjusted.
9. The method of claim 7, wherein the battery is qualified if the content of lead ions in the separator of the power lead storage battery is 0.1-5g/L, and the battery needs to be adjusted if the content of lead ions in the separator of the power lead storage battery is not within the above range.
10. The power lead acid battery separator lead ion of claim 1The method for detecting the content of the seeds is characterized in that the Pb in the sample is detected in the step 5)2+Is within the concentration range of the standard solution.
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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 |
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| 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 |
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