CN103308419A - Method for testing content of barium sulfate for negative plate of storage battery - Google Patents

Method for testing content of barium sulfate for negative plate of storage battery Download PDF

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Publication number
CN103308419A
CN103308419A CN2013102625258A CN201310262525A CN103308419A CN 103308419 A CN103308419 A CN 103308419A CN 2013102625258 A CN2013102625258 A CN 2013102625258A CN 201310262525 A CN201310262525 A CN 201310262525A CN 103308419 A CN103308419 A CN 103308419A
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hydrochloric acid
filtrates
barium sulfate
testing
minutes
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茆黎明
孙月姐
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Zhejiang Tianneng Battery Jiangsu Co Ltd
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Zhejiang Tianneng Battery Jiangsu Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10Energy storage using batteries

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Abstract

The invention discloses a method for testing the content of barium sulfate for a negative plate of a storage battery. By taking anion sulfate ions of a filtrate as invariant, the content of the barium sulfate is calculated in a constant manner, and the method is different from the existing test method with the idea in which solids are placed on filter paper, lotion is used for washing and the precipitation operation is performed. The method is simple and convenient, easy to learn, and capable of reducing the loss of the barium sulfate and improving the accuracy of barium sulfate content tests.

Description

A kind of accumulator negative plate barium sulfate content method of testing
Technical field
The present invention relates to accumulator production field, be specifically related to a kind of battery terminal negative utmost point barium sulfate content method of testing.
Background technology
Barium sulphate, molecular formula are BaSO4, white crystal, and 1580 ℃ of fusing points are insoluble in water and acid, can be used as paint, printing ink, rubber, plastics industry and make filler, and the filling agent of para tape also is used for pigment, pottery, accumulator, enamel, in the industry such as glass and spices.
Barium sulphate as battery terminal negative lead plaster adjuvant, has the lattice parameter approximate with lead sulfate in accumulator, be same eutectic substance, plays the effect of postponing passivation and preventing plumbous surface area shrinkage in charge and discharge process.Traditional barium sulfate content method of testing is according to GB/T 2899-2008, this method is take barium ion as invariant, and the barium sulphate dissolving is precipitated again, and process is more loaded down with trivial details, partial loss is arranged in the operating process unavoidably, cause the barium sulfate content that tests out more on the low side than actual content.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of accumulator negative plate barium sulfate content method of testing, take the anion sulfate acid radical ion as invariant, the content of constant calculating barium sulphate, method of testing is easy, easy operating, improves the order of accuarcy of test barium sulfate content.
The present invention is achieved through the following technical solutions:
A kind of accumulator negative plate barium sulfate content method of testing, the method may further comprise the steps: the sample that takes by weighing quality and be M1 is coated in the natrium carbonicum calcinatum and potassium carbonate mixtures that mass ratio is 1:1~3, in 800 ℃ ± 20 ℃ lower meltings 40~100 minutes, taking-up is cooled to room temperature, then soaking to melt with 50~90 ℃ hot water makes it fully loose, the filtration supernatant liquor is continued to employ, fully wash insolubles with 40~70 ℃ 2%~5% hot sodium carbonate liquor again, till the sulfate radical-free ion, discard filter residue and leave and take whole filtrates to the insolubles; In filtrate, added in the pure 1+1 of quantitative analysis~3 hydrochloric acid solutions and sodium carbonate, after heating is boiled 2 minutes, stir lower 5%~20% barium chloride solution that at the uniform velocity drips, boiling water bath kept 1~3 hour, cooling, filter, sediment with 50~90 ℃ hot wash extremely without till the chlorion; Sediment in 600 ℃ ± 20 ℃ lower calcinations to quality constant weight M2, is recorded barium sulfate content in massfraction X, be calculated as follows: X=M2/M1 * 100%.
