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Three-dimensional ordered macroporous alumina and preparation method thereof

A macroporous alumina, three-dimensional ordered technology, applied in the direction of alumina/aluminum hydroxide, etc., can solve the problems of low adhesion, collapse of macroporous structure, low mechanical strength, etc., to improve adhesion and good hydrophilicity. Effect

Active Publication Date: 2012-12-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, in the current process of preparing three-dimensional ordered macroporous alumina materials with polymer colloidal crystal templates, the amount of alumina precursors attached to the colloidal crystal templates is low due to the hydrophobic surface of polymer microspheres, which is The pore wall of the material is thinner and the mechanical strength is lower. Therefore, when the template is removed by high-temperature calcination, the large-pore structure will collapse, and the material is easily broken into fine powder.
Whether these powdery materials are used in the field of catalyst carrier or adsorption separation, they will face the problem of excessive resistance when the material passes through the particle bed.

Method used

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  • Three-dimensional ordered macroporous alumina and preparation method thereof
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Synthesis of Monodisperse Polymer Microspheres. Take 135 mL of twice distilled water and add it to a three-neck flask, then place the flask in a water bath and heat it to 75°C. Add 0.1348 g NaHCO 3 , start the stirrer, and start feeding N at the same time 2 , stabilized for 10 minutes to make NaHCO 3 Fully dissolve. Then add 0.0666 g of emulsifier and stabilize for 10 minutes, then add 30.7 mL of styrene (St) monomer and stabilize for 30 minutes. Finally, 0.1368 g of initiator potassium persulfate (KPS) was added. The reaction system was kept at a constant temperature of 75° C., and the stirrer rotated at 300 rpm. After 20 hours of reaction, the reaction was terminated, cooled naturally to room temperature, and the reaction mother liquor was left standing for future use. In this example, monodisperse polystyrene microspheres with a diameter of 240 nm were obtained. The specific test data are shown in Table 1.

[0030]

Embodiment 2~5

[0032] According to the method of Example 1, polystyrene emulsion microspheres with different particle sizes can be synthesized by changing the dosage of each reagent. The specific test data are shown in Table 1.

[0033]

[0034] Table 1 Polystyrene microspheres prepared by styrene emulsion polymerization

[0035] St / mL Emulsifier / mL NaHCO 3 / g KPS / g h 2 O / mL Reaction temperature / ℃ Particle size / nm Example 1 30.7 0.0666* 0.1348 0.1368 230 75 240 Example 2 28.6 0.2345 ＃ 0.1385 0.1323 230 80 65 Example 3 29.4 0.0496* 0.1011 0.1293 230 80 330 Example 4 32.7 0.0278* 0.1334 0.1378 230 75 430 Example 5 35.4 0.0325* 0.1395 0.1386 230 75 780

[0036] ＃ The emulsifier used is sodium lauryl sulfate;

[0037]*The emulsifier used was sodium p-styrenesulfonate.

[0038]

Embodiment 6

[0040] Measure 100 mL of the polystyrene microsphere emulsion obtained in Example 1, add sucrose and concentrated sulfuric acid to the emulsion, and the amount of the two accounts for 5.0wt% and 1.5wt% of the polystyrene microsphere emulsion respectively. After the emulsion was centrifugally settled, the liquid phase was removed, and after drying at 60° C. for 48 hours, a modified polymer microsphere colloidal crystal template with a particle size of 5 mm was obtained, which was named T6.

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Abstract

The present invention discloses three-dimensional ordered macroporous alumina and a preparation method thereof. The three-dimensional ordered macroporous alumina has a macropore diameter of 50-1000 nm, a particle size of 1-50 mm, and a mechanical strength of 80-280 g/mm. The method comprises the following steps: adding a saccharide compound and concentrated sulfuric acid to a monodisperse polymer microsphere emulsion to obtain a modified polymer microsphere colloid crystal template; filling an alumina sol; and then carrying out aging and calcination to obtain the three-dimensional ordered macroporous alumina. With the method of the present invention, an adhesion amount of the alumina precursor can be substantially improved, a mechanical strength of the material is enhanced, and the macroporous material is not easily broken into fine powder when high temperature calcination is performed to remove the template so as to maintain high integrity.

Description

technical field [0001] The invention relates to a three-dimensional ordered macroporous alumina and a preparation method thereof, belonging to the field of inorganic material preparation. Background technique [0002] As crude oil resources become increasingly heavy and inferior, the petroleum processing industry will face more and more processing problems of macromolecular hydrocarbons. Currently, porous alumina is a widely used catalytic support material in the field of hydrogenation catalysis in petrochemical industry. It is well known that the pore structure of the carrier directly affects the activity of the catalyst and the mass transfer efficiency of the heavy oil feedstock in the catalytic system, which in turn determines the performance of the catalyst. Therefore, it is an important subject to prepare a new type of alumina support material with large pores suitable for processing macromolecular hydrocarbons that is conducive to the process of macromolecular diffusi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02
Inventor 杨卫亚王少军沈智奇凌凤香王丽华季洪海郭长友孙万付
Owner CHINA PETROLEUM & CHEM CORP
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