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Separation method of lithium dihydrogen phosphate and preparation method thereof

A technology of lithium dihydrogen phosphate and separation method, which is applied in the field of preparation of lithium dihydrogen phosphate, can solve problems such as unevenness and large diameter of lithium dihydrogen phosphate particles, and achieve the effect of uniform particle diameter

Inactive Publication Date: 2011-01-26
SHANGHAI BYD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to overcome the defect that the particle diameter of lithium dihydrogen phosphate obtained in the separation method of lithium dihydrogen phosphate in the prior art is relatively large and uneven, and to provide a particle diameter that makes the obtained lithium dihydrogen phosphate A method for separating smaller and uniform lithium dihydrogen phosphate, and a method for preparing lithium dihydrogen phosphate

Method used

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  • Separation method of lithium dihydrogen phosphate and preparation method thereof
  • Separation method of lithium dihydrogen phosphate and preparation method thereof
  • Separation method of lithium dihydrogen phosphate and preparation method thereof

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preparation example Construction

[0029] The preparation method of lithium dihydrogen phosphate provided by the present invention comprises contacting and reacting lithium hydroxide and / or lithium carbonate with phosphoric acid in the presence of water to prepare an aqueous solution containing lithium dihydrogen phosphate, and then cooling and crystallizing to separate dihydrogen phosphate Lithium, wherein, the method for separating lithium dihydrogen phosphate is the method provided by the present invention.

[0030] According to the preparation method provided by the present invention, there is no special restriction on the order of adding lithium hydroxide and / or lithium carbonate, phosphoric acid and water. In order to mix well and uniformly, in preferred cases, add water first, and then add lithium hydroxide And / or lithium carbonate, finally add phosphoric acid to carry out contact reaction in order.

[0031] According to the preparation method provided by the present invention, the dosages of the lithium...

Embodiment 1

[0035] In a reactor equipped with a stirrer and 90°C circulating water in the jacket, 3 liters of water and 2239.1 grams of Li with a purity of 99% were successively added. 2 CO 3 powder and 8093.6 grams of 85% H 3 PO 4 The solution was reacted for 1 hour under stirring at a rotating speed of 800 r / min.

[0036] The reaction produces LiH 2 PO 4Continue heating to evaporate the water until the concentration of the aqueous solution is 80%, move the solution to another reactor equipped with a stirrer, and add 500 grams of liquid nitrogen rapidly under the high-speed stirring condition of 1200r / min , the reaction solution was rapidly cooled to 0°C, and LiH 2 PO 4 crystal particles. The mixed solution containing the crystal is centrifuged, and the separated solid product is poured into 7483 grams of ethanol solution stirred at a speed of 1200r / min for washing, then filtered, and finally dried at 60°C for 5 hours, and the separated liquid The product is subjected to the same...

Embodiment 2

[0040] In a reactor equipped with a stirrer and 98°C circulating water in the jacket, 5 liters of water and 2543.4 grams of LiOH·H with a purity of 99% were successively added. 2 O powder and 7609.1 g of 85% pure H 3 PO 4 solution, and reacted for 2 hours under stirring at a rotating speed of 800r / min.

[0041] The reaction produces LiH 2 PO 4 Continue heating to evaporate the water until the concentration of the aqueous solution is 70%, move the solution to another reactor equipped with a stirrer, and add 500 grams of liquid nitrogen rapidly under the high-speed stirring condition of 1200r / min , the reaction solution was rapidly cooled to 8°C, and LiH 2 PO 4 crystal particles. The mixed solution containing the crystal is centrifuged, and the separated solid product is poured into 9354 grams of ethanol solution stirred at a speed of 1200r / min for washing, then filtered, and finally dried at 90°C for 3 hours, and the separated liquid The product was subjected to the same...

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Abstract

The invention relates to a separation method for lithium dihydrogen phosphate, which comprises the steps: water solution containing lithium dihydrogen phosphate is cooled and crystallized, wherein, the cooling and crystallizing method comprises that a refrigerant is added into the water solution containing the lithium dihydrogen phosphate, and the amount of the refrigerant can lead the temperature of the water solution containing the lithium dihydrogen phosphate to be reduced to 0 DEG C to 20 DEG C so as to cause lithium dihydrogen phosphate to be crystallized. The particle diameter of the products prepared by adopting the method of the invention is small and the particle size is uniform.

Description

technical field [0001] The invention relates to a method for separating lithium dihydrogen phosphate, and also relates to a method for preparing lithium dihydrogen phosphate. Background technique [0002] At present, the cathode material commonly used in lithium batteries is lithium cobalt oxide (LiCoO 2 ), lithium nickel cobalt oxide (LiNi x co 1-x o 2 ), lithium nickel cobalt manganese oxide (LiNi x co y mn 1-x-y o 2 ) and lithium manganate (LiMn 2 o 4 ). They have high electrical conductivity and reversible Li-ion deintercalation. However, they react violently with the electrolyte when the battery is overcharged and overheated, releasing a large amount of heat that can cause the battery to catch fire or even explode, so they are less safe and costly. Lithium manganate (LiMn 2 o 4 ) is relatively cheap and safe, but it not only has a small discharge capacity, but also has poor cycle life under high temperature conditions, and its cycle life cannot meet the req...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/30
Inventor 夏文强徐茶清姜占峰贾文雯
Owner SHANGHAI BYD