CN111678835A - Method for measuring content of silicon dioxide in silica sol for storage battery - Google Patents
Method for measuring content of silicon dioxide in silica sol for storage battery Download PDFInfo
- Publication number
- CN111678835A CN111678835A CN202010571629.7A CN202010571629A CN111678835A CN 111678835 A CN111678835 A CN 111678835A CN 202010571629 A CN202010571629 A CN 202010571629A CN 111678835 A CN111678835 A CN 111678835A
- Authority
- CN
- China
- Prior art keywords
- content
- sample
- hydrochloric acid
- solution
- filter paper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
Abstract
The invention discloses a method for measuring the content of silicon dioxide in silica sol for a storage battery, which comprises the following steps: s1: weighing a sample: weighing a sample in a ceramic crucible, wherein the mass of the sample is m1Represents; s2: sample dissolution: slowly adding hydrochloric acid, heating and concentrating to dryness, cooling, adding hydrochloric acid again, and heating to slight boiling; s3: precipitation and filtration: and (3) adding 12-14ml of bone glue solution into the solution which is heated to slight boiling in S2 while the solution is hot, stirring vigorously for 1-2 min, and adding 15-30ml of hot water. When the method is used for detecting the content of the silicon dioxide in the industrial silica sol, the normal colloid can be filtered through the filter paper, the hydrochloric acid and the bone glue are added to ensure that the silicon dioxide forms a form which can not pass through the filter paper, namely, the bone glue can ensure that the silicon dioxide is condensed and remained on the filter paper, and the sodium oxide is directly filtered out, so that the calculated result does not contain the content of the sodium oxide, and the operation is accurate.
Description
Technical Field
The invention relates to the technical field of lead-acid storage batteries, in particular to a method for measuring the content of silicon dioxide in silica sol for a storage battery.
Background
The valve-controlled lead-acid accumulator for electric booster vehicle is a maintenance-free accumulator, and the electrolyte is added with silicon dioxide as gelatinizer to make sulfuric acid electrolyte become colloidal state, and under the conventional condition it has no flowing electrolyte. Silica sol is used as a material for providing silica, and is required to be checked and accepted when entering a factory, the content of the silica is required to be 30.0-31.0%, and according to the specification of industrial silica sol HG/T2521-2008, the content of the silica is detected as follows:
weighing about 2g of sample by using a porcelain crucible which is pre-burned to constant mass at 800-850 ℃, drying at 105 ℃, then burning to constant mass at 800-850 ℃, and calculating the final result minus the content of sodium oxide. While sodium oxide content provides a general test method, i.e., flame emission photometry. This method has the following problems:
1) the high-end instrument flame emission photometer is needed in the test process, the price is high, and a common laboratory is not necessarily equipped with the photometer.
2) The interference of the flame emission photometry for measuring sodium is large, and the content measurement of sodium oxide is inaccurate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for measuring the content of silicon dioxide in silica sol for a storage battery.
The invention is realized by the following technical scheme:
the invention provides a method for measuring the content of silicon dioxide in silica sol for a storage battery, which comprises the following steps:
s1: weighing a sample: weighing 10-15g of sample in a ceramic crucible, wherein the mass of the sample is m1Represents;
s2: sample dissolution: slowly adding hydrochloric acid, heating and concentrating to dryness, cooling, adding hydrochloric acid again, and heating to slight boiling;
s3: precipitation and filtration: s2, adding 12-14ml of bone glue solution into the solution which is heated to slight boiling while the solution is hot, stirring vigorously for 1-2 min, adding 15-30ml of hot water, filtering and precipitating with medium-speed quantitative filter paper, and washing the precipitate and the filter paper with hot water until no chloride ions exist;
s4: ashing: putting the precipitate and the filter paper in the S3 into a porcelain crucible for ashing, burning at high temperature, cooling to room temperature, and repeatedly burning until the weight is constant m2；
S5: content determination: calculating the content of the silica in the original sample, wherein the content is calculated by X1:
wherein m is1Is the weight of the sample, in g; m is2Is the weight of the dried silica, unit g.
Further, the hydrochloric acid content in the S2 is 36-38%, the volume of the first hydrochloric acid addition is 10ml, and the volume of the second hydrochloric acid addition is 5 ml.
