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Method for preparing ferric orthophosphate

A technology of iron orthophosphate and ferrophosphorus is applied in the field of preparation of primary particle nanosized iron orthophosphate, which can solve the problems affecting the low-temperature discharge performance of lithium iron phosphate, difficult to control the size of primary particles, and coarse lithium iron phosphate. Avoiding explosive precipitation, stable precipitation speed, and improved electrical properties

Inactive Publication Date: 2017-01-04
ZHEJIANG RICHPOWER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

The ferric orthophosphate prepared by this method is difficult to control the size of the primary particle in the reaction process, and the primary particle of the synthesized ferric orthophosphate is relatively coarse
The primary particles of lithium iron phosphate prepared by using iron orthophosphate prepared in this way as a raw material will also be relatively coarse, which will affect the low-temperature discharge performance of the prepared lithium iron phosphate

Method used

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  • Method for preparing ferric orthophosphate

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Effect test

Embodiment 1

[0024] The invention provides a kind of preparation method of ferric orthophosphate, and concrete steps are:

[0025] Configure ferric nitrate into a 2mol / L solution; add phosphoric acid to the ferric nitrate capacity according to the molar ratio of Fe:P=1:1.05 to prepare a phosphorus-iron mixed solution; configure sodium hydroxide into a 4mol / L solution;

[0026] After configuring the solution, prepare ferric orthophosphate as follows:

[0027] Step 1: Add 150L (15% of the volume of the whole kettle) of deionized water in a 1000L stirred reactor;

[0028] Step 2: After adding deionized water, adjust the temperature of the stirred reactor to 75°C, and then start to drop the ferrophosphorus mixed solution and sodium hydroxide solution;

[0029] Step 3: dropwise adding the ferrophosphorus mixed solution at a rate of 3L / min; dropwise adding the sodium hydroxide solution by controlling the pH=3 in the reactor, and forming ferric orthophosphate precipitation in the reactor;

[00...

Embodiment 2

[0036] The invention provides a kind of preparation method of ferric orthophosphate, and concrete steps are:

[0037] Prepare ferric nitrate into a 5mol / L solution; add phosphoric acid to the ferric nitrate capacity according to the molar ratio of Fe:P=1:1.05 to prepare a mixed ferrophosphorus solution; prepare sodium hydroxide into a 10mol / L solution;

[0038] After configuring the solution, prepare ferric orthophosphate as follows:

[0039] Step 1: Add 200L of deionized water to the 1000L stirred reactor;

[0040] Step 2: After adding deionized water, adjust the temperature of the stirred reactor to 80°C, and then start to drop the ferrophosphorus mixed solution and sodium hydroxide solution;

[0041] Step 3: dropwise adding the ferrophosphorus mixed solution at a rate of 1L / min, and dropwise adding the sodium hydroxide solution by controlling the pH in the reactor to 3.5, forming ferric orthophosphate precipitation in the reactor;

[0042] Step 4: After dropping the ferro...

Embodiment 3

[0047] The invention provides a kind of preparation method of ferric orthophosphate, and concrete steps are:

[0048] Prepare ferric nitrate into a 3mol / L solution; add phosphoric acid to the ferric nitrate capacity according to the ratio of Fe:P=1:1.05 to prepare an iron-phosphorus mixed solution; prepare sodium hydroxide into a 5mol / L solution;

[0049] After configuring the solution, prepare ferric orthophosphate as follows:

[0050] Step 1: Add 180L of deionized water to the 1000L stirred reactor;

[0051] Step 2: After adding deionized water, adjust the temperature of the stirred reactor to 70°C, and then start to drop the ferrophosphorus mixed solution and sodium hydroxide solution;

[0052]Step 3: dropwise adding the ferrophosphorus mixed solution at a rate of 5 L / min. Carry out dropwise addition of sodium hydroxide solution by controlling the pH=3 in the reactor to form ferric orthophosphate precipitation in the reactor;

[0053] Step 4: After starting to drop the f...

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Abstract

The invention discloses a method for preparing ferric orthophosphate, and belongs to the technical field of chemical preparing. The method for preparing the ferric orthophosphate includes the steps that ferric nitrate serves as an iron source, phosphoric acid serves as a phosphorus source, sodium hydroxide serves as a pH adjusting agent, parameters such as the temperature and the pH are controlled in a reaction kettle with stirring, and the ferric orthophosphate is synthesized. In the ferric orthophosphate synthetic process, slurry in the reaction kettle is circularly grinded through a sand milling machine, and primary particles of the synthesized ferric orthophosphate are effectively controlled. As a lithium iron phosphate material is synthesized with the prepared ferric orthophosphate as an iron source, the electrical performance is obviously improved; under the 1C condition, the discharge specific capacity reaches 155 mAh / h, and reaches 85% or above of the normal-temperature discharging capacity while discharging at the temperature of -20 DEG C; meanwhile, as bulk chemicals are uses as raw materials, the cost is low, and the preparing process is simple.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, relates to a method for preparing ferric orthophosphate, in particular to a method for preparing primary particle nanometerized ferric orthophosphate. Background technique [0002] Lithium iron phosphate, as a positive electrode active material for lithium-ion batteries, has a large number of applications in the fields of power batteries and energy storage batteries because of its cheap price, environmental friendliness, high safety, and good cycle performance. At present, the synthesis route of lithium iron phosphate can be divided into three types: ferrous oxalate route, ferric oxide route and orthophosphoric acid route according to the iron source. For these three routes, the lithium iron phosphate prepared by the iron orthophosphate route has the highest discharge capacity. The performance of lithium iron phosphate prepared by using the iron orthophosphate line mainly depends on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525C01B25/37
CPCC01B25/375H01M4/5825H01M10/0525Y02E60/10
Inventor 于文志陈家骅许丁丁郑金龙胡大伟
Owner ZHEJIANG RICHPOWER TECH
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