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Three-element determination method of nickel-cobalt-manganese ternary material

A ternary material and measurement method technology, which is applied in the direction of chemical analysis by titration method, analysis by making materials undergo chemical reactions, and material analysis by observing the impact on chemical indicators, etc., can solve the problem of low results and high accuracy. Low, error and other issues

Active Publication Date: 2015-01-28
JINGMEN GEM NEW MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The accuracy and precision of the ICP method are poor, and it is easy to cause large errors, while the chemical method detection of cobalt by potentiometric titration and nickel by precipitation method is cumbersome and time-consuming, and is not suitable for large-scale samples. detection
At present, there are also literature reports on the method of measuring single cobalt or nickel by EDTA titration method. For the detection of manganese, there are also literature reports on the detection method of detecting nickel and manganese respectively through precipitated manganese. Reagents such as NaCN are used to seal nickel, but NaCN is poisonous and harmful, and there are also literature reports. Using many reagents such as ammonium persulfate, triethanolamine, hydroxylamine hydrochloride, etc., the operation is cumbersome and the cost is high
In particular, NaCN is extremely toxic and is a highly toxic chemical. Considering safety factors, it is rarely used at present.
In addition, when using EDTA to measure manganese, since Mn 2+ In alkaline media, it is easy to be oxidized in the air, causing EDTA to be unable to coordinate and complex, resulting in low results, and a large amount of cobalt will be adsorbed in the process of manganese precipitation, resulting in detection errors, and the accuracy is low due to these interferences

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0035] Determination of the combined amount of cobalt, nickel and manganese: the sample name of the nickel-cobalt-manganese ternary material is ZJSY14072601 (abbreviated as 1# sample), weigh 1.0000g of the sample, add 10ml of concentrated HCl to heat to completely dissolve the sample, and set the sample after cooling. Fill to a 100ml volumetric flask. Accurately pipette 5ml of sample into a conical flask, add 80mL of water and heat to about 80°C, add 2g of hydroxylamine hydrochloride, 5mL of ammonia water (1:1), titrate with EDTA standard solution to about 1mL before the end point, add 20mL of pH=10 Ammonia-ammonium chloride buffer solution and about 0.2g of ammonium violinate indicator, continue to titrate the solution to bright purple as the end point, record the volume V of EDTA consumed at this time 0 mL.

[0036] Determination of single nickel content: take another 10mL of the tested solution in a 250mL Erlenmeyer flask, add 0.5g of ammonium chloride, then rinse the wal...

example 2

[0047] Determination of the combined amount of cobalt, nickel and manganese: the sample name of the nickel-cobalt-manganese ternary material is ZJSY14072602 (abbreviated as 2# sample), weigh 1.0000g of the sample, add 10ml of concentrated HCl to heat to completely dissolve the sample, and set the sample after cooling. Fill to a 100ml volumetric flask. Accurately pipette 10ml of sample into a conical flask, add 70mL of water and heat to about 75°C, add 1.5g of hydroxylamine hydrochloride, 5mL of ammonia water (1:1), titrate with EDTA standard solution to about 1.5mL before the end point, add 20mL of PH =10 ammonia-ammonium chloride buffer solution and about 0.2g of ammonium viurinate indicator, continue to titrate the solution to bright purple as the end point, and record the volume of EDTA consumed at this time.

[0048] Determination of single nickel content: Take another 10mL of the tested solution in a 250mL conical flask, add 0.5g of ammonium chloride, then rinse the wall ...

example 3

[0052]Determination of the combined amount of cobalt, nickel and manganese: the sample name of the nickel-cobalt-manganese ternary material is ZJSY14072603 (abbreviated as 3# sample), weigh 1.0000g of the sample, add 10ml of concentrated HCl to heat to completely dissolve the sample, and set it after cooling. Fill to a 100ml volumetric flask. Accurately pipette 10ml of sample into a conical flask, add 90mL of water and heat to about 85°C, add 1.5g of hydroxylamine hydrochloride, 5mL of ammonia water (1:1), titrate with EDTA standard solution to about 2mL before the end point, add 20mL of PH= 10% of ammonia-ammonium chloride buffer solution and about 0.2g of ammonium violinate indicator, continue to titrate the solution until the end point is bright purple, and record the volume of EDTA consumed at this time.

[0053] Determination of single nickel content: take another 10mL of the tested solution in a 250mL Erlenmeyer flask, add 1g of ammonium chloride, then rinse the wall of ...

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Abstract

The invention relates to a three-element determination method of a nickel-cobalt-manganese ternary material. The method comprises the following steps: determining the total quantity of cobalt, nickel and manganese ions by EDTA titration and recording titration consumption volume; sampling to an alkaline medium of ammonia chloride and ammonium to form nickel amine, oxidizing cobalt by utilizing hydrogen peroxide, complexing with ammonium to form a trivalent cobalt ammonia complex to generate manganese dioxide precipitate, filtering out the precipitate to obtain the filter liquid, titrating the filter liquid by utilizing EDTA in the presence of murexide serving as an indicator to determine the content of nickel, and recording the titration consumption volume; enabling the ammonia gas to escape from the solution after the nickel is determined through titration under the alkaline and heating condition and generating cobalt hydroxide precipitate at the same time, dissolving the cobalt hydroxide precipitate by utilizing acid, measuring the content of cobalt through EDTA titration, and recording the titration consumption volume; and calculating the respective content of the three elements according to the EDTA consumption volume in each step, the concentration of EDTA and the sample mass. The method is accurate in detection, high in detection efficiency, safe, environment-friendly and applicable to the detection of content of three elements in an anode material.

Description

technical field [0001] The invention relates to the technical field of multi-element content determination, in particular to a three-element determination method for a nickel-cobalt-manganese ternary material. Background technique [0002] With the continuous development of electronic products, lithium-ion batteries have been widely used, and the current electronic products are constantly being updated, and the requirements for lithium-ion battery products are also getting higher and higher. As we all know, the core component of a lithium-ion battery is the cell, and the composition and performance of the positive and negative materials in the cell play a vital role in the electrochemical performance of the battery. [0003] Ternary lithium battery is a new type of lithium battery developed in recent years with ternary materials as the positive electrode. The more commonly used ternary material is nickel-cobalt-manganese ternary material, and its performance is better than a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/79
Inventor 马琳许开华张云河刘文泽
Owner JINGMEN GEM NEW MATERIAL
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