The further improvement project of the present invention is, Described usefulness 2%~5% sodium carbonate liquor fully washs insolubles, the method of inspection to the insolubles till the sulfate radical-free ion is, get 2 milliliters of filtrates, add successively 2 1+1~3 hydrochloric acid solutions and 0.5 milliliter of 5~20% barium chloride solution, leave standstill 10 minutes rear filtrates and still keep transparent.
The present invention further improvement project is, describedly added in the filtrate in the pure 1+1 hydrochloric acid solution of quantitative analysis and the sodium carbonate step comprises and drips 2~3 of 0.5%~1% methyl orange indicators first in filtrate, and added again to analyze and added again 2 milliliters of the pure 1+1 of component analysis~3 hydrochloric acid solutions after pure 1+1~3 hydrochloric acid solution neutralization filtrates redden.
The present invention further improvement project is, described sediment to without the method for inspection till the chlorion being, is got 2 milliliters of filtrates with hot wash, adds 0.5 milliliter of 1%~3% liquor argenti nitratis ophthalmicus, leaves standstill that solution still keeps transparent after 10 minutes.
The present invention further improvement project is, 5%~20% barium chloride solution process that at the uniform velocity drips under the described stirring is, dropwise adds 5%~20% barium chloride solution, leave standstill a period of time after, in supernatant liquor, add again 1-2 and drip, produce without muddy, stop dripping.
The present invention further improvement project is that described filtration step adopts at a slow speed quantitative filter paper filtration.
The present invention further improvement project is that described filter paper and sediment are with putting calcination.
The present invention compared with prior art has following obvious advantage:
One, existing detection method is to get solid on the filter paper, and with the washing lotion washing, more loaded down with trivial details, the present invention gets filtrate, and take the anion sulfate acid radical ion as invariant, the content of constant calculating barium sulphate has changed a kind of thinking of precipitation, is easy to grasp.
Two, existing detection method need to be with six dissolution precipitations of (1+1) hydrochloric acid of 30ml heat, and more loaded down with trivial details, the present invention only need add excessive (1+1) hydrochloric acid, in and sodium carbonate, simplified step, reduced the loss of barium sulphate, make the result more accurate.
Embodiment
Embodiment 1
The reagent preparation
Hydrochloric acid (density is 1.18g/ml): 1+1
Sodium carbonate liquor: 2% (in mass ratio preparation)
Barium chloride solution: 10%(prepares in mass ratio)
Methyl orange indicator: 0.5% (in mass ratio preparation)
Molten mixture: 2g natrium carbonicum calcinatum+2g sal tartari
Liquor argenti nitratis ophthalmicus: 2%(prepares in mass ratio)
Take by weighing approximately the sample of drying of 1g, be accurate to 0.0002g, place the platinum crucible that adds the 4g molten mixture, then on it, build again the 4g molten mixture, crucible is placed in the high temperature furnace, in 800 ℃ ± 20 ℃ lower meltings 40 minutes, take out cooling; , soak and melt with 100 milliliters~150 milliliters 80 ℃ of hot water in whole white transfer of melt to 250 ml beakers in the crucible with the glass bar that wraps rubber tip, heating is boiled to fused mass loose.Leave standstill a moment, first supernatant liquor is filtered with quantitative filter paper at a slow speed and to continue to employ, then use 70 ℃ natrium carbonicum calcinatum solution washing insolubles, wash to the insolubles the (method of inspection: get 2 milliliters of filtrates till the sulfate radical-free, add 2 hydrochloric acid solutions and 0.5 milliliter of barium chloride solution, solution should keep transparent after 10 minutes), discard filter residue and leave and