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Preparation method of special alumina for high-purity lithium battery separation membranes

A lithium battery separator and battery separator technology, which is applied to lithium batteries, chemical instruments and methods, battery pack components, etc. The problem of high cost of elution of sodium, to achieve the effect of controllable crystal microscopic morphology, ideal phase composition, and low cost

Active Publication Date: 2019-10-22
苏州盛曼特新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this process is: there is a technical limit in the pickling process for sodium removal, and once pickling Na 2 O can be reduced to about 0.07%, and can only be reduced to about 0.03% after two steps, and the cost of acid washing to remove sodium is very high. Usually, industrial production is difficult to accept the cost of two-step pickling; in addition, after high-temperature calcination, alumina Crystal size and micromorphology are relatively difficult to control, α-Al 2 o 3 The microscopic morphology of the film mainly presents a flaky structure, and it is still difficult to completely achieve a spherical structure through mechanical grinding. The sharp particles are easy to scratch the diaphragm, resulting in coating defects and potential safety hazards on the diaphragm.
But the crystal size of alumina superfine powder raw material is D 50 At about 1 μm, further microcrystallization has not yet been achieved

Method used

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  • Preparation method of special alumina for high-purity lithium battery separation membranes
  • Preparation method of special alumina for high-purity lithium battery separation membranes
  • Preparation method of special alumina for high-purity lithium battery separation membranes

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Experimental program
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Effect test

Embodiment 1

[0039] A kind of preparation method of aluminum oxide for lithium battery diaphragm (flow chart is as figure 1 ), the steps are as follows: aluminum hydroxide material (D 50 = 8.1 μm, Na 2 O=0.37%, Fe 2 o 3 = 0.012%, SiO 2 =0.008%, water content 0.40%) and superfine aluminum hydroxide seed crystal (D 50 = 2.5 μm, Na 2 O=0.39%, Fe 2 o 3 =0.011%, SiO 2 =0.0082%, water content 0.45%) according to the mass ratio of 8:1 mixed to obtain the mixture M1, the mixture M1 and ammonia (ammonia nitrogen content is 26%) according to the mass ratio of 100:1 mixed to obtain the mixture M2, add Soft water to adjust the solid content to 220g / L; set the reaction temperature of the reactor to 220°C, and the holding time to 2h. After the hydrothermal reaction, filter and dry to obtain boehmite; put the boehmite into a high-temperature furnace, Calcined at 1200°C for 3 hours, then high-efficiency grinding and spray drying in a horizontal sander to obtain powder, that is, α-Al 2 o 3 Ultra...

Embodiment 2

[0042] A kind of preparation method of alumina for lithium battery separator, the steps are as follows: aluminum hydroxide (D 50 = 8.1 μm, Na 2 O=0.37%, Fe 2 o 3 = 0.012%, SiO 2 =0.008%, water content 0.40%) and superfine aluminum hydroxide seed crystal (D 50 = 2 μm, Na 2 O=0.39%, Fe 2 o 3 =0.011%, SiO 2 =0.0082%, water content 0.45%) according to the mass ratio of 8:2 mixed to obtain the mixture M1, then, M1 and ammonia water (ammonia nitrogen content is 26%) according to the mass ratio of 100:2 to obtain the mixture M2, Add soft water to adjust the solid content to 240g / L; set the reaction temperature of the reactor to 220°C, and the holding time to 2h. After the hydrothermal reaction is completed, filter and dry to obtain boehmite; put the boehmite into a high-temperature furnace, Calcined at a high temperature of 1200°C for 3 hours, and then efficiently ground through a jet mill to obtain α-Al 2 o 3 Ultrafine powder. The parameters of the jet mill are: the batch...

Embodiment 3

[0045] A kind of preparation method of alumina for lithium battery separator, the steps are as follows: aluminum hydroxide (D 50 = 8.1 μm, Na 2 O=0.37%, Fe 2 o 3 = 0.012%, SiO 2 =0.008%, water content 0.40%) and superfine aluminum hydroxide seed crystal (D 50 = 2 μm, Na 2 O=0.39%, Fe 2 o 3 =0.011%, SiO 2 =0.0082%, water content 0.45%) according to the mass ratio of 8:3 mixed to obtain the mixture M1, then, M1 and ammonia (ammonia nitrogen content is 26%) according to the mass ratio of 100:2 mixed to obtain the mixture M2, add Soft water adjusts the solid content to 250g / L, sets the reaction temperature of the reactor to 210°C, and the holding time to 1.5h. After the hydrothermal reaction is completed, filter and dry to obtain boehmite; put the boehmite into a high-temperature furnace, Calcined at a high temperature of 1100°C for 3 hours, and then efficiently ground through a jet mill to obtain α-Al 2 o 3 Ultrafine powder. The parameters of the jet mill are: the batc...

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Abstract

The invention discloses a preparation method of special alumina for high-purity lithium battery separation membranes. The preparation method comprises: preparing boehmite by using aluminum hydroxide as a raw material, using ultrafine aluminum hydroxide as a seed crystal, using ammonia water as an additive and using soft water as a reaction medium through a hydrothermal reaction; carrying out hightemperature calcination on the boehmite to obtain alpha-Al2O3 raw powder; and grinding the alpha-Al2O3 raw powder by a horizontal sander, and carrying out spray drying, or grinding by a jet mill to obtain the alumina for lithium battery separation membranes. According to the present invention, sodium oxide impurities can be removed through the hydrothermal reaction; and the obtained alumina has characteristics of high chemical purity, controllable crystal micro-morphology and relatively narrow particle size distribution, has the Al2O3 content of more than or equal to 99.95%, has the Na2O content of less than or equal to 0.02%, has the contents of impurities such as Fe2O3 and the like of less than or equal to 70 ppm, mainly has spherical and cubic structure, has a specific surface area of 3.5-6.0 m<2> / g, and can meet the requirements of electrochemical performance and safety performance of lithium battery separation membrane materials.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic non-metallic materials, and relates to a method for preparing alumina for lithium battery separators, in particular to a method for preparing special alumina for high-purity microcrystalline lithium battery separators, and the prepared alumina is applied to lithium battery separators Coating of material surfaces. Background technique [0002] Lithium battery separator is a thin film with a microporous structure (PE, PP, PE-PP composite film). As a key structural component with the most technical barriers in the lithium battery industry, its performance directly affects battery capacity, internal resistance , cycle performance, current density and safety performance. The biggest safety hazard of lithium batteries is the random internal short circuit of the battery. In order to solve this safety hazard, a thin layer of aluminum oxide coating needs to be coated on the lithium battery diaphragm....

Claims

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Application Information

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IPC IPC(8): C01F7/44H01M2/16H01M10/052
CPCC01F7/441C01P2004/51C01P2006/12C01P2006/80H01M10/052H01M50/431Y02E60/10
Inventor 张举张兰银
Owner 苏州盛曼特新材料有限公司
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