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Preparation method of iron phosphate and lithium iron phosphate

A technology of lithium iron phosphate and iron phosphate, which is applied in the field of preparation of positive electrode materials for lithium ion batteries, can solve the problems of inability to effectively control the size and morphology of the product iron phosphate, increase the difficulty of environmental protection and complexity, and achieve green production efficiency and product quality. The effect of uniform composition and simple preparation method

Inactive Publication Date: 2020-09-08
HUNAN YACHENG NEW MATERIAL CO LTD
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  • Description
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Problems solved by technology

[0004] The synthetic method of ferric phosphate industrialization in the prior art is the liquid phase precipitation method, promptly uses hydrogen peroxide to oxidize divalent iron salt into ferric iron, and then uses phosphoric acid or phosphate and ferric iron to generate ferric phosphate precipitation, although this method can Ferric phosphate is prepared in batches, but it cannot effectively control the size and shape of the product. In addition, the entire process is relatively long and involves processes such as press filtration, washing, drying, calcination, and crushing, which are time-consuming Long (usually more than 12 hours) and will generate a lot of washing wastewater, increasing the difficulty of environmental protection
Chinese invention patent application document CN110002417A discloses a low-cost anhydrous iron phosphate preparation method, which specifically discloses adding iron oxide red material to phosphoric acid, adding anhydrous alcohol and stirring, passing through a spray dryer, using hot nitrogen as a heat source , maintain the nitrogen inlet air temperature at 220-250°C, and the discharge temperature at 110-130°C. After obtaining the dried material, wash it with absolute alcohol for several times until the free phosphoric acid content in the dried material is lower than 20ppm, and then wash the dried material The material is dried to obtain anhydrous iron phosphate. Although this method must avoid the long process flow and time-consuming problems of the liquid phase precipitation method, it still needs to be washed repeatedly to remove free phosphoric acid, resulting in a large amount of waste water and still operating. Complicated

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  • Preparation method of iron phosphate and lithium iron phosphate
  • Preparation method of iron phosphate and lithium iron phosphate
  • Preparation method of iron phosphate and lithium iron phosphate

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Embodiment 1

[0032] Embodiment 1 of the present invention is: a preparation method of iron phosphate, such as figure 1 shown, including the following steps:

[0033] 1) prepare ferric salt solution and phosphate solution respectively, wherein, ferric salt (selected from FeCl 3 ·6H 2 O, FeCl 3 , Fe(NO 3 ) 3 9H 2 O, Fe(NO 3 ) 3 , Fe 2 (SO 4 ) 3 at least one of) solution and phosphate (selected from NH 4 h 2 PO 4 , (NH 4 ) 2 HPO 4 , (NH 4 ) 3 PO 4 , CO(NH 2 ) 2 ·H 3 PO 4 The concentration of at least one of the solutions) does not exceed 1.5mol / L; preferably between 0.1 and 1.5mol / L;

[0034] 2) mixing and stirring the iron salt and phosphate prepared in step 1) to form a mixed solution, wherein the molar ratio of phosphate and iron salt is 1:1;

[0035] 3) After reacting the mixed solution obtained in step 2) at room temperature for 0.5 to 3 hours, carry out spray pyrolysis (atomize the mixed solution at a rate of 10 to 100ml / h and pass it through a pyrolysis tube fur...

Embodiment 2

[0043] Embodiment 2 of the present invention is: a preparation method of iron phosphate, comprising the following steps: adding 27.0g FeCl to 100mL deionized water 3 ·6H 2 O and stir to dissolve completely then add 11.5g NH 4 h 2 PO 4 and stir for 10 minutes to dissolve completely. Thereafter, the obtained mixed solution was stirred and reacted at normal temperature for 0.5 hours. Subsequently, the mixed solution was first atomized by a spray pyrolysis device at a rate of 40 ml / h, and passed through a pyrolysis tube furnace at 600° C. under the delivery of carrier gas (air). The carrier gas flow rate was controlled at 4L / min. Finally, iron phosphate material powder is collected at the end of the pyrolysis furnace.

[0044] The product obtained by the above synthetic method was characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM), and the results were as follows: figure 2 and 3 shown. From figure 2 It can be seen from the figure that all t...

Embodiment 3

[0046] Embodiment three of the present invention is: a preparation method of iron phosphate, comprising the following steps: adding 40.5g FeCl to 100mL deionized water 3 ·6H 2 O and stir to dissolve completely then add 17.25g NH 4 h 2 PO 4 and stir for 15 minutes to dissolve completely. After that, the obtained mixed solution was stirred and reacted at normal temperature for 1 hour. Subsequently, the mixed solution was first atomized by a spray pyrolysis device at a rate of 15 ml / h, and passed through a pyrolysis tube furnace at 650° C. under the transport of carrier gas. The carrier gas flow rate was controlled at 7L / min. Finally, iron phosphate material powder is collected at the end of the pyrolysis furnace. The product obtained by the above synthesis method is characterized by SEM, the results are as follows: Figure 4 shown. From Figure 4 It can be seen that the product is a spherical FePO with a diameter of 0.2-5 microns 4 crystals. The detection specific sur...

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Abstract

The invention discloses a preparation method of iron phosphate and lithium iron phosphate. The preparation method of iron phosphate comprises the following steps: S1, preparing a mixed solution containing iron salt and phosphate; S2, performing spray pyrolysis on the mixed solution prepared in the step S1 to obtain iron phosphate, the concentrations of the ferric salt and the phosphate in the mixed solution in the step S1 do not exceed 1.5 mol / L, and the ratio of the amount of substance of the ferric salt to the amount of substance of the phosphate is (0.95-1.05):(0.95-1.05); the mixed solution in the step S2 is atomized at the rate of 10-100 ml / h and then reacts at the temperature of 500-750 DEG C, and the flow rate of carrier gas is 1-15 L / min. Compared with the prior art, the preparation method is simple, efficient, environment-friendly, controllable and stable, and the limitations of long time, large waste liquid amount and the like of an iron phosphate preparation method in the prior art are avoided.

Description

technical field [0001] The invention relates to the technical field of lithium batteries, in particular to the preparation technology of positive electrode materials of lithium ion batteries. Background technique [0002] With the emphasis on new energy vehicles in recent years, lithium-ion battery technology has developed rapidly. Lithium-ion battery is a kind of secondary battery, which mainly relies on the movement of lithium ions between the positive electrode and the negative electrode to work. During the charging and discharging process, Li + Intercalation and deintercalation between the two electrodes to achieve energy storage and supply. Lithium-ion batteries are mainly composed of positive electrodes, negative electrodes, and electrolytes. Among them, the performance of positive electrode materials has a direct impact on the performance of lithium-ion batteries, and its cost also plays a decisive role in the total cost of batteries. [0003] At present, the commer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/45H01M4/58
CPCC01B25/375C01B25/45C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2004/62C01P2006/12C01P2006/40H01M4/5825H01M10/0525Y02E60/10
Inventor 杨政万文治丁建华
Owner HUNAN YACHENG NEW MATERIAL CO LTD