take whole filtrates; In filtrate, add 2~3 methyl orange indicators, with (1+1) hydrochloric acid solution neutralization filtrate, after reddening, filtrate adds again 2 milliliters of excessive (1+1) hydrochloric acid solutions, boiled 2 minutes in heating, under constantly stirring, add 20 milliliters of barium chloride solutions with even speed, after leaving standstill a period of time, in supernatant liquor, add again 1-2 and drip barium chloride, produce without muddy, stop dripping, reaction is finished, then beaker is placed on the boiling water bath and kept 2 hours, filter with quantitative filter paper at a slow speed after the cooling, sediment with 70 ℃ of hot washes extremely without (method of inspection is got two milliliters of filtrates till the chlorion, add 0.5 milliliter of liquor argenti nitratis ophthalmicus, solution should keep transparent after 10 minutes).Place the porcelain of pre-burn to do in the pot together with filter paper sediment, dry, ashing, and in high-temperature electric resistance furnace with 600 ℃ ± 20 ℃ lower calcinations to constant mass 0.9795g.
Result's expression and calculating:
Barium sulfate content is in massfraction X, and numerical value represents with %, is calculated as follows:
X=M2/M1×100%
Figure DEST_PATH_IMAGE002A
=0.9795/1×100%=97.95%
In the formula: M2 is the barium sulphate quality after the calcination, the g of unit.
M1 is the quality of sample, the g of unit.
Embodiment 2
The reagent preparation
Hydrochloric acid (density is 1.19g/ml): 1+3
Sodium carbonate liquor: 5% (in mass ratio preparation)
Barium chloride solution: 20%(prepares in mass ratio)
Methyl orange indicator: 1% (in mass ratio preparation)
Molten mixture: 2g natrium carbonicum calcinatum+3g sal tartari
Liquor argenti nitratis ophthalmicus: 3%(prepares in mass ratio)
Take by weighing approximately the sample of drying of 1.5g, be accurate to 0.0002g, place the platinum crucible that adds the 4g molten mixture, then on it, build again the 4g molten mixture, crucible is placed in the high temperature furnace, in 800 ℃ ± 20 ℃ lower meltings 40 minutes, take out cooling; , soak and melt with 100 milliliters~150 milliliters 80 ℃ of hot water in whole white transfer of melt to 250 ml beakers in the crucible with the glass bar that wraps rubber tip, heating is boiled to fused mass loose.Leave standstill a moment, first supernatant liquor is filtered with quantitative filter paper at a slow speed and to continue to employ, then use 70 ℃ natrium carbonicum calcinatum solution washing insolubles, wash to the insolubles the (method of inspection: get 2 milliliters of filtrates till the sulfate radical-free, add 2 hydrochloric acid solutions and 0.5 milliliter of barium chloride solution, solution should keep transparent after 10 minutes), discard filter residue and leave and take whole filtrates; In filtrate, add 2~3 methyl orange indicators, with (1+1) hydrochloric acid solution neutralization filtrate, after reddening, filtrate adds again 2 milliliters of excessive (1+1) hydrochloric acid solutions, boiled 2 minutes in heating, under constantly stirring, add 20 milliliters of barium chloride solutions with even speed, after leaving standstill a period of time, in supernatant liquor, add again 1-2 and drip barium chloride, produce without muddy, stop dripping, reaction is finished, then beaker is placed on the boiling water bath and kept 2 hours, filter with quantitative filter paper at a slow speed after the cooling, sediment with 70 ℃ of hot washes extremely without (method of inspection is got two milliliters of filtrates till the chlorion, add 0.5 milliliter of liquor argenti nitratis ophthalmicus, solution should keep transparent after 10 minutes).Place the porcelain of pre-burn to do in the pot together with filter paper sediment, dry, ashing, and in high-temperature electric resistance furnace with 600 ℃ ± 20 ℃ lower calcinations to constant mass 1.4745g.
Result's expression and calculating:
Barium sulfate content is in massfraction X, and numerical value represents with %, is calculated as follows:
X=M2/M1×100%
Figure DEST_PATH_IMAGE002AA
=1.4745/1.5×100%=98.3%
In the formula: M2 is the barium sulphate quality after the calcination, the g of unit.
M1 is the quality of sample, the g of unit.

