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A kind of preparation method of cobalt trifluoride granulation

A technology of cobalt trifluoride particles and fluorination, applied in cobalt halide and other directions, can solve the problems of high cost, increase the difficulty of production, low production efficiency, etc., and achieve the effect of solving the powdering of cobalt fluoride

Active Publication Date: 2021-03-19
无锡玖和隆工程科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are two kinds of fluorination reactors, one is the fluidized bed reactor, or the stirred tank reactor, because such equipment has the problem of dynamic sealing, there is a great hidden danger in production safety, and the gas phase and solid phase powder are in contact with each other. The reaction efficiency is low, and the reaction generates a large amount of heat, which is difficult to dissipate
The second is a fixed bed reactor. When fluorinating organic compounds, cobalt trifluoride particles are usually added with a small amount of binder to cobalt difluoride, and then pressed into granules by a tablet machine. After drying and roasting, they react with fluorine gas. Cobalt trifluoride is produced. The particles made by this method are very easy to pulverize during the fluorination production process, which greatly increases the difficulty of production, low production efficiency and high cost.

Method used

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  • A kind of preparation method of cobalt trifluoride granulation
  • A kind of preparation method of cobalt trifluoride granulation
  • A kind of preparation method of cobalt trifluoride granulation

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The specific process is as figure 1 shown.

[0024] (1) Ingredients:

[0025] A, drop into cobalt chloride 282kg, aluminum trichloride 12kg, zinc chloride 6kg in reactor (stirred tank formula), promptly add up to drop into cobalt salt mixture 120kg;

[0026] b. Add 1500kg of deionized water into the reactor, stir and dissolve the cobalt salt mixture to form a solution;

[0027] c. Configure 550L of 5% caustic soda in the caustic soda mixing kettle;

[0028] (2) Reaction:

[0029] d, open the reactor agitator, pump 550L of caustic soda with 5% of the caustic soda tank into the reactor;

[0030] e, carry out reaction under stirring condition 10min, stop stirring and generate cobalt hydroxide, zinc hydroxide, aluminum hydroxide precipitation, finally complete reaction and be weak alkaline pH and be 8;

[0031] (3) Press filtration and granulation:

[0032] f, pressure filtration: use the transfer pump at the bottom of the reaction kettle to put cobalt hydroxide, zinc...

Embodiment 2

[0051] (1) Preparation of cobalt salt solution: 94 parts of cobalt chloride, aluminum trichloride part and zinc chloride part are put into the reactor, fully mixed, then 500 parts of deionized water are added, stirred and dissolved to form cobalt salt solution;

[0052] (2) Reaction: pump 150 parts of caustic soda with a mass concentration of 2%-12% into the cobalt salt solution obtained in step (1), stir and react for 20min at a rotating speed of 20r / min, and let it stand for precipitation;

[0053] (3) Pressure filtration and granulation: the precipitate obtained at the bottom of the reaction kettle in step (2) is put into a plate and frame filter press for pressure filtration through a delivery pump, and then washed with water for a second pressure filtration, and the obtained filter cake is dried, and then early granulated On-machine granulation with a mesh number of 20; finally, dry the obtained granules at 60°C for 40 hours and cool naturally;

[0054] (4) Tablet roasting:...

Embodiment 3

[0059] (1) Preparation of cobalt salt solution: 94 parts of cobalt chloride, aluminum trichloride part and zinc chloride part are put into the reactor, fully mixed, then 500 parts of deionized water are added, stirred and dissolved to form cobalt salt solution;

[0060] (2) Reaction: pump 200 parts of caustic soda with a mass concentration of 2%-12% into the cobalt salt solution obtained in step (1), stir and react for 2min at a rotating speed of 200r / min, and let stand for precipitation;

[0061] (3) Pressure filtration and granulation: the precipitate obtained at the bottom of the reaction kettle in step (2) is put into a plate and frame filter press for pressure filtration through a delivery pump, and then washed with water for a second pressure filtration, and the obtained filter cake is dried, and then early granulated Granulate on the machine with a mesh number of 25; finally dry the obtained granules at 100°C for 10 hours, and cool naturally;

[0062] (4) Tablet roastin...

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Abstract

The invention relates to a preparation method of cobaltic fluoride particles, and belongs to the technical field of fluorination catalyst. The preparation method comprises following steps: cobaltous chloride, zinc chloride, aluminium trichloride, and caustic soda are reacted so as to obtain a hydroxide; the hydroxide is subjected to pressing so as to obtain particles, and the particles are subjected to roasting so as to obtain a mixture of cobalt oxide, zinc oxide, and aluminium oxide crystals which is a fluorating agent precursor; the fluorating agent precursor is reacted with anhydrous hydrogen fluoride, and then is reacted with fluorine gas so as to obtain the cobaltic fluoride particles. The fluorating agent precursor extremely high in mechanical strength and stability is prepared firstly, and then the cobaltic fluoride particles are prepared, so that cobaltous fluoride efflorescence problem is solved, cobaltous fluoride is converted into cobaltic fluoride effectively, and cobalticfluoride fluorination efficiency is high.

Description

technical field [0001] The invention relates to a method for preparing granulated cobalt trifluoride, which belongs to the technical field of fluorination catalyst preparation. Background technique [0002] Cobalt trifluoride (chemical formula: CoF3), which is an unstable light brown deliquescent solid at room temperature, is a very commonly used fluorinating agent for the preparation of organic fluorine compounds (especially perfluorinated compounds). When cobalt trifluoride is used to fluorinate organic compounds, cobalt difluoride and fluorine gas are firstly used to react to form cobalt trifluoride, and then organic reactants are introduced to react with cobalt trifluoride. The cobalt difluoride produced after cobalt trifluoride is reduced can be recycled. [0003] At present, there are mainly two methods for the preparation of cobalt trifluoride, one is to react cobalt chloride with fluorine gas directly to generate cobalt trifluoride; the other is to react cobalt chlo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/08
CPCC01G51/08
Inventor 荀军杨文广张兴臣
Owner 无锡玖和隆工程科技有限公司