Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method

A dynamic hydrothermal and mesoporous technology, applied in the preparation of alumina/hydroxide, etc., can solve the problems of high roasting temperature, long time, and easy self-agglomeration of particles, and achieve simple experimental steps, increase the contact area, and prepare short cycle effect

Inactive Publication Date: 2012-07-18
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sol-gel method is not effective in the synthesis of mesoporous γ-Al 2 o 3 There are also deficiencies in the field, for example, when the template is removed, the calcination temperature is too high, the time is too long, the crystallization of the product is not perfect, and the particles are prone to self-agglomeration, etc.
[0006] The crystallization method is a method for preparing high-quality (higher crystallinity and larger specific surface area) crystals, but it belongs to a static preparation method like the above two methods, and this preparation method is not conducive to the reaction between substances. Fully contact and react between them, and the reaction time of the general crystallization method is too long, generally takes 24 to 72 hours
Moreover, the static preparation method is not suitable for large-scale continuous production

Method used

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  • Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method
  • Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method
  • Method for preparing mesoporous gamma-Al2O3 by dynamic hydrothermal method

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specific Embodiment approach 1

[0029] combine figure 1 This embodiment will be described.

[0030] The aqueous solution that is dissolved with 3.75g aluminum nitrate 5.25g urea is added respectively in the cetyl trimethyl ammonium bromide solution (the quality of cetyl trimethyl ammonium bromide 0.1g), its mass ratio is aluminum nitrate : urea: hexadecyltrimethylammonium bromide=1: 1.4: 0.027, continuously stirred for 1h at 30°C to make it uniformly mixed, then the mixed solution was transferred to an autoclave, and distilled water was added in the autoclave, Make its volume 1 / 2 of the volume of the whole inner tank (the volume of the whole inner tank is 300mL); then heat to 170°C and continuously stir for 4h; after the reaction is finished, the reaction product is suction filtered, and washed with distilled water until neutral, Dry at 100°C to constant weight, and bake at 600°C for 4 hours to obtain γ-Al 2 o 3 .

[0031] Carry out XRD detection on the product, detection conditions: application of X-ray...

specific Embodiment approach 2

[0033] combine figure 2 , image 3 To illustrate this embodiment, the aqueous solutions of 3.75g aluminum nitrate and 5.25g urea are added to the cetyltrimethylammonium bromide solution (the quality of cetyltrimethylammonium bromide is 0.05g) , its mass ratio is aluminum nitrate: urea: cetyltrimethylammonium bromide=1: 1.4: 0.0133, continuously stirred for 1h at 30°C, so that it can be uniformly mixed, and then the mixed solution is transferred into an autoclave, And add distilled water in the still, make its volume 1 / 2 of the volume of the whole inner tank (the volume of the whole inner tank is 300mL); then heat to 100 ℃ and continue to stir for 4h; Wash with distilled water until neutral, dry at 100°C to constant weight, and roast at 500°C and 550°C for 4 hours to obtain mesoporous γ-Al 2 o 3 The results are listed in Table 1, and Table 1 shows the properties of mesoporous alumina with different calcination temperatures.

[0034] Table 1

[0035]

[0036] Table 1 sh...

specific Embodiment approach 3

[0039] combine Figure 4 , Figure 5 , Figure 6To illustrate this embodiment, the aqueous solutions of 3.75g aluminum nitrate and 5.25g urea are added to the cetyltrimethylammonium bromide solution (the quality of cetyltrimethylammonium bromide is 0.05g) , its mass ratio is aluminum nitrate: urea: cetyltrimethylammonium bromide=1: 1.4: 0.0133, continuously stirred for 1h at 30°C, so that it can be uniformly mixed, and then the mixed solution is transferred into an autoclave, And add distilled water in the still, make its volume 1 / 2 of the volume of the whole inner tank (the volume of the whole inner tank is 300mL); then heat to 130 ℃ and continue to stir for 4h; after the reaction is finished, the reaction product is suction filtered, And washed with distilled water until neutral, dried at 100°C to constant weight, and calcined at 500°C for 4h to obtain mesoporous γ-Al 2 o 3 .

[0040] The XRD detection conditions of this embodiment are the same as those of Embodiment 1....

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Abstract

The invention relates to a method for preparing mesoporous gamma-Al2O3 by a dynamic hydrothermal method, belonging to the field of preparation of inorganic porous materials. The invention aims to solve the problems that in the prior art, reaction steps are multiple, experimental conditions are difficult to control, products are incompletely crystallized, the reaction time is too long, and a static reaction does not facilitate full contact among reaction materials. The method comprises the following steps of: adding inorganic aluminum salt and a precipitating agent into surfactant solution respectively, and uniformly mixing the inorganic aluminum salt with the precipitating agent; continuously stirring the mixed solution, and performing hydrothermal treatment; and washing and calcinating obtained products after finishing the reaction, and thus obtaining the mesoporous gamma-Al2O3. The method has the advantages that: the reaction is performed more fully, the formation of alumina precursors can be simply controlled, the formation of mesoporous alumina can be effectively controlled, the crystallization time is shortened to be less than 24 hours, the preparation period is short, and the method is suitable for large-scale continuous production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic porous materials, and in particular relates to the preparation of mesoporous γ-Al by a dynamic hydrothermal method 2 o 3 Methods. Background technique [0002] The large specific surface area and regular pore structure of inorganic mesoporous materials make them have high activity and large adsorption capacity. Mesoporous γ-Al 2 o 3 It is one of the important materials. Due to mesoporous γ-Al 2 o 3 It has the advantages of large specific surface area, uniform pore size and stable physical and chemical properties, so it is widely used as a binder in the field of catalyst carriers. [0003] At present, the methods for synthesizing mesoporous alumina are divided into the following types: precipitation method, sol-gel method and crystallization method. [0004] The precipitation method is to add a precipitating agent to the aqueous solution of aluminum-containing metal salts to form cry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/30
Inventor 赵振波赵彬
Owner CHANGCHUN UNIV OF TECH
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