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Preparation method for porous lithium zirconate block

A lithium zirconate block technology, which is applied in the field of preparation of porous lithium zirconate blocks, can solve the problems of undiscovered porous lithium zirconate block materials with co-continuous pore structure, and achieve low price and controllable pore quantity , skeleton continuous effect

Active Publication Date: 2015-04-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the patent whose publication number is CN101214977, the inventor introduced a kind of nanoscale ZrO 2 with micron Li 2 CO 3 compound method to prepare lithium zirconate material; in the patent publication number 102351244A, the inventor introduced a method for preparing lithium zirconate powder by sol-gel method; Related reports on porous lithium zirconate bulk materials

Method used

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  • Preparation method for porous lithium zirconate block
  • Preparation method for porous lithium zirconate block
  • Preparation method for porous lithium zirconate block

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Embodiment 1

[0031] Embodiment 1, a kind of preparation method of porous lithium zirconate block body, first prepare main raw material according to following ratio: With 0.0025mol (about 0.70g) zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O) as the source of zirconium, with 0.005mol (about 0.45g) of lithium acetate dihydrate (LiAc·2H 2 O) is the lithium source, with ethylene glycol (EG) of 0.40ml as a complexing agent, with 0.32g polyoxyethylene (PEO, the average molecular weight is 1000000) as a phase separation inducer, with 0.50ml of propylene oxide (PO ) is a gel accelerator; carry out the following steps successively:

[0032] 1), at room temperature, respectively dissolve zirconium oxychloride octahydrate, lithium acetate dihydrate, polyoxyethylene and ethylene glycol in 7ml solvent (the solvent is mixed with deionized water and absolute ethanol according to the volume ratio of 1:0.4 obtained), after stirring for 2 to 3 hours, a transparent and clear solution was obtained;

[...

Embodiment 2

[0041] Embodiment 2. A preparation method of a porous lithium zirconate block, the heat treatment temperature in step 5) of embodiment 1 is changed from 650° C. to 800° C., and the rest is the same as that of embodiment 1.

[0042] The prepared porous lithium zirconate block remains intact and has a small amount of shrinkage, but its co-continuous pore structure and porosity are good, with a porosity of 40%. The lithium zirconate is a mixture of tetragonal phase and monoclinic phase , has good adsorption properties.

Embodiment 3

[0043] Embodiment 3, a preparation method of a porous lithium zirconate block, the zirconium source in embodiment 1 is changed from zirconium oxychloride octahydrate to zirconyl nitrate (0.0025mol), and the lithium source is changed from lithium acetate dihydrate to nitric acid Lithium (0.005mol), complexing agent is changed into citric acid (0.40ml) by ethylene glycol, all the other are equal to embodiment 1.

[0044] The prepared porous lithium zirconate block remains intact, and the microstructure is shown in Figure 5 As shown, its co-continuous pore structure and porosity are good, and the lithium zirconate block also has good performance.

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Abstract

The invention discloses a method for a porous lithium zirconate block. The method comprises the following steps sequentially: (1), dissolving inorganic zirconium salt, inorganic lithium salt, a complexing agent and a phase separation inducer in a solvent, and stirring until a transparent clear solution is obtained; (2), slowly adding a gel accelerator into the transparent clear solution, uniformly stirring, and ultrasonically processing in an ultrasonic instrument until air bubbles in the solution are removed; (3), putting a homogenous solution obtained in the step (2) into a container, sealing, and gelling at 60-90 DEG C for 5-25 minutes to obtain wet gel; (4), ageing the wet gel obtained in the step (3) at 60-90 DEG C for 4-10 hours; (5), drying the aged gel obtained in the step (4) at 20-50 DEG C for 50-100 hours, heating to 650-1,200 DEG C, and performing heat treatment for 6-12 hours to obtain the porous lithium zirconate block. The porous lithium zirconate block prepared with the method has the characteristics of common continuous porous structure and the like.

Description

technical field [0001] The invention relates to a preparation method for preparing a porous lithium zirconate block, in particular to a preparation method for preparing a porous lithium zirconate block by an epoxy-regulated sol-gel accompanying phase separation method. Background technique [0002] Lithium zirconate (usually with the formula Li 2 ZrO 3 ) is Li 2 O-ZrO 2 A functional ceramic with great application prospects in the binary system. Lithium zirconate has two crystal structures of tetragonal phase and monoclinic phase. In the low temperature zone (500-700°C), the calcined product is tetragonal phase lithium zirconate powder, and contains a considerable amount of amorphous components; 850°C) the calcined product is a mixed powder of tetragonal phase and monoclinic lithium zirconate; in the high temperature zone the calcined product is monoclinic lithium zirconate powder. Quartet 2 ZrO 3 Metastable, it will transform into a stable monoclinic phase at elevated...

Claims

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Application Information

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IPC IPC(8): C04B38/00C04B35/48C04B35/624
Inventor 郭兴忠任静杨辉朱文均
Owner ZHEJIANG UNIV
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