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Preparation method of cobalt trifluoride

A technology of cobalt trifluoride and cobalt difluoride, applied in cobalt halide and other directions, can solve problems such as unclear structure, achieve good fluorination effect, ensure internal and external reactions, and reduce fluorine gas consumption.

Active Publication Date: 2019-11-01
HUBEI ZHUOXI FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cobalt trifluoride also has hydrates, CoF 3 3.5H 2 O, but the structure is unclear

Method used

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  • Preparation method of cobalt trifluoride
  • Preparation method of cobalt trifluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method for cobalt trifluoride, said method comprising the steps of:

[0024] Step 1, pulverize 2000g coke, mix with the ammonium chloride of 50g;

[0025] Step 2, transfer to the reactor for fluorination production. The reaction kettle has a heating device, and a drying device is installed at the outlet of the tail gas of the reaction kettle, and the tail gas is passed into an aqueous potassium hydroxide solution for absorption. After starting the heating device and raising the temperature to 50°C, start feeding fluorine gas until the pressure in the kettle is 2 kg, continue to raise the temperature to 200°C to start the reaction, and evacuate the pressure in the kettle after 20 minutes. Continue to feed fluorine gas to a pressure of 2 kg to continue the reaction. During the whole reaction process, the temperature in the kettle was controlled at about 200°C.

[0026] Until the completion of the reaction, 1200 g of fluorine gas was consumed. A total of ...

Embodiment 2

[0028] A preparation method for cobalt trifluoride, said method comprising the steps of:

[0029] Step 1, pulverize 2100g of coke and mix with 35g of ammonium chloride;

[0030] Step 2, transfer to the reactor for fluorination production. The reaction kettle has a heating device, and a drying device is installed at the outlet of the tail gas of the reaction kettle, and the tail gas is passed into an aqueous potassium hydroxide solution for absorption. After starting the heating device and raising the temperature to 50°C, start feeding fluorine gas until the pressure in the kettle is 1.8 kg, continue to raise the temperature to 190°C to start the reaction, and evacuate the pressure in the kettle after 20 minutes. Continue to feed fluorine gas to a pressure of 1.8 kg to continue the reaction. During the whole reaction process, the temperature in the kettle was controlled at about 190°C.

[0031] Until the completion of the reaction, 1280g of fluorine gas was consumed. A tota...

Embodiment 3

[0033] A preparation method for cobalt trifluoride, said method comprising the steps of:

[0034] Step 1, pulverize 2000g of coke and mix with 100g of ammonium chloride;

[0035] Step 2, transfer to the reactor for fluorination production. The reaction kettle has a heating device, and a drying device is installed at the outlet of the tail gas of the reaction kettle, and the tail gas is passed into an aqueous potassium hydroxide solution for absorption. After starting the heating device and raising the temperature to 50°C, start feeding fluorine gas until the pressure in the kettle is 2.2 kg, continue to heat up to 210°C to start the reaction, and evacuate the pressure in the kettle after 20 minutes. Continue to feed fluorine gas to a pressure of 2.2 kg to continue the reaction. During the whole reaction process, the temperature in the kettle was controlled at about 210°C.

[0036] Until the completion of the reaction, 1210 g of fluorine gas was consumed. A total of 2369 g ...

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Abstract

The invention provides a preparation method of cobalt trifluoride, which comprises the following steps: step 1, mixing cobalt difluoride with ammonium salt in a weight ratio of (20-60):1; 2, feeding the reactants into a reaction kettle, and feeding fluorine gas to carry out fluorination reaction. According to the preparation method, cobalt difluoride and ammonium salt are mixed and then fed into areaction kettle before fluorination production, so that the fluorine consumption is reduced, and the content of cobalt trifluoride in a final product is increased. The content of cobalt trifluoride in the produced cobalt trifluoride product can reach 95.81%, and the content of cobalt difluoride does not exceed 5%.

Description

technical field [0001] The invention relates to the technical field of lithium battery materials, in particular to a preparation method of cobalt trifluoride. Background technique [0002] Cobalt trifluoride (chemical formula: CoF 3 ), it is an unstable light brown deliquescent solid at room temperature, with a density of 3.88g / mL (25°C), dissolves in water and releases oxygen, and is a very commonly used fluorinating agent. in CO 2 When heated to 250°C in the air stream, it begins to emit F 2 , at 350°C, it completely transforms into CoF 2 . Cobalt trifluoride can react with many metals or non-metal elements to form corresponding fluorides, which can be reduced to cobalt difluoride itself. Cobalt trifluoride also has hydrates, CoF 3 3.5H 2 O, but the structure is unclear. When using cobalt trifluoride to fluorinate organic compounds, first react cobalt difluoride and fluorine gas at about 300°C to form cobalt trifluoride, and then introduce organic reactants to reac...

Claims

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Application Information

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IPC IPC(8): C01G51/08
CPCC01G51/08C01P2006/80
Inventor 谢子卓谢学归谢洁珊张雨寒于铉
Owner HUBEI ZHUOXI FLUOROCHEM
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