Preparation method of manganese phosphate

A technology of manganese phosphate and concentrated phosphoric acid, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as complex reaction system, long reaction time, and introduction of sulfate radicals, and achieve simple process, low cost, and simple reaction Effect

Active Publication Date: 2020-12-29
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction system is complex, the reaction time is long (more than 24h), and sulfate radicals will be introduced, which requires a large amount of water to clean

Method used

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  • Preparation method of manganese phosphate
  • Preparation method of manganese phosphate
  • Preparation method of manganese phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 4g of potassium permanganate, measure 20mL of phosphoric acid with a mass fraction of 85wt%, add it into a 50mL reaction kettle and stir evenly. After the reaction kettle is sealed, put it in an oven and react at 180°C for 12 hours. After cooling, filter, wash and dry the slurry to obtain gray-green manganese phosphate MnPO 4 ·H 2 O powder, manganese phosphate yield is ~ 99%. Carry out XRD detection to the manganese phosphate prepared, its result is as follows figure 1 shown. From figure 1 It can be seen that the manganese phosphate obtained in this example is pure phase manganese phosphate monohydrate.

[0020] Carry out SEM detection to the manganese phosphate prepared by the present embodiment, the result is as follows figure 2 shown. Depend on figure 2 It can be seen that the particle size distribution of the manganese phosphate prepared in this example is uniform, and its secondary particles are dumbbell-shaped.

Embodiment 2

[0022] Weigh 3g of potassium permanganate, measure 20mL of phosphoric acid with a mass fraction of 85wt%, add it into a 100mL four-neck flask and stir evenly. Heat the oil bath to 150°C and react for 6 hours. After cooling, filter, wash and dry the slurry to obtain gray-green manganese phosphate MnPO 4 ·H 2 O powder, manganese phosphate yield is ~ 99%.

Embodiment 3

[0030] Weigh 4g of potassium permanganate, measure 40mL of phosphoric acid with a mass fraction of 85wt%, add to a 50mL reaction kettle and stir evenly. After the reaction kettle is sealed, put it into an oven and react at 140°C for 14 hours. After cooling, filter, wash and dry the slurry to obtain gray-green manganese phosphate MnPO 4 ·H 2 O powder, manganese phosphate yield is ~ 99%.

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Abstract

The invention discloses a manganese phosphate preparation method, which comprises the following steps: taking concentrated phosphoric acid and potassium permanganate according to a set ratio, and uniformly mixing; reacting the mixture at a set temperature; and after the reaction is finished, filtering, washing and drying the reaction solution to obtain manganese phosphate MnPO4.H2O. According to the invention, different from the traditional technical route for preparing manganese phosphate by oxidizing a low-valence manganese source, the method provided by the invention takes potassium permanganate and commercial phosphoric acid as raw materials, and does not need to additionally add a solvent and an oxidation-reduction agent so as to simplify the reaction process and reduce the cost; compared with the patent CN102849715A preparation method of nano manganese phosphate, the method of the invention has the following characteristics that sulfuric acid and oxalic acid are not needed, extrawater is not needed except water in phosphoric acid, the concentration and pH value of the solution do not need to be controlled, the reaction is simple, and the yield is high; and the method for producing manganese phosphate has the advantages of low cost, simple process, environmental protection and environmental protection, and has industrial value.

Description

technical field [0001] The invention belongs to the technical field of preparation of positive electrode materials of lithium ion batteries, and in particular relates to a preparation method of manganese phosphate. Background technique [0002] Transition metal phosphate is a chemical raw material with a wide range of uses. It can not only be used as an adsorbent, catalyst, ion exchanger, and phosphating agent, but also has potential application prospects in ceramics, dielectrics, magnetism, and electricity. In recent years, manganese phosphate has important application value as the precursor of lithium manganese phosphate, the cathode material of lithium ion batteries. [0003] LiFePO is currently the cathode material for lithium-ion batteries 4 The mainstream preparation method is to use iron phosphate FePO 4 ·H 2 O as a precursor. Manganese phosphate MnPO 4 ·H 2 O precursors are difficult to resemble FePO 4 ·H 2 O is prepared on a large scale, which is mainly due ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/377C01P2002/72C01P2004/03C01P2004/61
Inventor 胡国荣杜柯曹雁冰彭忠东王永志
Owner CENT SOUTH UNIV
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