Claims (7)

1. accumulator negative plate barium sulfate content method of testing, it is characterized in that, the method may further comprise the steps: the sample that takes by weighing quality and be M1 is coated in the natrium carbonicum calcinatum and potassium carbonate mixtures that mass ratio is 1:1~3, in 800 ℃ ± 20 ℃ lower meltings 40~100 minutes, taking-up is cooled to room temperature, then soaking to melt with 50~90 ℃ hot water makes it fully loose, the filtration supernatant liquor is continued to employ, fully wash insolubles with 40~70 ℃ 2%~5% hot sodium carbonate liquor again, till the sulfate radical-free ion, discard filter residue and leave and take whole filtrates to the insolubles; In filtrate, added in the pure 1+1 of quantitative analysis~3 hydrochloric acid solutions and sodium carbonate, after heating is boiled 2 minutes, stir lower 5%~20% barium chloride solution that at the uniform velocity drips, boiling water bath kept 1~3 hour, cooling, filter, sediment with 50~90 ℃ hot wash extremely without till the chlorion; Sediment in 600 ℃ ± 20 ℃ lower calcinations to quality constant weight M2, is recorded barium sulfate content in massfraction X, be calculated as follows: X=M2/M1 * 100%.
2.
Figure 2013102625258100001DEST_PATH_IMAGE002
. method of testing according to claim 1, it is characterized in that: described usefulness 2%~5% sodium carbonate liquor fully washs insolubles, the method of inspection to the insolubles till the sulfate radical-free ion is, get 2 milliliters of filtrates, add successively 2 1+1~3 hydrochloric acid solutions and 0.5 milliliter of 5~20% barium chloride solution, leave standstill 10 minutes rear filtrates and still keep transparent.
3. method of testing according to claim 1, it is characterized in that: describedly added in the filtrate in the pure 1+1 hydrochloric acid solution of quantitative analysis and the sodium carbonate step comprises and drips 2~3 of 0.5%~1% methyl orange indicators first in filtrate, and added again to analyze and added again 2 milliliters of the pure 1+1 of component analysis~3 hydrochloric acid solutions after pure 1+1~3 hydrochloric acid solution neutralization filtrates redden.
4. method of testing according to claim 1 is characterized in that: described sediment to without the method for inspection till the chlorion being, is got 2 milliliters of filtrates with hot wash, adds 0.5 milliliter of 1%~3% liquor argenti nitratis ophthalmicus, leaves standstill that solution still keeps transparent after 10 minutes.
5. according to claim 1 described method of testing, it is characterized in that: 5%~20% barium chloride solution process that at the uniform velocity drips under the described stirring is dropwise to add 5%~20% barium chloride solution, after leaving standstill a period of time, in supernatant liquor, add again 1-2 and drip, produce without muddy, stop dripping.
6. method of testing according to claim 1 is characterized in that: described filtration step adopts at a slow speed that quantitative filter paper filters.
7. method of testing according to claim 6 is characterized in that: described filter paper and sediment are with putting calcination.
CN2013102625258A 2013-06-27 2013-06-27 Method for testing content of barium sulfate for negative plate of storage battery Pending CN103308419A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN104237059A (en) * 2014-09-25 2014-12-24 武汉钢铁(集团)公司 Determination method of sulfate radical content in chromium plating solution
CN105987900A (en) * 2015-01-27 2016-10-05 张家港市国泰华荣化工新材料有限公司 Detection method of sulfate ion in electrolyte used for lithium ion battery
CN106018160A (en) * 2016-06-24 2016-10-12 安徽创新检测技术有限公司 Method for measuring content of water-soluble and acid-soluble sulfate in soil
CN111678835A (en) * 2020-06-22 2020-09-18 浙江天能电池(江苏)有限公司 Method for measuring content of silicon dioxide in silica sol for storage battery
CN113740199A (en) * 2021-08-30 2021-12-03 承德建龙特殊钢有限公司 Method for measuring sulfur content in sulfur cored wire
CN114112770A (en) * 2021-11-17 2022-03-01 超威电源集团有限公司 Method for detecting uniformity of lead paste of negative electrode of lead-acid storage battery

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CN102323179A (en) * 2011-08-29 2012-01-18 山西太钢不锈钢股份有限公司 Method for detecting sulfur dioxide in desulfurized gypsum

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104237059A (en) * 2014-09-25 2014-12-24 武汉钢铁(集团)公司 Determination method of sulfate radical content in chromium plating solution
CN105987900A (en) * 2015-01-27 2016-10-05 张家港市国泰华荣化工新材料有限公司 Detection method of sulfate ion in electrolyte used for lithium ion battery
CN105987900B (en) * 2015-01-27 2019-01-29 张家港市国泰华荣化工新材料有限公司 The measuring method of sulfate ion in a kind of electrolyte for lithium ion battery
CN106018160A (en) * 2016-06-24 2016-10-12 安徽创新检测技术有限公司 Method for measuring content of water-soluble and acid-soluble sulfate in soil
CN111678835A (en) * 2020-06-22 2020-09-18 浙江天能电池(江苏)有限公司 Method for measuring content of silicon dioxide in silica sol for storage battery
CN113740199A (en) * 2021-08-30 2021-12-03 承德建龙特殊钢有限公司 Method for measuring sulfur content in sulfur cored wire
CN114112770A (en) * 2021-11-17 2022-03-01 超威电源集团有限公司 Method for detecting uniformity of lead paste of negative electrode of lead-acid storage battery

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Application publication date: 20130918