Further, the detection method of no chloride ion in S3 is to take 2% silver nitrate solution on the surface dish and drip several drops of washing solution on the surface dish.
Further, the concentration of the bone glue solution in the S3 is 1% -2%.
Further, the bone glue is purchased from Water-balancing and money-making adhesive company Limited, manufactured according to QB/T1996-2005.
Further, the burning temperature in the S4 is 950-.
The invention has the beneficial effects that:
when the content of the silicon dioxide in the industrial silica sol is detected, normal colloid can be filtered through filter paper, hydrochloric acid and bone glue are added to enable the silicon dioxide to form a form which can not pass through the filter paper, namely the bone glue enables the silicon dioxide to be condensed and remain on the filter paper, and sodium oxide is directly filtered out, the calculated result does not contain the content of the sodium oxide, and the result is accurate in operation;
and reagents and equipment used in the whole detection process are commonly used in laboratories, are low in reagent toxicity and equipment cost, and greatly save the production cost under the condition of meeting the production requirements of enterprises.
Detailed Description
The technical solutions of the present invention will be described in detail below with reference to specific examples, which are provided only for illustrating the present invention in detail and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that many more modifications and variations are possible in light of the above teaching, without necessarily requiring all of the described embodiments to be included herein.
Medium-speed quantitative filter paper: the manufacturer is Hangzhou special paper industry Co., Ltd, model 202, ash content is less than or equal to 0.01, and diameter is 12.5 cm.
The following examples 1 to 3 relate to a test sample obtained from industrial silica sol purchased from energy batteries in Jiangsu province, Inc. in 2019, 12 months and 20 days, and the content of silica therein was measured;
the principle of spot inspection is as follows: sampling at 5%, namely 100 barrels, extracting 5 barrels of 50kg of goods from each barrel, extracting 20ml of goods from each barrel, and mixing together.
Embodiment mode 1
Weighing 10g of sample in a 120mL porcelain crucible, slowly adding 10mL of hydrochloric acid with the content of 36-38%, heating and concentrating the solution to dryness, cooling, adding 5mL of hydrochloric acid with the content of 36-38%, and heating to slight boiling; adding 1% bone glue solution 10mL while hot, stirring vigorously for 1min-2min, adding 20mL hot water, immediately filtering with medium-speed quantitative filter paper, precipitating, and washing with hot water until no chloride ion is detected (with AgNO)3Checking), placing the precipitate and the filter paper in a porcelain crucible with constant weight, carefully ashing, burning for 30min in a high-temperature resistance furnace with the temperature of 950 ℃ and 1000 ℃, then placing in a common glass drier with the caliber of 400mm, cooling to room temperature, repeatedly burning until the constant weight is achieved, namely, the absolute value of the weight difference between the two previous times and the two subsequent times is less than 3 mg.
The detection result is qualified, and the silica sol are mixed to be 1.26g/cm3Diluted sulfuric acid is diluted at a ratio of 1.85:100, stirred, cooled and then added to the battery for charging.
Embodiment mode 2
Weighing 15g of sample in a 120mL porcelain crucible, slowly adding 10mL of hydrochloric acid with the content of 36-38%, heating and concentrating the solution to dryness, cooling, adding 5mL of hydrochloric acid with the content of 36-38%, and heating to slight boiling; adding 10mL of 1.5% bone glue solution while hot, stirring vigorously for 1-2 min, adding 20mL of hot water, immediately filtering with medium-speed quantitative filter paper, precipitating, and washing the filter paper with hot water until no chloride ion is generated (AgNO is used)3Checking), placing the precipitate and the filter paper in a porcelain crucible with constant weight, carefully ashing, burning for 60min in a high-temperature resistance furnace with the temperature of 950 ℃ and 1000 ℃, then placing in a common glass drier with the caliber of 400mm, cooling to room temperature, repeatedly burning until the constant weight is achieved, namely, the absolute value of the weight difference between the two previous times and the two subsequent times is less than 3 mg.
The detection result is not qualified, such as silica sol and 1.26g/cm3Diluted sulfuric acid is diluted according to the proportion of 1.85:100, stirred, cooled and then added into a battery for charging, so that the gelation effect in the later use process is influenced, and unqualified products are caused.
