CN113607595A - Detection method of green plate corrosion layer - Google Patents
Detection method of green plate corrosion layer Download PDFInfo
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- CN113607595A CN113607595A CN202110797478.1A CN202110797478A CN113607595A CN 113607595 A CN113607595 A CN 113607595A CN 202110797478 A CN202110797478 A CN 202110797478A CN 113607595 A CN113607595 A CN 113607595A
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- 230000007797 corrosion Effects 0.000 title claims abstract description 68
- 238000005260 corrosion Methods 0.000 title claims abstract description 68
- 238000001514 detection method Methods 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 239000011505 plaster Substances 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000005303 weighing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 238000012795 verification Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 25
- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005259 measurement Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 239000013585 weight reducing agent Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001999 grid alloy Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention provides a method for detecting a corrosion layer of a green plate, which comprises the steps of knocking off lead plaster of the cured green plate, charging a grid, converting the corrosion layer on the grid into lead dioxide, treating the converted lead dioxide with sugar alkali, subtracting the weight of the grid after sugar alkali treatment from the weight of the grid before charging, and subtracting the amount of the charged corrosion grid, wherein the final difference is the corrosion layer formed in the curing process. The detection method can accurately measure the corrosion layer formed in the curing process, judge the excellent condition of the corrosion layer formed in the curing process, standardize the measurement process of the corrosion layer, reduce the test error and improve the accuracy of the measurement of the corrosion layer; the invention effectively avoids the deviation caused by the individual difference of the test samples, the difference of the external circuit, the difference of the connection resistance of the lead, the temperature or the concentration of the electrolyte of the grid and the like.
Description
Technical Field
The invention belongs to the technical field of lead-acid storage batteries, and relates to a detection method for a green plate corrosion layer of a corrosion layer formed in a curing process.
Background
The green plate of the lead-acid storage battery needs to be subjected to processes of curing and the like, the curing process is a very complex process, the moisture and free lead in the lead paste gradually reach specified indexes in the curing process, and a transition layer, namely a corrosion layer, is formed between the grid and the lead paste along with the formation of 3BS and 4 BS. Whether the pole plate solidified in the whole industry reaches the standard or not is generally determined according to the contents of moisture content, free lead, pole plate falling weight loss rate and the like. The determination of the corrosion layer is to knock off the lead plaster of the green plate, observe the lead plaster remained on the grid or observe whether the grid still has metallic luster, if the lead plaster remained on the grid is less or the metallic luster of the grid is obvious, the corrosion layer formed in the curing process is poor, otherwise, the corrosion layer in the curing process is good; however, such an observation to determine the corrosion layer usually requires sufficient experience and also does not provide sufficient quantitative data.
Whether the curing process meets the requirements or not is judged through observation, subjective factor difference exists, and meanwhile, the final judgment result is directly influenced through the paste knocking process; the change of the water content of the polar plate at the end of curing has great influence on the judgment of the corrosion layer; in addition, the observation method determines that the corrosion layer has no quantitative value, and the quality monitoring cannot be clear.
Patent CN 104075960B discloses a method for rapidly measuring corrosion resistance of a storage battery grid alloy, which mainly comprises the following steps: weighing a grid with the corrosion resistance to be measured; the grid is used as the anode, other materials with the same area and any conductivity and corrosion resistance are used as the cathode to form an electrolysis loop, and the electrolysis loop is connected with a lead and put into an electrolysis bath; adding a sulfuric acid solution into an electrolytic cell, and placing the electrolytic cell in a constant-temperature water bath box; connecting an electrolysis loop to a charge and discharge machine, and performing constant current corrosion and charge and discharge circulation; taking down the positive plate grid, soaking in boiling sugar-alkali solution, and stripping off corrosion products; and drying and weighing the positive grid stripped by the corrosion product, calculating a weight difference value before and after the grid is corroded, and calculating the weight loss rate of the grid according to the weight difference value. This method suffers from the following drawbacks: the positive plate grid and the negative plate grid are not effectively blocked, so that the contact short circuit of the positive and negative electrodes cannot be prevented, different positive plate grids respectively form an electrolytic loop, and the test error caused by the difference between the loops cannot be avoided; adding a sulfuric acid solution into the electrolytic tank to enable the liquid level of the sulfuric acid solution to be slightly higher than the top end of the grid, but the liquid level can be reduced in the test process, so that part of the grid can be exposed out of the liquid level; the boiled sugar alkaline water can dissolve corrosion products and corrode the lead alloy matrix of the grid, and the method does not consider the influence of the factors and the like.
