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Method for reducing and removing nitride in metal lithium or lithium alloy

A lithium alloy and metal lithium technology, applied in the field of lithium metal, can solve the problems affecting the quality of metal lithium or alloy, the inability to remove active metal aluminum, and the inability to remove metal lithium, and achieve a short reaction time, low cost, and strong practicability. Effect

Active Publication Date: 2017-05-31
TIANQI LITHIUM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is only applicable to occasions where N and Ca need to be removed at the same time. If the metal lithium to be treated does not contain Ca, this method will cause a combustion reaction, and the N in the metal lithium cannot be removed.
[0010] In addition, the existing methods are to add active metals such as aluminum as a source of nitrogen removal, and the remaining active metal aluminum will remain in the lithium solution and cannot be removed, resulting in a high residual amount of aluminum.
If there is a slight deviation between the theoretical amount and the actual amount, or there is a large error in the analysis data, the remaining metal aluminum will affect the quality of metal lithium or alloy

Method used

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  • Method for reducing and removing nitride in metal lithium or lithium alloy
  • Method for reducing and removing nitride in metal lithium or lithium alloy
  • Method for reducing and removing nitride in metal lithium or lithium alloy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Example 1 Nitrogen removal by metal lithium with excessive nitrogen content

[0047] Put 1.51 kg of battery-grade lithium metal with nitrogen content exceeding the standard in a sealed reactor, evacuate the reactor to stabilize it to <0.1Pa, and heat the material at a heating rate of 200°C / h. When the lithium metal is completely melted Stop heating and start stirring to ensure that the nitrogen content of each part of the lithium solution is evenly distributed, and then sample and analyze the nitrogen content in the product according to the national standard analysis method, and the measured nitrogen content is 982ppm. Accurately weighed magnesium-aluminum alloys are added to the molten lithium liquid at a molar ratio of Mg-Al:N=1:1. Reheat the reactor, control the temperature rise rate at 100°C / h, and control the reaction temperature at 300°C, the stirring rate is 300rpm, the reaction time is 0.1h, the forward rotation and the reverse rotation account for half, and aft...

Embodiment 2

[0051] Example 2 Processing Lithium Metal under the Changed Situation of Nitrogen Removal Source

[0052] The experimental method is as described in Example 1. The nitrogen removal source in the experiment was changed to obtain the treatment results under different conditions. These factors are the use of metal aluminum-titanium, aluminum-zirconium alloy or magnesium-aluminum alloy (the shape is alloy foil). The test arrangement is shown in Table 2, and the residual amount of nitrogen and nitrogen removal source in the lithium metal after nitrogen removal and the recovery rate of metal lithium are shown in Table 3.

[0053] Table 2

[0054]

[0055] table 3

[0056] Test No. A content (ppm) N content (ppm) Recovery rate of Li (%) 2-1 (Al-Zr)4 41 98 2-2 (Al-Ti)4 38 99 2-3 (Mg-Al)5 44 99 2-4 (Al-Zr)6 41 98 2-5 (Li-Al)3 40 99

Embodiment 3

[0057] Example 3 Nitrogen removal by lithium aluminum alloy with excessive nitrogen content

[0058] Place 1.78kg of lithium aluminum alloy (standard aluminum content is 3000ppm) with excessive nitrogen content due to damaged packaging in a sealed reactor, feed nitrogen into the reactor, and heat the material under the protection of nitrogen. When the alloy is completely melted, stop heating and start stirring to ensure that the nitrogen content in each part of the lithium liquid is evenly distributed, and then take samples to analyze the nitrogen content and aluminum content in the product according to the industry standard analysis method. The measured nitrogen content is 467ppm , the aluminum content is 2915ppm. Add 1.603 g of accurately weighed aluminum-zirconium alloy grains to the molten lithium liquid at a molar ratio of Al-Zr:N=1:1. Reheat the reactor, control the heating rate at 200°C / h, and control the reaction temperature at 600°C, the stirring rate is 300rpm, the ...

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Abstract

The invention relates to a method for reducing and removing nitride in metal lithium or lithium alloy, and belongs to the technical field of lithium metal. The method achieves the technical effect of reducing and removing nitride in metal lithium or lithium alloy. The method comprises the steps that in the vacuum or inert gas shielding atmosphere, metal lithium or lithium alloy is molten and stirred, a nitride removal source A is added for a reaction, the reaction temperature is controlled to be 180-1000 DEG C, the reaction time is 0.1-10 h, sedimentation and filtration are carried out after the reaction is finished, and the filtrate is nitride-removed metal lithium or lithium alloy. The active metal alloy is adopted as the nitride removal source, practicability is high, the cost is low, reaction time is short, and operation is simple and easy to implement. The recovery rate of the metal lithium or lithium alloy treated by the method is 98% or above, meanwhile, the active metal alloy residual quantity is low, the purity of the treated metal lithium or lithium alloy is not affected, and the nitrogen content in the metal lithium or lithium alloy can be reduced to be 50 ppm or below and is far lower than the standard value 300 ppm or below in the national standard.

Description

technical field [0001] The invention relates to a method for reducing nitrides in lithium metal or lithium alloy, and belongs to the technical field of lithium metal. Background technique [0002] Lithium is the lightest metal in nature, silvery white, density 0.534g / cm 3 , a melting point of 180.54°C and a boiling point of 1336°C. Since the Swedish geologist A. Arfvedson first discovered lithium in lepidolite and lepidolite in 1817, lithium has been used in glass ceramics, petrochemicals, metallurgy, aluminum smelting, textiles, synthetic rubber, and lubricating materials. , medical and other traditional fields have been widely used. In recent years, with the increase in the demand for lithium in the above-mentioned traditional fields, and the deepening of research on the development and application of lithium in high-tech fields such as nuclear power generation, aerospace, high-energy-density power batteries, and lightweight high-specific-strength alloys, lithium has bec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/12C22B9/10C22C24/00C22C1/06
CPCC22B9/103C22B26/12C22C1/06C22C24/00
Inventor 曹乃珍徐川刘强高洁邹崴廖仕英
Owner TIANQI LITHIUM CORP
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