Method for preparing difluorophosphates
A technology of difluorophosphate and hexafluorophosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of increasing labor and time costs, increasing the difficulty of purification and separation, and increasing the difficulty of purification. Residence time, increase the effect of mass transfer and heat transfer, the effect of excellent mass transfer and heat transfer effect
Inactive Publication Date: 2017-05-31
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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However, difluorophosphoric acid is used to synthesize difluorophosphate, because a large amount of by-product hydrohalic acid or water will be generated during the synthesis process, which increases the difficulty of subsequent purification and increases the cost; while using phosphorus pentoxide and LiF for synthesis, High energy consumption, more lithium phosphate by-products, greatly increase the difficulty of subsequent purification and separation; in addition, the traditional kettle reaction has a long installation period, heavy workload, increased manpower and time costs, and low efficiency
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[0027] The technical solutions of the present invention will be further described below in conjunction with specific examples, but the protection scope of the present invention is not limited thereto. The raw materials used in the following examples are commercially available unless otherwise specified.
[0028] The preparation method of difluorophosphate comprises the following steps: prepare 300g of hexafluorophosphate solution in a container, add a certain amount of cyclosiloxane or acetal in another container, and (use a metering pump to set a certain metering ratio) into the microchannel The reactor reacts at a constant temperature, and the obtained reaction solution is filtered through a membrane, then concentrated and dried to obtain a difluorophosphate solid. The raw materials and parameters of specific examples are shown in Table 1.
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Abstract
The invention belongs to the technical field of lithium-ion batteries and particularly relates to an efficient method for preparing difluorophosphates. The method comprises the following steps: metering a hexafluorophosphate solution with the concentration being 5wt% to 50wt% and a cyclosiloxane or an acetal, then, introducing the metered materials to a microchannel reactor, carrying out a reaction for 60 to 900 seconds at the temperature of 20 DEG C to 150 DEG C, carrying out membrane filtration on an obtained reaction solution, and then, carrying out concentrating and drying, thereby obtaining a corresponding difluorophosphate product. The method disclosed by the invention has the advantages that the process route is simple, the raw materials are readily available, the reaction efficiency is high, the energy consumption is low, the product purity is high, and the like.
Description
technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a method for preparing an efficient difluorophosphate. Background technique [0002] At present, with the widespread application of portable electronic mobile devices and the country's strong support for electric vehicles, the demand for lithium-ion batteries continues to increase, especially for lightweight, high-performance lithium-ion batteries, and the safety performance requirements of lithium-ion batteries are also increasing. Higher and higher. Difluorophosphate, especially lithium difluorophosphate, as an electrolyte salt additive for lithium-ion batteries, has aroused widespread interest in lithium battery manufacturers due to its excellent properties of improving low-temperature performance of batteries. [0003] There are many existing synthetic methods of difluorophosphate, and Chinese patent CN102985361 adopts P 4 o 10 and LiF at a high t...
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IPC IPC(8): C01B25/455
CPCC01B25/455C01P2002/82C01P2002/86
Inventor 刘陈海
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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