Disclosure of Invention
The invention aims to provide a method for detecting a green plate corrosion layer for accurately measuring a corrosion layer formed in a curing process, aiming at solving the defects that whether the curing process meets requirements or not is judged by observation and subjective factor difference exists.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for detecting a corrosion layer of a green plate comprises the following steps:
a) removing lead plaster from the smeared wet grid, cleaning, drying in vacuum, welding a lead on a lug of the wet grid, weighing the lead and recording the weight as m1；
b) Removing lead plaster from the cured dry green grid, cleaning, drying in vacuum, welding a lead on a tab of the dry green grid, weighing the lead and the lead as M1；
c) Placing the wet green grid in the step a) and the dry green grid in the step b) in different cells, and connecting the two cells in series to form a battery by adopting a normal negative plate as a negative electrode;
d) adding sulfuric acid into the single cells in the step c), and charging after soaking;
e) the charging is divided into two steps;
f) taking out the wet raw grid and the dry raw grid after charging, washing, putting the washed wet raw grid and the dry raw grid into a sugar-alkali solution, boiling for 25-45mnin, washing and then drying in vacuum;
g) weighing the dried wet green grids in the step f), and recording the weights as m2And f) weighing the dried dry green grid in the step f), and recording as M2；
The corrosion layer calculation method comprises the following steps: n ═ M1-M2)-(m1-m2) (ii) a Wherein, n: weight of corrosion layer formed during curing, g.
In the technical scheme, the cured green plate is knocked off lead plaster, the grid is charged, the corrosion layer on the grid is converted into lead dioxide, the converted lead dioxide is treated by sugar alkali, the weight of the grid before charging is reduced by the weight of the grid after sugar alkali treatment, and the amount of the charged corrosion grid is reduced, so that the final difference is the corrosion layer formed in the curing process.
The invention solves the problem that the corrosion layer can not be quantized, specifies the method for measuring the corrosion of the green plate, determines the calculation process of the corrosion layer, reduces the error in the measurement process and improves the accuracy of the measurement of the corrosion layer.
As a preferred embodiment of the present invention, in step d), 800g of 700-800g of the additive with the density of 1.25-1.35g/cm are added into each single cell3Sulfuric acid (c).
3. The method for detecting the corrosion layer of the green plate according to claim 1, wherein in the step d), the green plate is kept still for 24-30 hours after the sulfuric acid is added.
As a preferable scheme of the invention, in the step e), the first step of charging is 0.4-0.6A for 25-35min, and the second step of charging is 2.8-3.2A for 1-5 h.
In a preferred embodiment of the present invention, in step e), the first charging step is 0.5A charging for 30min, and the second charging step is 3A charging for 3 h.
In a preferred embodiment of the present invention, in step f), 15-25g of glucose and 95-110g of sodium hydroxide are added to 1L of distilled water as the sugar alkali solution.
As a preferable scheme of the invention, the dosage of the sugar-alkali solution is 3-8 times of the total weight of the wet raw grid and the dry raw grid.
As a preferable scheme of the invention, the method further comprises a step h) of error verification, wherein a plurality of wet green grids in the step a) and dry green grids in the step b) are taken, and an average value of weight differences before and after corrosion is calculated to obtain the error verification, and the calculation method comprises the following steps:
wherein the content of the first and second substances,
g, the average value of the weight difference of the dry-green grid before and after charging;
average of weight difference before and after charging, g, for wet green grids.
As a preferable scheme of the present invention, in the step h), 5 wet green grids and 5 dry green grids are taken to calculate an average value.
Compared with the prior art, the invention has the following beneficial effects:
the detection method can accurately measure the corrosion layer formed in the curing process, judge the excellent condition of the corrosion layer formed in the curing process, standardize the measurement process of the corrosion layer, reduce the test error and improve the accuracy of the measurement of the corrosion layer; the invention effectively avoids the deviation caused by the individual difference of the test samples, the difference of the external circuit, the difference of the connection resistance of the lead, the temperature or the concentration of the electrolyte of the grid and other environmental differences.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Measurement Process
A. After smearing, extracting a wet grid, knocking off lead plaster, cleaning the residual lead plaster on the grid by using pure water, welding a lead on a tab of the grid after vacuum drying, and finally weighing and recording the lead and the lead as m1(the grids are marked as uncured grids).
