Process for preparing LixFeyPzO4 from ferrophosphorus

A technology of NH4H2PO4 and ferrophosphorus, which is applied in the field of material manufacturing process, can solve the problems of high preparation cost and single raw material, and achieve the effects of improving performance, eliminating pollutant discharge, and green, environmental protection and clean production.

Inactive Publication Date: 2011-04-20
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is in order to make up for existing preparation Li x Fe y P z o 4 The shortcomings of single raw material and high preparation cost solve the diversification of ferrophosphorus composition and the preparation of Li by ferrophosphorus x Fe y P z o 4 The problems that arise in the process, propose a method to prepare Li by ferrophosphorus x Fe y P z o 4 unique craftsmanship

Method used

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  • Process for preparing LixFeyPzO4 from ferrophosphorus
  • Process for preparing LixFeyPzO4 from ferrophosphorus
  • Process for preparing LixFeyPzO4 from ferrophosphorus

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Effect test

Embodiment 1

[0023] The by-product phosphorus iron Fe of thermal phosphoric acid was analyzed by rheological phase method. 1.5 P as raw material to prepare LiFePO 4 As the positive electrode material, first crush ferrophosphorus to a certain particle size, use ferrophosphorus powder as the iron source and part of the phosphorus source, and use NH 4 h 2 PO 4 To supplement the phosphorus source, LiOH·H 2 O and Li 2 CO3 As a combined lithium source, iron phosphorus Fe 1.5 P, NH 4 h 2 PO 4 , LiOH·H 2 O and Li 2 CO 3 The ratio of the amount of the substance is 2:1:1:1. After adding industrial ethanol to disperse into a rheological phase, put it in a muffle furnace at 300°C for pretreatment for 5 hours, and transfer it to a ceramic tube furnace at 700°C for roasting after cooling. 15h, using the raw material and oxygen in the air as the oxygen source, supplying oxygen in a diffuse manner, and obtaining black LiFePO after cooling 4 , whose crystal structure is attached figure 1 shown...

Embodiment 2

[0028] Fe 2.2 P as raw material to prepare LiFePO 4 As the positive electrode material, first crush ferrophosphorus to a certain particle size, use ferrophosphorus powder as the source of iron and phosphorus, and use NH 4 h 2 PO 4 To supplement the phosphorus source, LiOH·H 2 O and Li 2 CO 3 As a combined lithium source, iron phosphorus Fe 2.2 P, NH 4 h 2 PO 4 , LiOH·H 2 O and Li 2 CO 3 The ratio of the amount of the substance is 2:1:1:1, after adding industrial ethanol to disperse into a rheological phase, put it into a muffle furnace at 600°C for full oxidation treatment, after cooling, a certain amount of carbon is mixed into the precursor powder, and then transfer Put it into a quartz tube furnace at 750 ° C for 15 hours, use the raw material and oxygen in the air as the oxygen source, adopt the method of concentrated oxygen supply first, and then gradually reduce it, and obtain black LiFePO after cooling. 4 , the overall reaction equation is as follows:

[0...

Embodiment 3

[0034] The by-product phosphorus iron Fe of the yellow phosphorus production plant is recovered by reaction pulverization 2 P as raw material to prepare LiFePO 4 Cathode material, with phosphorus iron powder as phosphorus source and iron source, with Li 3 PO 4 As lithium source and supplementary phosphorus source, insufficient P is replaced by P 2 o 5 Supplement, the material ratio of the three is 6:4:1, a certain amount of oxygen is passed into the ball mill tank, after ball milling for 5 to 20 hours, it is put into a controlled atmosphere tube furnace at 700°C for 0.5 to 20 hours of roasting. 5 hours, control a certain air flow, use the raw material, oxygen and oxygen in the air as the oxygen source, and make black LiFePO 4 Electrode material, its morphology is as attached image 3 As shown, the reaction equation is as follows:

[0035] 12Fe 2 P+8Li 3 PO 4 +2P 2 o 5 +27O 2 →24LiFePO 4

[0036] No other by-products are produced during the reaction, and the morph...

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Abstract

The invention relates to a process for preparing LixFeyPzO4 from ferrophosphorus, especially for preparing LiFePO4, LiFe2 / 3PO4 and Li4 / 7Fe4 / 7P8 / 7O4. A phosphorus source or an iron source which needs supplementing is determined according to the ferrophosphorus and the composition of the LixFeyPzO4 to be prepared. The phosphorus source or the iron source is supplemented according to a mol ratio of 1.0:(0.2-5.0):(0.2-1.5) among total phosphorus elements, total iron elements and total lithium elements. A lithium-containing substance is added and then evenly mixed with the ferrophosphorus. The mixture is then roasted for 0.2-35 hours at the temperature of 400-900 DEG C so as to obtain the LixFeyPzO4. By means of reaction design, raw material combination and byproduct reaction, the process can be a clean production process realizing zero emission. The process adopts the ferrophosphorus as the raw material for preparing the LixFeyPzO4 and has wide raw material source, low cost, high resourceutilization rate and little pollution. The reaction process has relatively low demand on apparatuses. The preparation process is simple, realizes easy oxygen amount control in the reaction process, short production flow, low investment and good benefit, has good application value and is suitable for large-scale, industrial and low-cost preparation of LixFeyPzO4.

Description

technical field [0001] The invention belongs to the technical field of material manufacturing technology, in particular to a method for preparing Li x Fe y P z o 4 The process can be applied to the development of new high-performance electrode materials. Background technique [0002] Li x Fe y P z o 4 It is a new type of green energy electrode material with great potential, mainly including LiFePO 4 , LiFe 2 / 3 PO 4 and Li 4 / 7 Fe 4 / 7 P 8 / 7 o 4 And its compound, have very big market space. Among these electrode materials, LiFePO 4 It is a research hotspot at present, and people reduce cost and improve performance through various ways one after another. However, due to the bottleneck of the process route and raw materials, the commercial LiFePO on the market 4 The output is not very large, there are still high prices, high raw material costs (mostly using H 2 Reducing atmosphere), unstable product performance, low electronic conductivity (about 10 -9 ~10 -10...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/12Y02E60/10
Inventor 王贵欣闫康平刘睿陈妙
Owner SICHUAN UNIV
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