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A preparation method and production device of battery-grade iron phosphate

An iron phosphate and battery-level technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of inability to obtain stable products, blockage of undissolved solids, high local concentration, etc., to eliminate quality differences and artificial interference factors, reduced back-mixing, and short reaction times

Active Publication Date: 2021-07-16
山东彩客新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is easy to cause blockage of undissolved solids in pipeline 1, resulting in unstable feeding, excessive local concentration, and failure to obtain products with stable properties.

Method used

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  • A preparation method and production device of battery-grade iron phosphate
  • A preparation method and production device of battery-grade iron phosphate
  • A preparation method and production device of battery-grade iron phosphate

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preparation example Construction

[0028] The preparation method of ferric phosphate of the present invention, comprises the steps:

[0029] Step a, preparation of iron salt solution: iron source is dissolved in pure water of 15 ℃-40 ℃ to make iron salt solution, the mass percentage concentration of ferrous ion in the solution is 5%-8% (wt), the solution after dissolving The pH value is 2.0-4.0. The iron source is one of ferrous sulfate, ferrous chloride, ferrous nitrate or ferrous oxalate.

[0030] Iron powder can also be placed in sulfuric acid, hydrochloric acid, nitric acid or oxalic acid solution to react to obtain iron salt solution.

[0031] Step b. Prepare phosphorus source solution: add phosphorus source into pure water at a temperature of 20°C-35°C, dissolve and add oxidant and surfactant, and stir evenly to prepare phosphorus source solution. The pH of the solution was 7-8.5.

[0032] The phosphorus source is one of sodium phosphate, potassium phosphate, disodium hydrogen phosphate, sodium dihydro...

Embodiment 1

[0042] In the phosphate storage tank of 1000L, add 235.0kg disodium hydrogen phosphate solid and 700.0kg pure water, after dissolving, add 70.8kg hydrogen peroxide (the concentration of hydrogen peroxide is 30%) and 2.0kg triethanolamine oleic acid soap, stir well and set aside , make phosphorus source solution, the concentration of phosphate ion in the solution is 15.60%. In another 2000L ferric salt storage tank, prepare 1200kg concentration of 14.0% ferrous chloride solution for subsequent use to make ferric salt solution, the concentration of iron ions in the solution is 6.17%.

[0043] Add 10kg of pure water to a 100L reactor, and use two metering pumps to add the filtered phosphorus source solution and iron salt solution to the reactor at the same time. The temperature of the feed liquid in the reactor is 57°C, and the phosphorus source solution The addition amount of the ferrous solution is 0.616kg / min, the addition amount of the ferrous solution is 0.984kg / min, and the...

Embodiment 2

[0046] Take a 1000L phosphate storage tank, add 256.0kg of disodium hydrogen phosphate solid, 700.0kg of pure water, 70.8kg of hydrogen peroxide (concentration is 30%) and 2.5kg of PEG-400, stir well and set aside to make phosphorus source solution , the concentration of phosphate ions in the solution is 16.64%. In another 2000L ferric salt storage tank, prepare 1200kg concentration of 14.0% ferrous chloride solution as ferric salt solution.

[0047] Add 40kg of pure water to a 250L reactor in advance, and then use two metering pumps to add the filtered phosphorus source and iron salt solution to the reactor at the same time. The pump is 0.616kg / min, the ferrous metering pump is 0.923kg / min, and the stirring speed is 300rpm. After the material in the kettle stays for 40 minutes, start to continuously extract the material, so that the output speed and the feeding speed are kept consistent. Collect the reaction liquid for 1 hour, press filter and wash, and obtain the iron phos...

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Abstract

A method for preparing battery-grade iron phosphate, comprising the following steps: preparing an iron salt solution, preparing a phosphorus source solution, and performing an oxidation precipitation reaction; the reacted feed liquid is filtered through a plate and frame; the filter cake is washed and sintered to finally obtain an iron phosphate product . The production device includes an iron salt storage tank, a phosphate storage tank, a reaction kettle, a retention kettle and a plate frame, and the iron salt storage tank and the phosphate storage tank are respectively connected to the top of the reaction kettle through a feeding pipeline. Connected to the board and frame in turn. The above preparation process adopts a continuous feeding and discharging production device, so that the oxidation precipitation reaction is in a state of dynamic equilibrium, the reaction time is short, the quality of the produced iron phosphate is stable, and the particle size is controllable, realizing the continuous industrial production of iron phosphate.

Description

technical field [0001] The invention relates to the technical field of iron phosphate preparation technology, in particular to a production technology of iron phosphate suitable for manufacturing batteries. Background technique [0002] Iron phosphate (FePO 4 ·nH 2 O, n=0-2), also known as ferric orthophosphate or ferric phosphate, with the decrease of crystal water, the color gradually turns yellow, and anhydrous ferric phosphate is yellow-white powder. It is mainly used in the manufacture of lithium iron phosphate, and can also be used as a catalyst and in the manufacture of ceramics. The product performance of iron phosphate is very important for the preparation of lithium iron phosphate for the positive electrode of the battery. Its main performance indicators are particle size and distribution, iron-phosphorus ratio, specific surface area, tap density, etc. At present, there are many manufacturers producing battery-grade iron phosphate at home and abroad. Due to the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/61C01P2006/40
Inventor 晋平柯君雄王镖王猛李亚鹏王红强崔凤桐张吉晔段卫东
Owner 山东彩客新材料有限公司
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