B. After the solidification is finished, the dry and raw grid is extractedKnocking off lead plaster, cleaning the residual lead plaster on the grid by using pure water, welding a lead on a tab of the grid after vacuum drying, and finally weighing and recording the lead and the lead as M1(the grid is marked as a cured grid).
C. The two grids are used as positive electrodes and placed in different units, a normal negative plate is used as a negative electrode, the PE bag type partition plate is used for encapsulating the positive electrode, the two single grids are connected in series to form a battery, a positive electrode and a negative electrode are reserved to be used as external connectors, and the external connectors are connected with a charge-discharge machine.
D. 750g of 1.280g/cm are added to each cell3Soaking in sulfuric acid for 24 hr and charging.
E. The charging was carried out in two steps, first 0.5A for 30min and second 3A for 3 h.
F. And (3) taking out the two grids after charging is finished, washing off residual sulfuric acid by using pure water, putting the grids into a sugar-alkali solution, boiling for 30min, repeatedly cleaning by using clear water, and finally performing vacuum drying.
G. Weighing the two dried grids again, wherein the weight of the uncured grid is m2The weight of the cured grid is M2。
H. The formula of the sugar alkali capacity is as follows: for every 1L of distilled water, 20g of glucose and 100g of strong sodium oxide were added.
Corrosion layer calculation method:
formula 1: n ═ M1-M2)-(m1-m2):
Formula 2:
n: weight of corrosion layer formed during curing, g.
M1: weight before charging of the cured grid, g.
M2: weight of the cured grid after charging, g.
m1: weight of uncured grid before charging, g.
m2: weight of uncured grid after charging, g.
The following are calculated data for the corrosion layers of the uncured and cured plates of the present invention, as shown in tables 1 and 2.
TABLE 1 uncured plate data
TABLE 2 cured plate data
The corrosion weight column in table 1 is the amount of weight reduction of the grid after the lead paste is knocked off from the uncured plate and the plate is charged and treated with sugar and alkali according to the above expression method, and the part of the reduced weight is actually caused by corrosion of the grid by current during charging; the corrosion weight column in the table is the weight reduction of the grid after the solidified plate is knocked off the lead paste and is subjected to charging and sugar-alkali treatment according to the expression method, the weight reduction is actually the corrosion of the grid caused by current during charging and the corrosion formed in the solidification process, the weight of the corrosion layer formed in the solidification process can be obtained by subtracting the average value of the corrosion weight of the current in the table 1, and the weight column of the corrosion layer in the table 2 is the weight of the finally required corrosion layer.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and alterations without departing from the spirit and scope of the present invention, and all equivalent changes, modifications and alterations to the present invention are equivalent embodiments of the present invention; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (9)
1. The method for detecting the corrosion layer of the green plate is characterized by comprising the following steps of:
a) removing lead plaster from the smeared wet grid, cleaning, drying in vacuum, welding a lead on a lug of the wet grid, weighing the lead and recording the weight as m1；
b) Removing lead plaster from the cured dry green grid, cleaning, drying in vacuum, welding a lead on a tab of the dry green grid, weighing the lead and the lead as M1；
c) Placing the wet grid in the step a) and the dry grid in the step b) in different cells, and connecting the two cells in series to form a battery by adopting a normal negative plate as a negative electrode;
d) adding sulfuric acid into the single cells in the step c), and charging after soaking;
e) the charging is divided into two steps;
f) taking out the wet raw grid and the dry raw grid after charging, washing, putting the washed wet raw grid and the dry raw grid into a sugar-alkali solution, boiling for 25-45mnin, washing and then drying in vacuum;
g) weighing the dried wet green grids in the step f), and recording the weights as m2And f) weighing the dried dry green grid in the step f), and recording as M2；
The corrosion layer calculation method comprises the following steps: n ═ M1-M2)-(m1-m2) (ii) a Wherein, n: weight of corrosion layer formed during curing, g.
