A kind of detection method of elemental manganese in lithium manganese phosphate

A detection method and technology for lithium manganese phosphate, applied in the field of chemical analysis, can solve the problems of difficulty in detecting the content of elemental manganese, inability to separate lithium manganese phosphate, and reduced cycle stability, achieving convenient on-site detection, accurate endpoint judgment, and easy observation. Effect

Active Publication Date: 2015-08-12
SHENZHEN DYNANONIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Lithium manganese phosphate as a lithium ion cathode material makes the battery have better performance, but if the lithium manganese phosphate contains elemental manganese, it will have a great impact on the performance of the material, seriously affecting the performance of the battery, resulting in a decrease in battery capacity, cycle stability, and battery short circuit. and many more
[0003] At present, the detection methods for elemental manganese are basically to dissolve the sample with an acid solution before detection, and the divalent manganese in lithium manganese phosphate is also dissolved in the acid solution, and the detected manganese content is the total manganese content in lithium manganese phosphate, Because lithium manganese phosphate is only soluble in acid solution, not in alkaline solution, and elemental manganese and acid will also react and dissolve, making it difficult to detect the content of elemental manganese under acidic conditions
Although elemental manganese can react with hot water to release hydrogen, the resulting precipitate Mn(OH) 2 Inseparable from lithium manganese phosphate, the equation is as follows: Mn+2H 2 O=Mn(OH) 2 ↓+H 2 ↑; To detect the content of elemental manganese in lithium manganese phosphate, it is necessary to find a method to separate lithium manganese phosphate and elemental manganese to avoid interference during the detection process

Method used

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  • A kind of detection method of elemental manganese in lithium manganese phosphate
  • A kind of detection method of elemental manganese in lithium manganese phosphate
  • A kind of detection method of elemental manganese in lithium manganese phosphate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0057] Mix 9.00g of elemental manganese in every 1.00g of pure lithium manganese phosphate, and detect it as a sample, including the following steps:

[0058] (1) Weigh 0.12g of the sample into a conical flask, put it into a stirring bar, add 60mL of ammonium nitrate-ammonia buffer solution, and stir evenly;

[0059] (2) Put the sample obtained in step (1) on the stirrer immediately and heat it for 10 minutes. 100mL volumetric flask, constant volume;

[0060] (3) Pipette 25mL of the solution obtained in step (2) into an Erlenmeyer flask, add 15mL of phosphoric acid, mix well, place on a high-temperature electric furnace to heat, the solution evaporates until phosphoric acid fumes come out, and the temperature is about 220-240°C , stop heating;

[0061] (4) Immediately add 4.0g ammonium nitrate, shake well, let it stand still, remove nitrogen oxides, cool to 50°C, add 60mL deionized water, shake well, continue to cool to room temperature, and then titrate the solution with fe...

Embodiment 2

[0073] Mix 1.00g of elemental manganese in every 9.00g of pure lithium manganese phosphate, and detect it as a sample, including the following steps:

[0074] (1) Weigh 1.15g of the sample into a conical flask, put it into a stirrer, add 60mL of ammonium nitrate-ammonia buffer solution, and stir evenly;

[0075] (2) Put the sample obtained in step (1) on the stirrer immediately, heat for 20 minutes, after the end, use four layers of slow-speed filter paper, add pulp, and filter under reduced pressure; wash 8 times with deionized water, combine the filtrates, and transfer to 100mL volumetric flask, constant volume;

[0076] (3) Pipette 25mL of the solution obtained in step (2) into an Erlenmeyer flask, add 15mL of phosphoric acid, mix well, place on a high-temperature electric furnace to heat, the solution evaporates until phosphoric acid fumes come out, and the temperature is about 220-240°C , stop heating;

[0077] (4) Immediately add 3.0g ammonium nitrate, shake well, let ...

Embodiment 3

[0090] Mix 0.05g elemental manganese in every 9.95g pure lithium manganese phosphate, detect as sample, comprise the following steps:

[0091] (1) Weigh 15.56g of the sample into a conical flask, put it into a stirrer, add 60mL of phosphate buffer (pH7.6), and stir evenly;

[0092] (2) Put the sample obtained in step (1) on the stirrer immediately and heat it for 10 minutes. 100mL volumetric flask, constant volume;

[0093] (3) Pipette 25mL of the solution obtained in step (2) into an Erlenmeyer flask, add 15mL of phosphoric acid, mix well, place on a high-temperature electric furnace to heat, the solution evaporates until phosphoric acid fumes come out, and the temperature is about 220-240°C , stop heating;

[0094] (4) Immediately add 2.0g ammonium nitrate, shake well, let it stand still, remove nitrogen oxides, cool to 50°C, add 60mL deionized water, shake well, continue to cool to room temperature, and then titrate the solution with ferrous ammonium sulfate standard Tit...

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Abstract

The invention provides a detection method of simple substance manganese in lithium manganese phosphate, which realizes the separation of lithium manganese phosphate from simple substance manganese by dissolving simple substance manganese in a hot solution containing a buffer solution, and thus realizes simple and accurate detection of the simple substance manganese content in lithium manganese phosphate; the invention has the advantages of simple method, convenient operation, accurate end point determination, good reproducibility, and accurate data, and has wide industrial applications.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for detecting elemental manganese in lithium manganese phosphate. Background technique [0002] Lithium manganese phosphate as a lithium ion cathode material makes the battery have better performance, but if the lithium manganese phosphate contains elemental manganese, it will have a great impact on the performance of the material, seriously affecting the performance of the battery, resulting in a decrease in battery capacity, cycle stability, and battery short circuit. etc. [0003] At present, the detection methods for elemental manganese are basically to dissolve the sample with an acid solution before detection, and the divalent manganese in lithium manganese phosphate is also dissolved in the acid solution, and the detected manganese content is the total manganese content in lithium manganese phosphate, Because lithium manganese phosphate is only dissolve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/79
Inventor 孔令涌尚伟丽何艳艳黄永侃赖玉丽
Owner SHENZHEN DYNANONIC
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