Micro-chemical preparation method of nano-iron phosphate and nano-iron phosphate

Abstract

The invention discloses a nano iron phosphate micro chemical preparation method and nano iron phosphate. The method comprises the following steps of: S1, respectively dissolving soluble iron salt and phosphate into deionized water according to a ratio that Fe: P=1:(0.8-1.2), wherein the concentrations of solutions are both 0.1-1mol / L, and the final volume parts of an iron salt solution and a phosphate solution are the same; S2, weighing and dissolving a surfactant which can theoretically generate 1wt.%-10wt.% of iron phosphate into the iron salt solution; S3, dropwise adding ammonia water into the phosphate solution, and regulating the pH to be 8-10; S4, regulating the rotation speed of a mechanical pump to be 10-300 rounds / minute, simultaneously adding the same flow of the iron salt solution and the phosphate solution into a microreactor of a micro chemical system to react for 10-60 minutes, and thus obtaining a turbid liquid; and S5, filtering and separating the turbid liquid, washing and drying at 70-90 DEG C so as to obtain spherical nano iron phosphate. The method can be used for preparing the nano iron phosphate with regular shape, good dispersibility, uniform size distribution and high reactivity.

Description

technical field [0001] The invention relates to the preparation technology of the cathode material of the lithium ion secondary battery, in particular to a micro-chemical preparation method of nano-iron phosphate and a nano-iron phosphate. Background technique [0002] For lithium-ion batteries, its wide application mainly depends on battery performance, price and safety. The further improvement of the performance of lithium-ion batteries depends to a large extent on the improvement of the performance of positive and negative electrode materials, and the decline in the cost of lithium-ion batteries depends largely on the decline in the cost of positive electrode materials. Therefore, the development of positive electrode materials with good performance and price has become the focus of lithium-ion battery research. At present, the development of cathode materials for lithium-ion batteries is relatively lagging behind, which seriously affects the powerization process of lith...

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Problems solved by technology

[0005] The disclosed ferric phosphate preparation method generally uses a conventional tank reaction, which has obvious defects such as time-consuming and discontinuous processes for auxiliary operations such as loading and unloading; Weak, poor ability to control the reaction process, resulting in poor product quality stability

[0006] The patent application with the publication number CN101891176A discloses a method for preparing iron orthophosphate for lithium-ion battery materials with non-ionic surfactants, but the particle size of the prepared iron orthophosphate is large and uneven (50-300nm), indicating that Simple non-ionic surfactants can not play a good dispersion effect, this method is not suitable for the preparation of lithium iron phosphate precursor iron phosphate

The patent application with the publication number CN10695998A discloses a method for preparing nanoscale iron phosphate. Although the particle size of the prepared iron phosphate is small, the distribution is uneven (10-100nm), and the rotating packed bed reactor used Complicated to use, not suitable for mass production

In the patent application with the publication number CN1021101662A, ferrous oxalate and phosphoric acid are used as raw materials to prepare anhydrous crystalline ferric phosphate. Because of the high temperature treatment at 500°C in the process, the energy consumption is large and the ferric phosphate is easy to grow. The performance of lithium has adverse effects on

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