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Preparation method and application of iron phosphate

A technology of ferric phosphate and ammonium ferric phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of increasing production cost, increasing production cost, consumption price, etc. The effect of high solid density

Active Publication Date: 2021-04-09
GUANGDONG BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is recorded in the prior art that ferrous salt is used as an iron source, and hydrogen peroxide is added as an oxidizing agent to oxidize ferrous iron to ferric iron to finally produce ferric phosphate. This method needs to consume more expensive hydrogen peroxide as an oxidizing agent, increasing cost of production
The prior art also discloses a method for preparing high-density basic ammonium ferric phosphate. Due to the presence of divalent iron in the raw material, it is necessary to consume a large amount of hydrogen peroxide as an oxidant to oxidize divalent iron to ferric iron, thereby improving The production cost is reduced; and although the tap density of basic ammonium ferric ammonium phosphate produced by it is high, reaching 1.3-1.6g / cm3, its particle size D50 is relatively large, which is easy to cause crushing difficulties. Therefore, there are certain disadvantages to the preparation of high-performance lithium iron phosphate
[0004] At present, there is still a lack of reports on the preparation of battery-grade iron phosphate by using ferric iron source to prepare small-sized and controllable basic ferric ammonium phosphate

Method used

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  • Preparation method and application of iron phosphate

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Experimental program
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Embodiment 1

[0053] The preparation method of the iron phosphate of the present embodiment specifically comprises the following steps:

[0054] (1) the waste iron phosphate dihydrate of 50kg is roasted at 350 DEG C for 3h to remove crystal water, the material after roasting is about 40kg, and the material is dropped into the sulfuric acid solution kettle storing 270L, 1.5mol / L and stirred at 200rpm rotating speed, Heated to 50°C to dissolve for about 5 hours, and then left to stand. The filter residue was filtered out by a precision filter and then transferred to a storage tank to obtain Fe-containing 3+ and PO4 3- solution, the iron and phosphorus content in the detection solution were 43.28g / L and 24.78g / L respectively, and the molar ratio of Fe:P=1:1.03;

[0055] (2) 50L deionized water is the bottom liquid, which will contain Fe 3+ and PO4 3- The solution and ammonia water are injected into the reaction kettle in parallel from the bottom of the reactor at a 6:1 liquid feed rate, adj...

Embodiment 2

[0063] The preparation method of the iron phosphate of the present embodiment specifically comprises the following steps:

[0064] (1) the ferric phosphate waste material of 10kg is roasted at 400 DEG C for 5h to remove crystal water, the material after roasting is about 8kg, and at 200rpm rotating speed, the material is put into the sulfuric acid solution still storing 34L, 2.4mol / L and stirred, heated to After dissolving at 50 °C for about 5 hours, let it stand, filter out the filter residue with a precision filter, and transfer it to a storage tank to obtain Fe-containing 3+ and PO4 3- The iron and phosphorus content in the detection solution were 83.20g / L and 47.9g / L respectively, and the Fe:P molar ratio=1:1.04;

[0065] (2) 50L deionized water is the bottom liquid, which will contain Fe 3+ and PO4 3- The solution and ammonia water are injected into the reactor by the bottom of the reactor at a rate of 3:1, and the fine-tuning feeding speed of the lye is adjusted by th...

Embodiment 3

[0073] The preparation method of the battery-grade iron phosphate of the present embodiment specifically includes the following steps:

[0074] (1) the ferric phosphate waste material of 4kg is roasted at 300 DEG C for 3h to remove crystal water, the material after roasting is about 4kg, and the material is dropped into the sulfuric acid solution kettle that stores 27L, 1.5mol / L under 200rpm rotating speed and stirred, heated to After dissolving at 50 °C for about 5 hours, let it stand, filter out the filter residue with a precision filter, and transfer it to a storage tank to obtain Fe-containing 3+ and PO4 3- The iron and phosphorus content in the detection solution were 63.42g / L and 37.17g / L respectively, and the Fe:P molar ratio=1:1.05;

[0075] (2) 20L deionized water is used as the bottom liquid, which will contain Fe 3+ and PO4 3- The solution and ammonia water are injected into the reactor by the bottom of the reactor at a rate of 8:1, and the fine-tuning feeding sp...

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Abstract

The invention belongs to the field of battery materials, and discloses a preparation method and application of iron phosphate. The preparation method comprises the following steps: roasting iron phosphate waste, adding into an acid solution, dissolving, filtering, and taking the filtrate to obtain a solution A containing iron and phosphorus elements; stirring the solution A and alkali liquor, adjusting the pH value to be acidic, reacting, washing, filtering, and taking filter residues to obtain an amorphous iron phosphate yellow filter cake; aging, pulping and heating the iron phosphate yellow filter cake, adding phosphoric acid and alkali liquor, washing, filtering, taking filter residues to obtain a basic ammonium iron phosphate filter cake, and drying to obtain basic ammonium iron phosphate crystal powder; and roasting, dehydrating and cooling the basic ammonium ferric phosphate crystal powder to obtain the iron phosphate. According to the invention, recycled ferrophosphorus waste is used as a raw material, amorphous iron phosphate is precipitated by adopting alkali liquor, and ammonia water and phosphoric acid are used as an aging agent under a high-temperature stirring condition, so that the purpose of controllable crystallization of basic ammonium ferric phosphate is achieved.

Description

technical field [0001] The invention belongs to the field of battery materials, and in particular relates to a preparation method and application of iron phosphate. Background technique [0002] With the country's strong support in the field of new energy vehicles and the enhancement of public awareness of environmental protection, lithium-ion batteries have gradually become widely used power storage devices. Lithium iron phosphate batteries have gradually become the first choice in the field of rechargeable batteries for new energy vehicles due to their good safety performance, long cycle life and low price, and because they do not contain precious metals and rare elements, the raw material reserves are abundant and will not cause environmental damage. Too much pollution, lithium iron phosphate batteries gradually glow with new vitality, and many new energy battery companies currently use them as mainstream energy storage batteries. [0003] Iron phosphate is an important ...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58C01B25/45
CPCC01B25/375H01M4/5825C01B25/45C01P2004/61C01P2006/11C01P2006/12C01P2002/72C01P2004/03C01P2006/80Y02E60/10C01B25/451H01M2004/028H01M2004/021C01P2006/40
Inventor 秦存鹏韦吉刘更好阮丁山李长东
Owner GUANGDONG BRUNP RECYCLING TECH
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