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Doping modified lithium ion sieve and preparation method thereof

A technology of lithium ion modification, which is applied in the field of doped modified lithium ion sieve and its preparation, can solve the problems of reducing manganese dissolution loss rate, reduce dissolution loss, reduce manganese dissolution loss, and improve cycle stability Effect

Pending Publication Date: 2022-03-01
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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Problems solved by technology

[0005] In view of the deficiencies in the prior art, the present invention provides a doped modified lithium ion sieve and its preparation method to solve the problem of how to reduce the manganese dissolution rate of lithium manganese oxide lithium ion sieve

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  • Doping modified lithium ion sieve and preparation method thereof
  • Doping modified lithium ion sieve and preparation method thereof
  • Doping modified lithium ion sieve and preparation method thereof

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preparation example Construction

[0037] refer to figure 1 , the preparation method of the lithium ion sieve of doping modification as mentioned above comprises the following steps:

[0038] Step S10, using a sol-gel method, dissolving the aluminum salt and manganese carbonate in an organic solvent, stirring and mixing evenly, and then drying to obtain manganese carbonate powder coated with aluminum salt.

[0039] In a specific scheme, the aluminum salt can be selected as C 9 h 21 o 3 Al, AlCl 3 、Al 2 (SO 4 ) 3 or Al 2 (SiO 3 ) 3 . The organic solvent is, for example, ethanol.

[0040] In a specific scheme, the aluminum salt and the manganese carbonate are mixed according to a molar ratio of aluminum element to manganese element of 1:(15-31). Preferably, the molar ratio of aluminum and manganese is mixed in a ratio of 1:20.

[0041] Step S20, performing a first calcination treatment on the manganese carbonate powder coated with aluminum salt in an air or oxygen atmosphere to obtain a first calcina...

Embodiment 1

[0059] (1), using the sol-gel method, according to the ratio of the molar ratio of Al to Mn is 1:20, the C 9 h 21 o 3 Al and MnCO 3 Dissolved in ethanol, stirred evenly and dried.

[0060] (2) Put the dried powder in step (1) in a calciner, feed air, control the heating rate to 5°C / min to 800°C, and calcinate at 800°C for 5h.

[0061] (3) The calcined product of step (2) is mixed with lithium hydroxide according to the molar ratio of Li to Mn of 1.05:1, ground, and then heated at 120° C. for 24 hours for drying.

[0062] (4) Place the dried product of step (3) in a calciner, feed in air, control the temperature rise rate to 5°C / min to 450°C, and calcinate at 450°C for 5h.

[0063] (5), the calcined product of step (4) and NH 4 F is ground after mixing according to the molar ratio of O and F of 3.95:0.05.

[0064] (6), the ground product of step (5) is placed in a calciner, air is introduced, the temperature rise rate is controlled to be 5° C. / min and the temperature is r...

Embodiment 2

[0069] The difference between embodiment 2 and embodiment 1 is: in step (5), the calcined product of step (4) is mixed with NH 4 F is ground after mixing according to the molar ratio of O and F of 3.95:0.1. The remaining process steps of embodiment 2 are exactly the same as those of embodiment 1, so they are not repeated here.

[0070] In this example, a doped modified lithium ion sieve product 2 was prepared.

[0071] Lithium ion sieve product 2 obtained in this embodiment is carried out XRD test and SEM test respectively, obtains Figure 4 The XRD patterns and Figure 5 SEM image.

[0072] according to Figure 4 Shown XRD collection of illustrative plates, the lithium ion sieve product 2 of the present embodiment still keeps the same as Li 1.6 mn 1.6 o 4 The same characteristic peaks, compared with the lithium ion sieve product 1 of Example 1, no impurity phase occurs, and the lattice parameter is slightly reduced, as

[0073] according to Figure 5 As shown in th...

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Abstract

The invention discloses a doped modified lithium ion sieve and a preparation method thereof.The preparation method comprises the steps that a sol-gel method is adopted, aluminum salt and manganese carbonate are dissolved in an organic solvent, the mixture is evenly mixed and then dried, and manganese carbonate powder coated with the aluminum salt is obtained; carrying out first calcining treatment on the manganese carbonate powder coated with the aluminum salt in an air or oxygen atmosphere to obtain a first calcined product; mixing the first calcined product with lithium hydroxide, grinding, heating and drying to obtain first ground powder; carrying out second calcination treatment on the first grinding powder in an air or oxygen atmosphere to obtain a second calcined product; mixing the second calcined product with fluoride, and grinding to form second grinding powder; and carrying out third calcination treatment on the second ground powder in an air atmosphere to obtain the aluminum and fluorine co-doped modified lithium manganese oxide lithium ion sieve. According to the doped modified lithium ion sieve prepared by the invention, the manganese solution loss rate of the lithium manganese oxide lithium ion sieve can be reduced.

Description

technical field [0001] The invention relates to the technical field of lithium ion extraction, in particular to a doped modified lithium ion sieve and a preparation method thereof. Background technique [0002] Lithium is known as "the new energy metal of the 21st century" and has a wide range of applications in new energy materials, medicine, ceramic glass, and lithium-ion secondary batteries. Lithium resources mainly exist in two forms of solid minerals and liquid deposits in nature, and most of them are distributed in brine and seawater. Lithium present in salt lake brine is characterized by a high ratio of magnesium to lithium, and because the properties of magnesium and lithium are very similar, the concentration of lithium is low, which has caused great difficulties in the extraction of lithium from salt lake brine. [0003] At present, the methods for extracting lithium from salt lakes mainly include: precipitation method, solvent extraction method, calcination leach...

Claims

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Application Information

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IPC IPC(8): B01J20/04B01J20/30
CPCB01J20/041
Inventor 海春喜张果泰周园曾金波申月孙艳霞董生德彭桂萍
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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