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Preparation method for mesopore/macropore compound hole structure silica gel and silicon and aluminum oxide material

A compound pore and mesoporous technology, applied in chemical instruments and methods, silicon oxide, silicon dioxide, etc., can solve the problems of long aging time and high gel temperature

Active Publication Date: 2014-07-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still problems of high gel temperature and long aging time. We solve these problems by changing the type of silicon source

Method used

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  • Preparation method for mesopore/macropore compound hole structure silica gel and silicon and aluminum oxide material
  • Preparation method for mesopore/macropore compound hole structure silica gel and silicon and aluminum oxide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 15 grams of hydrochloric acid solution of 1 mol / liter, add 2.0 grams of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 5000, P123) and stir to dissolve at room temperature, add polyethylene glycol (molecular weight 10000) to the mixed solution 0.7 g, transferred to an ice-water mixed bath and continued to stir for 5 minutes. Add 5 grams of 1,6-bis(trimethoxysilyl)hexane to the mixed solution, stir vigorously for 10 minutes, pour the mixed solution into a mold and seal it, let it stand at room temperature for 0.1 hour, take it out, demould it, and dry it at room temperature , and finally baked at 550°C for 5 hours. figure 1 It is the SEM photo of the product, which shows that the product has a continuous double continuous macroporous structure, and the specific texture parameters are: specific surface area 951 meters 2 / g, the pore volume is 1.5 cm3 / g, the macropore diameter is 0.2 micron, and the mesopore diameter is 7 nanometers.

Embodiment 2

[0017] Weigh 10 grams of 0.5 mol / liter acetic acid solution, add 1.0 gram of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 2000, P123) and stir to dissolve at room temperature, add polyethylene glycol (molecular weight 10000) to the mixed solution 1.0 g, transferred to an ice-water mixed bath and continued to stir for 5 minutes. Add 7 grams of 1,6-bis(trimethoxysilyl)hexane and 0.1 gram of aluminum isopropoxide to the mixed solution, stir vigorously for 10 minutes, pour the mixed solution into a mold and seal it, and let it stand at room temperature for 1 hour. After taking it out, it was demolded, dried at room temperature, and finally baked at 6000°C for 7 hours. The pore structure of the product is similar to the product of Example 1. The specific texture parameters are: the specific surface area is 835 meters 2 / g, the pore volume is 1.1 cm3 / g, the macropore diameter is 0.4 micron, and the mesopore diameter is 4 nanometers.

Embodiment 3～9

[0019] Synthetic method is identical with embodiment 1, just changes silicon source (bis(triethoxysilyl) methane, 1,4-bis(triethoxysilyl) benzene), aluminum source (aluminum nitrate, aluminum chloride, aluminum sulfate, pseudoboehmite), phase separation inducer R1 (polyoxyethylene, polyethylene oxide) or structure directing agent R2 (long-chain alkyltrimethylammonium halide, citric acid, tartaric acid, malic acid, Lactic acid) type, raw material ratio, gel temperature and other parameters.

[0020] See Table 1 for the specific synthesis conditions and proportions of Examples 3-9. The synthesized product has a composite pore structure similar to that of the product in Example 1, and its specific structural parameters are shown in Table 1.

[0021] Table 1

[0022]

[0023] *Generate SiO according to silicon source theory 2 volume calculation.

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Abstract

The invention relates to a preparation method for mesopore / macropore compound hole structure silica gel and silicon and aluminum oxide material, which mainly solves the problems of high gel temperature and long ageing time when the mesopore / macropore compound hole structure silica gel and silicon and aluminum oxide material is prepared in the prior art. The preparation method comprises the following steps: mixing phase separation inducer R1, structure-directing agent R2, acid catalyst and water; adding an organic silicon source or the mixture of the organic silicon source and an aluminum source to carry out full hydrolysis reaction at the temperature of 0-30DEG C, wherein the mass ratio of the mixture is as follows: R1 / SiO2 is equal to 0.3-1.0, R2 / SiO2 is equal to 0.3-2.0, H2O / SiO2 is equal to 4-7, H+ / SiO2 is equal to 0.1-0.35, and Al2O3 / SiO2 is equal to 0-0.85; pouring the mixture into a die; gelling the mixture at the room temperature; continuously standing and ageing for 0.1-10hours; demoulding an aged product; drying at the temperature of 20-100DEG C for 1-7 days; and then, after calcining at the temperature of 450-800DEG C for 0.5-24hours, preparing the macropore structure oxide material. The problems can be better solved by the technical scheme. The preparation method can be used for the industrial production of the mesopore / macropore compound hole structure silica gel and silicon and aluminum oxide material.

Description

technical field [0001] The invention relates to a preparation method of silica gel and silicon-aluminum oxide materials with mesoporous / macropore composite pore structure. Background technique [0002] In recent years, the combination of organic molecules and inorganic oxides to synthesize new porous materials with special structures and properties has attracted widespread attention. Composite porous materials composed of mesopores and macropores are also a research hotspot. Comparing with ordinary materials, composite porous materials are beneficial to species transfer and diffusion, so they show broad application prospects in the fields of adsorption, separation and catalysis. Patents CN 101525137A and CN 101723393A respectively report the preparation methods of mesoporous / macroporous composite pore structure silica gel and silicon aluminum oxide materials. The prepared materials all have monolithic macroscopic morphology with high specific surface area and well-develope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12C01B39/00
Inventor 何欣高焕新刘志成李宏旭
Owner CHINA PETROLEUM & CHEM CORP