2. The method for detecting the corrosion layer of the green plate as claimed in claim 1, wherein 700-8% is added into each unit cell in the step d)00g, density 1.25-1.35g/cm3Sulfuric acid (c).
3. The method for detecting the corrosion layer of the green plate according to claim 1, wherein in the step d), the green plate is kept still for 24-30 hours after the sulfuric acid is added.
4. The method for detecting the corrosion layer of the green plate as claimed in claim 1, wherein in the step e), the first charging is performed for 25-35min at a charging rate of 0.4-0.6A, and the second charging is performed for 1-5h at a charging rate of 2.8-3.2A.
5. The method for detecting the corrosion layer of the green plate as claimed in claim 4, wherein in the step e), the first charging is performed for 30min at 0.5A, and the second charging is performed for 3h at 3A.
6. The method for detecting the corrosion layer of the green plate as claimed in claim 1, wherein the sugar alkali solution is prepared by adding 15-25g of glucose and 95-110g of sodium hydroxide to 1L of distilled water in step f).
7. The method for detecting the corrosion layer of the green plate as claimed in claim 6, wherein the amount of the sugar alkali solution is 3-8 times of the total weight of the wet green grid and the dry green grid.
8. The method for detecting the corrosion layer of the green plate according to claim 1, further comprising a step h) of error verification, wherein a plurality of wet green grids in the step a) and dry green grids in the step b) are taken, and an average value of weight differences before and after corrosion is calculated, and the calculation method comprises the following steps:
wherein the content of the first and second substances,
g, the average value of the weight difference of the dry-green grid before and after charging;
average of weight difference before and after charging, g, for wet green grids.
9. The method for detecting the corrosion layer of the green plate according to claim 8, wherein in the step h), 5 wet green grids and 5 dry green grids are taken to calculate an average value.
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| CN202110797478.1A CN113607595A (en) | 2021-07-14 | 2021-07-14 | Detection method of green plate corrosion layer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114544418A (en) * | 2022-01-27 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Polar plate performance determination method based on positive plate grid corrosion layer and paste adhesion of lead storage battery |
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| CN104075960A (en) * | 2014-06-27 | 2014-10-01 | 天能集团江苏科技有限公司 | Method for rapidly determining corrosion resistance of storage battery grid alloy |
| CN106323852A (en) * | 2016-08-23 | 2017-01-11 | 天能电池集团有限公司 | Test method for corrosion- resistance performance contrast of lead-acid battery grid |
| CN107219145A (en) * | 2017-04-21 | 2017-09-29 | 超威电源有限公司 | A kind of method for measuring battery grid extent of corrosion |
| KR20200045224A (en) * | 2018-10-22 | 2020-05-04 | 주식회사 한국아트라스비엑스 | Manufacture of gold-plated grid for the production of lead-acid batteries for high temperature regions and lead acid battery |
| CN111595761A (en) * | 2019-04-11 | 2020-08-28 | 湖北骆驼海峡新型蓄电池有限公司 | Method for testing corrosion resistance of positive plate grid |
-
2021
- 2021-07-14 CN CN202110797478.1A patent/CN113607595A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104075960A (en) * | 2014-06-27 | 2014-10-01 | 天能集团江苏科技有限公司 | Method for rapidly determining corrosion resistance of storage battery grid alloy |
| CN106323852A (en) * | 2016-08-23 | 2017-01-11 | 天能电池集团有限公司 | Test method for corrosion- resistance performance contrast of lead-acid battery grid |
| CN107219145A (en) * | 2017-04-21 | 2017-09-29 | 超威电源有限公司 | A kind of method for measuring battery grid extent of corrosion |
| KR20200045224A (en) * | 2018-10-22 | 2020-05-04 | 주식회사 한국아트라스비엑스 | Manufacture of gold-plated grid for the production of lead-acid batteries for high temperature regions and lead acid battery |
| CN111595761A (en) * | 2019-04-11 | 2020-08-28 | 湖北骆驼海峡新型蓄电池有限公司 | Method for testing corrosion resistance of positive plate grid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114544418A (en) * | 2022-01-27 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Polar plate performance determination method based on positive plate grid corrosion layer and paste adhesion of lead storage battery |
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