Method for determining total amount of nickel, cobalt and manganese in NCM material through complexometric titration method

A complexometric titration and material technology, which is applied in the direction of chemical analysis by titration, can solve the problems of long time consumption, poor reproducibility, and errors, and achieves reduction of weighing errors, accurate results, and improved stability. Effect

Inactive Publication Date: 2018-11-30
HUAYOU NEW ENERGY TECH (QUZHOU) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the total amount of nickel, cobalt, and manganese in NCM materials, the traditional method is to use conventional chemical methods to first measure the content of nickel, cobalt, and manganese in the material separately, and then add the three components to get the total amount; therefore, three conventional methods are required. Chemical analysis and test analysis take a long time, and there are errors in each test, so the reproducibility of the total nickel, cobalt and manganese tests is not good
Now, although the industry tries to use EDTA complexometric titration to quickly test the total amount of nickel, cobalt and manganese, there are still many differences in the specific test operations

Method used

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  • Method for determining total amount of nickel, cobalt and manganese in NCM material through complexometric titration method
  • Method for determining total amount of nickel, cobalt and manganese in NCM material through complexometric titration method
  • Method for determining total amount of nickel, cobalt and manganese in NCM material through complexometric titration method

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Embodiment 1

[0077] In this embodiment, high-purity nickel flakes, high-purity cobalt flakes, and high-purity manganese flakes are used to prepare NCM materials with a ratio of 5:2:3. The measured values ​​are measured by the complexometric titration method of the present invention, and the measured values ​​are compared with the theoretical values. To verify the accuracy of the present invention. The specific implementation steps are as follows:

[0078] 1. Calibration of EDTA standard solution

[0079] 1.1) Weigh the reference material

[0080] Take by weighing 0.93g high-purity nickel sheet, its purity and weight are as follows:

[0081] Table 1

[0082] Reference substance name

Nickel content (%)

Sample weight (g)

High-purity nickel sheet

99.99

0.9378

High-purity nickel sheet

99.99

0.9349

[0083] 1.2) Dissolution of Reference Substances

[0084] Put the weighed reference substance in a 250mL beaker, add 30mL of concentrated nitric a...

Embodiment 2

[0123] In this embodiment, high-purity nickel flakes, high-purity cobalt flakes, and high-purity manganese flakes are used to prepare NCM materials with a ratio of 3:3:3. The measured values ​​are measured by the complexometric titration method of the present invention, and the measured values ​​are compared with the theoretical values. To verify the accuracy of the present invention. The specific implementation steps are as follows:

[0124] 1. Calibration of EDTA standard solution

[0125] Adopt the method identical with embodiment 1 to obtain the concentration of EDTA standard solution.

[0126] 2. Preparation of standard samples (preparation of standard solutions of NCM materials with a ratio of 3:3:3)

[0127] 2.1) Nickel standard solution (7500mg / L): Weigh 7.5000g of metallic nickel in a 400mL beaker, add a small amount of water to moisten it, slowly add 50mL of nitric acid, heat at low temperature until completely dissolved, add about 30mL of water and boil to drive o...

Embodiment 3

[0154] In this embodiment, high-purity nickel flakes, high-purity cobalt flakes, and high-purity manganese flakes are used to prepare NCM materials with a ratio of 6:2:2. The measured values ​​are measured by the complexometric titration method of the present invention, and the measured values ​​are compared with the theoretical values. To verify the accuracy of the present invention. The specific implementation steps are as follows:

[0155] 1. Calibration of EDTA standard solution

[0156] Adopt the method identical with embodiment 1 to obtain the concentration of EDTA standard solution.

[0157] 2. Preparation of standard samples (preparation of standard solutions of NCM materials with a ratio of 6:2:2)

[0158] 2.1) Nickel standard solution (7500mg / L): Weigh 7.5000g of metallic nickel in a 400mL beaker, add a small amount of water to moisten it, slowly add 50mL of nitric acid, heat at low temperature until completely dissolved, add about 30mL of water and boil to drive o...

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Abstract

The invention discloses a method for determining the total amount of nickel, cobalt and manganese in a NCM material through a complexometric titration method. In the prior art, the rapid test of the total amount of nickel, cobalt and manganese is performed by using the EDTA complexometric titration method, and a lot of differences exist in the specific test operations. According to the present invention, the auxiliary reagent hydroxylamine hydrochloride is additionally used in the complexometric titration method, wherein the color change at the ending point is significant and the test result is stable and accurate by adding the reagent; during the titration test, the buffer solution and the murexide indicator are added at 1-2 ml position before the ending point, such that the test result is stable and accurate; with the method, the total amount of nickel, cobalt and manganese in the NCM material can be quickly, accurately and stably determined, wherein the test result is close to the real value by verifying the standard sample; and the method has characteristics of low requirements on operators, easy grasping, good reproducibility of test result and significantly-shortened test time, and can completely meet the requirements of large-scale and continuous production.

Description

technical field [0001] The invention belongs to the field of detection and analysis of positive electrode materials of lithium batteries, and relates to a method for rapidly, accurately and stably measuring the total amount of nickel, cobalt and manganese in NCM materials by complexometric titration. Background technique [0002] With the rapid development of new energy technologies, the application of lithium batteries is becoming more and more extensive. At the same time, because people are paying more and more attention to environmental protection, Western European countries, Japan, India, the United States, China and other countries have formulated a timetable for the withdrawal of fuel vehicles, and will replace fuel-powered vehicles with new energy vehicles. [0003] Nickel cobalt lithium manganese oxide (NCM series) lithium-ion battery cathode material has the advantages of high specific capacity, wide discharge voltage range, stable electrochemical performance, and g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 欧阳曦郁惠坤童锋刘茨梅陈要忠
Owner HUAYOU NEW ENERGY TECH (QUZHOU) CO LTD
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