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Ferromanganese phosphate intermediate, lithium ferromanganese phosphate, and method for producing same

A technology of lithium manganese iron phosphate and intermediates, applied in lithium manganese iron phosphate, lithium manganese iron phosphate in the field of lithium batteries, can solve the problem of reducing the volume energy ratio of materials, low compaction density of lithium manganese iron phosphate, and difficulty in obtaining synthetic methods Theoretical measurement ratio and other issues

Pending Publication Date: 2020-06-12
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However: in the preparation process of ferromanganese phosphate precursor, due to the unstable and strong oxidizing properties of Mn(III), it is difficult to obtain the theoretical stoichiometric ratio of Mn 1-x Fe x PO 4 materials, or harsh synthesis conditions are required; and ferromanganese oxalate has a large gas production capacity, resulting in a low compaction density of the obtained lithium manganese iron phosphate, which reduces the volume energy ratio of the material

Method used

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  • Ferromanganese phosphate intermediate, lithium ferromanganese phosphate, and method for producing same
  • Ferromanganese phosphate intermediate, lithium ferromanganese phosphate, and method for producing same
  • Ferromanganese phosphate intermediate, lithium ferromanganese phosphate, and method for producing same

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Effect test

Embodiment 1

[0109] According to the molar ratio of Mn:Fe=50:50, the content of manganese sulfate and ferrous sulfate is 10g / L (with MnSO 4 ·H 2 O and FeSO 4 ·7H 2 O (meter) of the aqueous solution, a total of 5500 mL, the equivalent metal molar weight is 0.246 mol, denoted as liquid A-1.

[0110] Using 30g 85% industrial phosphoric acid as the phosphorus source (0.26mol), using the sulfuric acid with a concentration of 1M as the pH control reagent, and about 33.2g 26%wt ammonia water as the nitrogen source (0.247mol), under stirring, liquid A-1 , industrial phosphoric acid and ammonia water are simultaneously added into the reaction kettle whose temperature is room temperature ± 5 ℃, and the pH is controlled to be 3.0 ± 0.2 by regulating the adding speed of sulfuric acid. After the addition of materials, the reaction was completed by stirring at a constant temperature for 24 hours.

[0111] The precipitate obtained above was filtered, washed with deionized water, and then dried in an ...

Embodiment 2

[0116] According to the molar ratio of Mn:Fe=80:20, an aqueous solution of manganese chloride (tetrahydrate) and ferrous chloride (tetrahydrate) with a content of 200g / L was prepared, a total of 3000mL, and the equivalent metal molar weight was 3.03mol, denoted as Liquid Armor-2.

[0117] Take 350g 85% phosphoric acid (3.03mol) as the phosphorus source, take the 2kg ammonium sulfate (3.03mol) aqueous solution with a concentration of 20%wt as the nitrogen source, and take the sodium hydroxide with a concentration of 10M as the pH control reagent, under stirring, the Liquid A-2, phosphoric acid and ammonium sulfate solution were simultaneously added to the reaction kettle with a temperature range of 70±5°C, and the pH was controlled to be 5.5±0.2 by regulating the addition rate of sodium hydroxide. After the addition was completed, the temperature was kept constant for 12 hours to complete the reaction.

[0118] The precipitate obtained above was filtered, washed with deionized...

Embodiment 3

[0123] According to the molar ratio of Mn:Fe=7:1, an aqueous solution with a content of manganese chloride (tetrahydrate) and ferrous chloride (tetrahydrate) of 200g / L was prepared, a total of 3000mL, and the equivalent metal molar amount was 3.03mol, which was recorded as Liquid Armor-3.

[0124] With 350g 85% phosphoric acid (3.03mol) as phosphorus source, with concentration of 1.2kg ammonium bicarbonate (3.03mol) aqueous solution of 20%wt as nitrogen source, with concentration of 1M sodium hydroxide as pH control reagent, under stirring , the liquid methyl-2, phosphoric acid, and ammonium bicarbonate solution were simultaneously added to the reaction kettle with a temperature range of 70±5°C, and the pH was controlled to be 5.5±0.2 by regulating the adding speed of sodium hydroxide. After the addition was completed, the temperature was kept constant for 12 hours to complete the reaction.

[0125] The precipitate obtained above was filtered, washed with deionized water, and...

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Abstract

Ferromanganese phosphate intermediates, lithium ferromanganese phosphate, and methods of making the same are disclosed. The intermediate has a chemical formula of (NH4)Mn(1-x-y)FexMyPO4.H2O, wherein the x is equal to 0.05 to 0.5 and y is equal to 0 to 0.2; the M is a divalent metal and is selected from one or more of Mg, Ca, Co, Mn and Zn. The intermediate has a crystal structure with an orthogonal structure, belongs to a Pmnm (59) space group, and has a two-dimensional nanosheet structure in product morphology.

Description

technical field [0001] The present invention relates to an intermediate of iron manganese phosphate, and the lithium iron manganese phosphate formed by using the intermediate has improved electrochemical activity and high compaction density. The present invention also relates to the lithium iron manganese phosphate formed with the intermediate, the production method of the intermediate and the lithium iron manganese phosphate, and the use of the lithium iron manganese phosphate in a lithium battery. [0002] technical background [0003] Lithium-ion batteries for vehicles require high energy density, high power, high safety and long life, which is one of the development trends of lithium batteries in the future. Among many cathode materials, the olivine-type transition metal phosphate system represented by lithium iron phosphate has good power, safety and cycle life, and is widely used in electric buses, electric logistics vehicles, start-stop In the field of automotive batt...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58H01M10/052B82Y40/00
CPCC01B25/451H01M4/5825H01M10/052B82Y40/00C01P2002/72C01P2004/03C01P2002/85C01P2006/40C01P2004/22Y02E60/10
Inventor 杭道金陆君肖天辉朱灵霖
Owner SHANGHAI HUAYI GRP CO
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