Embodiment 3
Weighing 10g of sample in a 120mL porcelain crucible, slowly adding 10mL of hydrochloric acid with the content of 36-38%, heating and concentrating the solution to dryness, cooling, adding 5mL of hydrochloric acid with the content of 36-38%, and heating to slight boiling; adding 10mL of 2% bone glue solution while hot, stirring vigorously for 1-2 min, adding 20mL of hot water, immediately filtering with medium-speed quantitative filter paper, precipitating, and washing with hot water until no chloride ion is detected (with AgNO)3Checking), placing the precipitate and the filter paper in a porcelain crucible with constant weight, carefully ashing, burning for 30min in a high-temperature resistance furnace with the temperature of 950 ℃ and 1000 ℃, then placing in a common glass drier with the caliber of 400mm, cooling to room temperature, repeatedly burning until the constant weight is achieved, namely, the absolute value of the weight difference between the two previous times and the two subsequent times is less than 3 mg.
The detection result is qualified, and the silica sol are mixed to be 1.26g/cm3Diluted sulfuric acid is diluted at a ratio of 1.85:100, stirred, cooled and then added to the battery for charging.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for measuring the content of silicon dioxide in silica sol for a storage battery is characterized by comprising the following steps:
s1: weighing a sample: weighing 10-15g of sample in a ceramic crucible, wherein the mass of the sample is m1Represents;
s2: sample dissolution: slowly adding hydrochloric acid, heating and concentrating to dryness, cooling, adding hydrochloric acid again, and heating to slight boiling;
s3: precipitation and filtration: s2, adding 12-14ml of bone glue solution into the solution which is heated to slight boiling while the solution is hot, stirring vigorously for 1-2 min, adding 15-30ml of hot water, filtering and precipitating with medium-speed quantitative filter paper, and washing the precipitate and the filter paper with hot water until no chloride ions exist;
s4: ashing: putting the precipitate and the filter paper in the S3 into a porcelain crucible for ashing, burning at high temperature, cooling to room temperature, and repeatedly burning until the weight is constant m2；
S5: content determination: calculating the content of the silica in the original sample, wherein the content is calculated by X1:
wherein m is1Is the weight of the sample, in g; m is2Is the weight of the dried silica, unit g.
2. The method for determining the content of silica in silica sol according to claim 1, wherein the hydrochloric acid content in S2 is 36% -38%, the volume of the first hydrochloric acid addition is 10ml, and the volume of the second hydrochloric acid addition is 5 ml.
3. The method according to claim 1, wherein the chloride ion-free detection method in S3 comprises dropping a few drops of washing solution on a watch glass with a 2% silver nitrate solution.
4. The method for determining the content of silica in silica sol according to claim 1, wherein the concentration of the solution of gelatin in S3 is 1% -2%.
5. The method according to claim 4, wherein the bone glue is purchased from Water-balancing and money-transporting Adhesives GmbH, manufactured according to QB/T1996-2005.
6. The method as set forth in any one of claims 1 to 5, wherein the burning temperature in S4 is 950-1000 ℃ and the burning time is 30-60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010571629.7A CN111678835A (en) | 2020-06-22 | 2020-06-22 | Method for measuring content of silicon dioxide in silica sol for storage battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010571629.7A CN111678835A (en) | 2020-06-22 | 2020-06-22 | Method for measuring content of silicon dioxide in silica sol for storage battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111678835A true CN111678835A (en) | 2020-09-18 |
Family
ID=72436220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010571629.7A Pending CN111678835A (en) | 2020-06-22 | 2020-06-22 | Method for measuring content of silicon dioxide in silica sol for storage battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111678835A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010096592A (en) * | 2008-10-15 | 2010-04-30 | Nippon Steel Corp | Evaluation method of blended iron ore for sintering |
| CN102175684A (en) * | 2011-01-07 | 2011-09-07 | 华东师范大学 | Measuring method of glass phase components of alumina ceramic |
