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Preparation method of lithium iron phosphate precursor

A technology of lithium iron phosphate and precursors, which is applied in the field of preparation of lithium iron phosphate precursors to achieve the effects of low production cost, good stability and regular shape

Inactive Publication Date: 2017-07-04
沧州凯盛达新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the deficiency of existing lithium iron phosphate precursor preparation method, propose a kind of production process simple, reaction condition mildness, the preparation method of the lithium iron phosphate precursor (iron phosphate) that is easy to large-scale production

Method used

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Effect test

Embodiment 1

[0025] The preparation method of the lithium iron phosphate precursor of this embodiment is prepared according to the following steps:

[0026] (1) Roasting the ferric oxalate by temperature programming, first pre-calcining at a low temperature of 350°C for 8 hours, and then roasting at a high temperature of 650°C with a programmed temperature rise, to remove free water and crystal water in the ore, and obtain anhydrous ferric oxalate;

[0027] (2) cross 100 mesh sieves after the anhydrous ferric oxalate is pulverized, wash 3 times with supercritical water according to the quality of anhydrous ferric oxalate after sieving, filter, and make ferric oxalate powder;

[0028] (3) iron oxalate powder is put into reactor, feeds oxygen, fully reacts, makes purified iron oxalate;

[0029] (4) Sodium phosphate is added to phosphoric acid acidification with a concentration of 25%, and the pH is adjusted to 4 to obtain a sodium phosphate solution;

[0030] (5) Add the purified ferric oxa...

Embodiment 2

[0034] The preparation method of the lithium iron phosphate precursor of this embodiment is prepared according to the following steps:

[0035] (1) Roasting the ferric oxalate by temperature programming, first pre-calcining at a low temperature of 350°C for 8 hours, and then calcining at a high temperature of 850°C with a programmed temperature increase, to remove free water and crystal water in the ore, and prepare anhydrous ferric oxalate;

[0036] (2) cross 200 mesh sieves after the anhydrous ferric oxalate is pulverized, wash 3 times with supercritical water according to the quality of anhydrous ferric oxalate after sieving, filter, and make ferric oxalate powder;

[0037] (3) iron oxalate powder is put into reactor, feeds oxygen, fully reacts, makes purified iron oxalate;

[0038] (4) Sodium phosphate is acidified by adding phosphoric acid with a concentration of 35%, and the pH is adjusted to 6.5 to obtain a sodium phosphate solution;

[0039] (5) Add the purified ferri...

Embodiment 3

[0043] The preparation method of the lithium iron phosphate precursor of this embodiment is prepared according to the following steps:

[0044] (1) Roasting the ferric oxalate by temperature programming, first pre-calcining at a low temperature of 350°C for 8 hours, and then roasting at a high temperature at a temperature of 750°C to remove free water and crystal water in the ore to obtain anhydrous ferric oxalate;

[0045] (2) cross 150 mesh sieves after the anhydrous ferric oxalate is pulverized, wash 3 times with supercritical water according to the quality of anhydrous ferric oxalate after sieving, filter, and make ferric oxalate powder;

[0046] (3) iron oxalate powder is put into reactor, feeds oxygen, fully reacts, makes purified iron oxalate;

[0047] (4) Sodium phosphate is acidified by adding phosphoric acid with a concentration of 30%, and the pH is adjusted to 5.5 to obtain a sodium phosphate solution;

[0048] (5) Add the purified ferric oxalate and sodium phosph...

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Abstract

The invention relates to a preparation method of a lithium iron phosphate precursor. The method includes the steps of: subjecting ferric oxalate to temperature-programmed calcination to obtain anhydrous ferric oxalate; crushing the anhydrous ferric oxalate and performing sieving, then according to the mass of the sieved anhydrous ferric oxalate, using supercritical water to perform washing 3 times so as to obtain ferric oxalate powder; putting the ferric oxalate powder into a reactor, introducing oxygen, and carrying out full reaction for 5min so as to obtain purified ferric oxalate; adding sodium phosphate into phosphoric acid for acidification, and adjusting the pH so as to obtain a sodium phosphate solution; transferring the purified ferric oxalate and the sodium phosphate solution into a hydrothermal high temperature and high pressure kettle, then adding iron phosphate seed crystal to carry out reaction for 14h, thus obtaining iron phosphate crystals; adding a dispersant into the iron phosphate crystals, and fully mixing the substances, thus obtaining a lithium iron phosphate precursor. The preparation method of the lithium iron phosphate precursor provided by the invention has the characteristics of simple production process and mild reaction conditions, and the precursor product has high purity, regular shape and good consistency, thus being capable of realizing industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium battery materials, and relates to a lithium iron phosphate precursor, in particular to a preparation method of the lithium iron phosphate precursor. Background technique [0002] With the continuous development of the global economy, existing resources can no longer meet people's growing needs. Energy storage battery technology is of great significance to the comprehensive utilization of various clean energy sources and the adjustment of energy consumption structure, and the study of the performance of power battery cathode materials is the key . Currently available commercial secondary batteries mainly include lead-acid batteries, nickel-chromium batteries, nickel-metal hydride batteries and lithium-ion batteries. Compared with traditional lead-acid batteries, nickel-cadmium batteries and nickel-hydrogen batteries, lithium-ion secondary batteries have working With many advantages such as high vo...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B25/45
CPCC01B25/375C01B25/45C01P2006/11C01P2006/80Y02P20/54
Inventor 王金锋张万红
Owner 沧州凯盛达新能源科技有限公司
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