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Preparation method of iron(III) fluoride positive material

A cathode material, iron trifluoride technology, applied in the field of preparation of iron trifluoride cathode materials, can solve the problems of complicated operation, increase the shearing of rock samples, and consume manpower, etc., to avoid specific surface area, increase specific surface area, particle size Evenly distributed effect

Active Publication Date: 2018-12-28
郑忆依
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the rock samples are drilled using the wet drilling method, but most of the drilled rock samples do not have fixing devices to fix them during the drilling process, and even need manual support to fix them, which consumes manpower and cannot guarantee the quality of the rock samples. Artificial damage to rock samples
Because artificial support cannot ensure that the force on the rock wall of the rock sample is uniform, this will increase the probability of the rock sample being sheared
[0003] In the existing technology, although there are also devices to fix rock samples during the drilling process, such as the published patent "An Anti-fragmentation Core Sampling Device" [Application No.: 201620652000.4, Application Date: 2016.06.27], the The core is fixed in the environment of particles in the box, but this method is a bit cumbersome to operate for the drilled sample, it is not easy to fix, and it cannot guarantee that the rock sample will not rotate during the drilling process

Method used

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  • Preparation method of iron(III) fluoride positive material
  • Preparation method of iron(III) fluoride positive material
  • Preparation method of iron(III) fluoride positive material

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preparation example Construction

[0025] A preparation method of iron trifluoride positive electrode material, it is the following steps:

[0026] (1) Dissolve high-purity ferrous sulfate crystals in pure water, put them into a sealed reaction kettle, stir and dissolve completely to obtain a ferrous sulfate solution, add urea, and heat up to a temperature of 95-150°C under the protection of an inert atmosphere , stirring and reacting at this temperature for 4-8 hours;

[0027] (2) Cool down the reacted material to a temperature of 5-15°C, then add hydrogen peroxide and hydrofluoric acid solution with stirring at this temperature, maintain the pH of the reaction process at 2-2.5, filter after the addition, and wash with alcohol get crystals;

[0028] (3) adding the crystals to a saturated ferric gluconate solution at a temperature of 5-10°C, then cooling to a temperature of -5°C to 5°C under stirring, filtering, washing with alcohol, and drying to obtain solid particles;

[0029] (4) Put the obtained solid pa...

Embodiment 1

[0039] A preparation method of iron trifluoride positive electrode material, it is the following steps:

[0040] (1) Dissolve high-purity ferrous sulfate crystals in pure water, put them into a sealed reaction kettle, stir and dissolve completely to obtain a ferrous sulfate solution, add urea, and under the protection of an inert atmosphere, heat up to a temperature of 110°C. Stirring reaction under this temperature 6 hours;

[0041] (2) cooling the reacted material to a temperature of 12° C., then adding hydrogen peroxide and hydrofluoric acid solution with stirring at this temperature, maintaining the pH of the reaction process at 2.25, filtering after the addition, and washing with alcohol to obtain crystals;

[0042] (3) adding the crystals to a saturated ferric gluconate solution at a temperature of 8°C, then cooling to a temperature of 2°C under stirring, filtering, washing with alcohol, and drying to obtain solid particles;

[0043] (4) Put the obtained solid particles...

Embodiment 2

[0055] A preparation method of iron trifluoride positive electrode material, it is the following steps:

[0056] (1) Dissolve high-purity ferrous sulfate crystals in pure water, put them into a sealed reaction kettle, stir and dissolve completely to obtain a ferrous sulfate solution, add urea, and under the protection of an inert atmosphere, heat up to a temperature of 120°C. Stirring reaction under this temperature 6.2 hours;

[0057] (2) cooling the reacted material to a temperature of 8° C., then stirring and adding hydrogen peroxide and hydrofluoric acid solution at this temperature, maintaining the pH of the reaction process at 2.1, filtering after the addition, and washing with alcohol to obtain crystals;

[0058] (3) adding the crystals to a saturated ferric gluconate solution at a temperature of 8°C, then cooling to a temperature of -2°C under stirring, filtering, washing with alcohol, and drying to obtain solid particles;

[0059] (4) Put the obtained solid particles...

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Abstract

The invention discloses a preparation method of an iron(III) fluoride positive material. The preparation method comprises the following steps of dissolving high-purity ferrous sulfate crystals in purewater to obtain a ferrous sulfate solution; adding urea, performing temperature rise, performing a stirring reaction, reducing the temperature to 5-15 DEG C, then at the temperature being 5-15 DEG C,performing stirring, adding a hydrogen peroxide solution and a hydrofluoric acid solution, performing a reaction, and performing washing with alcohol so as to obtain crystallization substances; adding the crystallization substances to a ferrous gluconate saturated solution, then under the condition of stirring, performing cooling and temperature reduction, performing filtration, performing washing with alcohol, and performing baking so as to obtain solid granules; and putting the obtained solid granules into a roller furnace, performing calcination, wherein the calcination is divided into three stages which sequentially include a temperature rise stage, a heat preservation stage and a temperature reduction stage, performing crushing by air currents on materials out of the furnace, and performing sieving so as to obtain the iron(III) fluoride positive material. Through the adoption of the preparation method disclosed by the invention, spheroidal agglomeration-free iron(III) fluoride positive material can be prepared; through coating, generation of large particles in the sintering course is avoided; and besides, the electric conductivity and the cycle performance of the positive material are improved.

Description

technical field [0001] The invention belongs to the technical field of new energy lithium battery materials, and in particular relates to a preparation method of an iron trifluoride positive electrode material. Background technique [0002] In the study of rock properties, laboratory tests usually need to extract rock sample cores to obtain various performance parameters. Most of the rock samples are drilled using the wet drilling method, but most of the drilled rock samples do not have fixing devices to fix them during the drilling process, and even need manual support to fix them, which consumes manpower and cannot guarantee the quality of the rock samples. There is no artificial damage to rock samples. Because artificial support cannot ensure that the force on the rock wall of the rock sample is uniform, this will increase the probability of the rock sample being sheared. [0003] In the existing technology, although there are also devices to fix the rock samples during...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/10
CPCC01G49/10C01P2004/03C01P2004/32C01P2004/61
Inventor 郑忆依
Owner 郑忆依