| CN102621030A (en) * | 2012-03-31 | 2012-08-01 | 武汉钢铁(集团)公司 | Method for determining silicon dioxide in limestone and dolomite by using gravimetric method |
| CN102735573A (en) * | 2012-07-06 | 2012-10-17 | 武汉钢铁(集团)公司 | Method for measuring content of silicon dioxide in blast furnace stem |
| CN103308419A (en) * | 2013-06-27 | 2013-09-18 | 浙江天能电池(江苏)有限公司 | Method for testing content of barium sulfate for negative plate of storage battery |
| CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
| CN107436270A (en) * | 2017-07-14 | 2017-12-05 | 南通市产品质量监督检验所 | The assay method of silica usage amount in a kind of formulated food additive |
-
2020
- 2020-06-22 CN CN202010571629.7A patent/CN111678835A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010096592A (en) * | 2008-10-15 | 2010-04-30 | Nippon Steel Corp | Evaluation method of blended iron ore for sintering |
| CN102175684A (en) * | 2011-01-07 | 2011-09-07 | 华东师范大学 | Measuring method of glass phase components of alumina ceramic |
| CN102621030A (en) * | 2012-03-31 | 2012-08-01 | 武汉钢铁(集团)公司 | Method for determining silicon dioxide in limestone and dolomite by using gravimetric method |
| CN102735573A (en) * | 2012-07-06 | 2012-10-17 | 武汉钢铁(集团)公司 | Method for measuring content of silicon dioxide in blast furnace stem |
| CN103308419A (en) * | 2013-06-27 | 2013-09-18 | 浙江天能电池(江苏)有限公司 | Method for testing content of barium sulfate for negative plate of storage battery |
| CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
| CN107436270A (en) * | 2017-07-14 | 2017-12-05 | 南通市产品质量监督检验所 | The assay method of silica usage amount in a kind of formulated food additive |
Non-Patent Citations (2)
| Title |
|---|
| 朱松然: "《铅蓄电池实用手册》", 28 February 1993, 机械工业出版社 * |
| 王娜: ""动物胶凝聚重量法测定超基性岩中的二氧化硅"", 《新疆有色金属》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102539511B (en) | Method for detecting content of bromine in fire retardant through automatic potentiometric titration | |
| CN104034722B (en) | Content of material assay method in a kind of complex silicon carbide | |
| CN107132263A (en) | The method of testing of aluminium composition in aluminium etching solution | |
| CN110907509B (en) | Method for detecting hydrofluoric acid in electronic-grade mixed acid | |
| CN106404814A (en) | Method for measuring potassium content of black powder | |
| KR101431235B1 (en) | Method for detecting content of chitosan fiber in textile | |
| CN105372193A (en) | Detection method of sulfate radical in chromic anhydride | |
| CN111678835A (en) | Method for measuring content of silicon dioxide in silica sol for storage battery | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN106855504B (en) | Method for rapidly determining sulfate radical content | |
| CN113092510A (en) | X-fluorescence determination method for potassium nitrate as high-alumina glass raw material | |
| Fernandopulle et al. | The spectrophotometric determination of fluorine in organic compounds | |
| CN111289686A (en) | Method for measuring content of residual alkali in solution and application thereof | |
| Wagner et al. | Homogeneous precipitation of barium sulfate by hydrolysis of sulfamic acid | |
| CN103760055B (en) | The method of testing of silver content in a kind of silver paste | |
| CN211955359U (en) | Device for measuring chloride ion content of concrete admixture by potentiometric titration method | |
| WO2017071123A1 (en) | Method for testing surface coverage effect of positive electrode active material | |
| CN111366489B (en) | Semi-quantitative detection method for lithium content in primary mixed material sample of ternary cathode material | |
| CN108593636B (en) | Method for measuring calcium fluoride in 90# fluorite | |
| CN113533629B (en) | Method for measuring content of free hydrochloric acid in tellurium tetrachloride sample | |
| CN110715902A (en) | Method for detecting uniformity of positive lead paste of lead-acid storage battery | |
| CN106370685A (en) | Method for determining content of potassium in industrial potassium chloride | |
| CN106093097A (en) | A kind of measure the method for content of strontium in fireworks and firecrackers firework medicament | |
| CN114002205B (en) | Method for measuring impurity element content in optical grade monocalcium phosphate | |
| CN111189818A (en) | Detection box for detecting residual chloride ions on surface of electrode foil as well as preparation method and application of detection box |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200918 |
|
| RJ01 | Rejection of invention patent application after publication |