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Preparation method of macropore mayenite block body

A macroporous calcium-aluminum and stone technology is applied in the field of preparation of mayenite block materials to achieve the effects of high porosity, simple preparation process and reduced preparation cost

Active Publication Date: 2017-05-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of chlorine-containing precursors, free oxygen ions are easily replaced by chloride ions during the crystallization of mayenite, thereby forming Ca 12 Al 14 o 32 Cl 2 , rather than the pure mayenite compound

Method used

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  • Preparation method of macropore mayenite block body
  • Preparation method of macropore mayenite block body
  • Preparation method of macropore mayenite block body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0025] Embodiment 1-1, a method for preparing a macroporous mayenite block, the following steps are performed in sequence:

[0026] 1), at room temperature, dissolve 0.6 g of polyvinylpyrrolidone as a phase separation inducer in a mixed solvent composed of 2.5 g of water and 3.5 g of ethanol (absolute ethanol), and after magnetic stirring, add nine 1.0g of aluminum nitrate hydrate and 0.6g of calcium nitrate tetrahydrate, 0.1ml of polystyrene microspheres (particle size: 50-100nm) as a template agent and 0.3ml of ethylene glycol as a chelating agent and stir for 50-70min, after stirring evenly Add 2.5ml of propylene oxide as a gel accelerator, ultrasonic (frequency 53KHz, output power 100%, water temperature 20°C) for 10-20 seconds to obtain a homogeneous solution;

[0027] 2), put the homogeneous solution obtained in step 1) in an airtight container, and react in an oven at 35-45°C for 24 hours;

[0028] 3) The aged gel obtained in step 2) is dried in a vacuum environment (v...

Embodiment 1-2

[0031] The phase separation inducer polyvinylpyrrolidone in step 1) of Example 1-1 was changed from 0.6 g to 0.2 g; the rest were the same as in Example 1-1.

[0032] Observation by scanning electron microscope at low magnification and high magnification, mayenite still has a coherent macroporous structure at the same time, but with the decrease of polyvinylpyrrolidone amount, the macropore diameter decreases as ( figure 2 , the pore size is about 0.2 μm), which is due to the weakening of the phase separation effect of polyvinylpyrrolidone. According to the mercury intrusion test, the porosity of the macroporous mayenite block prepared in this embodiment is 64%.

Embodiment 1-3

[0034] The phase separation inducer polyvinylpyrrolidone in step 1) of Example 1-1 was changed from 0.6 g to 1.5 g; the rest were the same as in Example 1-1.

[0035] The microscopic morphology of the mayenite block has changed to the accumulation of mayenite particles by scanning electron microscopy at low and high magnifications, that is, it does not present a coherent macropore structure, such as image 3 , this is because with the increase of the amount of polyvinylpyrrolidone, the phase separation effect of polyvinylpyrrolidone is further enhanced, and excessive phase separation occurs. The porosity is 56% according to the mercury intrusion test.

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Abstract

The invention discloses a preparation method of a macropore mayenite block body. The preparation method comprises the following steps: 1) at room temperature, dissolving 0.2 to 1.5 g of a phase-separation inducer into 5 to 7 g of a mixed solvent, after stirring uniformly, adding 1.0 g of aluminum nitrate nonahydrate, 0.6 to 0.8 g of calcium nitrate tetrahydrate, 0.1 ml of a template and 0.3 ml of a chelating agent for stirring for 50 to 70 min, and then adding 1.5 to 2.5 ml of a gel accelerant for ultrasonic treatment for 10 to 20 seconds so as to obtain a homogenizing solution; 2) putting the homogenizing solution obtained in the step 1) into a closed container, and conducting reaction in a drying oven at the temperature of 35 to 45 DEG C for 24+ / -1 hours; 3) putting aged gel obtained in the step 2) in a vacuum environment at the temperature of 50 to 70 DEG C for drying for 80 to 90 h; then carrying out heat temperature at the temperature of 400 to 1100 DEG C for 2 to 4 h so as to obtain the macropore mayenite block body.

Description

technical field [0001] The invention belongs to the field of preparation of porous block materials, in particular to a method for preparing mayenite block materials with a co-continuous macroporous structure. Background technique [0002] A porous block refers to a block-like material with a certain size and number of ordered pore structures. According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), a block is an article that has a certain shape, can be structured, has a uniform microstructure, and is difficult to process. Because of its low relative density, high specific surface area, good permeability and superior adsorption performance, porous blocks are widely used as carrier materials in the fields of adsorption, separation, filtration, catalysis, etc. hotspot. [0003] Nakanishi's group first reported the phenomenon of sol-gel accompanied by phase separation in siloxane systems, and initially established a theoretical criterion fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B38/00C04B35/44C04B35/624
CPCC04B35/44C04B35/624C04B38/0054C04B38/0003C04B38/0045C04B38/0074
Inventor 郭兴忠王睿白盛池杨辉
Owner ZHEJIANG UNIV