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Preparation method and application of iron phosphate

A technology of iron phosphate and lithium iron phosphate, which is applied in the preparation/purification of carbon, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of affecting the performance of lithium iron phosphate, high cost of ferric salt, and high cost of environmental protection treatment, To achieve the effect of being beneficial to washing, high utilization rate and low cost

Pending Publication Date: 2022-06-21
上海鑫忆丹新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the cost of ferric salt is too high to meet the current low-cost iron phosphate market requirements, this route has been gradually abandoned by manufacturers; the second method is to use ferrous sulfate (ferrous sulfate can be dissolved by sulfuric acid) One or more of diammonium hydrogen phosphate, ammonium dihydrogen phosphate, phosphoric acid or sodium dihydrogen phosphate is used as a phosphorus source, and ferric phosphate is prepared by adding hydrogen peroxide to oxidize, which is currently the mainstream of iron phosphate manufacturers However, the process inevitably has by-product ammonium salt (ammonium sulfate), and a large amount of sulfate radicals are easily adsorbed on the surface of iron phosphate, which is not easy to wash. In order to reduce the sulfur content in iron phosphate, a large amount of water is often used in the washing process. , the cost of environmental protection treatment is high, and the existence of too high sulfur will affect the performance of lithium iron phosphate to a certain extent, and at the same time, sulfur dioxide gas is released during the preparation of lithium iron phosphate, causing environmental pollution

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  • Preparation method and application of iron phosphate
  • Preparation method and application of iron phosphate
  • Preparation method and application of iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Preparation of iron phosphate

[0056] Slowly add 554g of 85% phosphoric acid into a 2L beaker filled with 1014g of deionized water, stir with a glass rod to obtain a 30% phosphoric acid solution, and then slowly add the weighed 111.8g of iron flakes to a solution containing 30 % phosphoric acid solution (in order to avoid the evaporation of water in the beaker during the long-term heating process, cover the beaker with a watch glass in advance), and then put the beaker into a water bath for heating, and the heating temperature is 55 degrees , and kept at this temperature for 16 hours, after 16 hours, the iron sheet was completely dissolved, and filtered, and the bright green Fe(H) was obtained after filtration. 2 PO 4 ) 2 The solution and 3.354 g of tetrabutyl titanate accounting for 3% of the mass of the iron source were transferred into a 5L glass reaction kettle. After the addition was completed, the reaction kettle was stirred at a rotating speed of 300 r / min...

Embodiment 2

[0062] (1) Preparation of iron phosphate

[0063] Slowly add 530.4g of 85% phosphoric acid into a 2L beaker containing 879g of deionized water, stir with a glass rod to obtain a 32% phosphoric acid solution, and then slowly add the weighed 111.8g of iron powder to the solution containing 2L of 32% phosphoric acid solution (in order to avoid the evaporation of water in the beaker during long-term heating, cover the beaker with a watch glass in advance), and then put the beaker into a water bath for heating, and the heating temperature is 50 10 hours at a constant temperature at this temperature, after 10 hours the iron powder is completely dissolved, filter, and filter to obtain bright green Fe(H 2 PO 4 ) 2 The solution was transferred to a 5L glass reaction kettle. After the addition was completed, the reaction kettle was turned on and stirred at a speed of 300 r / min. At the same time, the glass reaction kettle was heated at a heating temperature of 80 degrees. When the solu...

Embodiment 3

[0068] (1) Preparation of iron phosphate

[0069] Slowly add 530.4g of 85% phosphoric acid into a 2L beaker filled with 1203g of deionized water, stir with a glass rod to obtain a 26% phosphoric acid solution, and then slowly add the weighed 111.8g iron flakes to the beaker containing In 2L of 26% phosphoric acid solution (in order to avoid the evaporation of water in the beaker during long-term heating, cover the beaker with a watch glass in advance), and then put the beaker into a water bath for heating, and the heating temperature is 55 16 hours at a constant temperature at this temperature, after 16 hours the iron flakes are completely dissolved, filter, and filter to obtain bright green Fe(H 2 PO 4 ) 2 The solution and 2.236g magnesium hydroxide (accounting for 2% of the iron source mass) were transferred into the 5L glass reaction kettle. After adding, the reaction kettle was stirred at a rotating speed of 300r / min, and the glass reaction kettle was heated at a heating...

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Abstract

The invention belongs to the technical field of lithium ion battery positive electrode materials, and particularly provides a preparation method of iron phosphate which is low in cost, low in specific surface area (less than 3m < 2 > / g), low in impurity content, high in performance and suitable for industrial production and application of the iron phosphate. According to the method, the iron source and the phosphoric acid react under certain conditions such as low temperature, then the filtrate after the reaction and the hydrogen peroxide are subjected to oxidation reaction, the iron phosphate is directly prepared, and the prepared iron phosphate can be used as a precursor and can be used for preparing the lithium iron phosphate / carbon composite material with excellent performance. In the whole process, the acid-base adjusting process and the surfactant using process of a traditional iron phosphate production process are avoided. The iron phosphate prepared by the method has the advantages of special morphology, few types of byproducts (only phosphoric acid is left), small specific surface area, facilitation of washing, reduction of the use amount of washing water, facilitation of improvement of the recycling rate of mother liquor, avoiding of the introduction of sulfate ions and some cations, and further reduction of the pollution to the environment.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials for lithium ion batteries, and in particular relates to a preparation method of an iron phosphate intermediate with low cost, high performance, low surface area and quasi-polyhedral shape. Background technique [0002] With the gradual increase in the requirements of battery energy density, ternary cathode materials have attracted more and more attention. However, their high price and low thermal stability make the market slowly turn to low price, stable structure, safe performance and cycle. Lithium iron phosphate cathode material with good performance. [0003] Among various methods for preparing lithium iron phosphate, the production process using iron phosphate as a precursor has the advantages of simple production process and low production cost compared with the ferrous oxalate and iron red processes. With high capacity, high purity and high compaction, it has become th...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B25/45C01B32/05H01M4/58H01M10/0525
CPCC01B25/375C01B25/45C01B32/05H01M4/5825H01M10/0525C01P2004/80C01P2006/12C01P2006/40C01P2004/03C01P2002/72Y02E60/10
Inventor 程冲
Owner 上海鑫忆丹新材料有限公司
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