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Three-dimensional ordered macroporous alumina and preparation method thereof

A macroporous alumina, three-dimensional ordered technology, applied in chemical instruments and methods, alumina/aluminum hydroxide, and other chemical processes, can solve the problems of uneven particle size of alumina, material specific surface area loss, and control difficulties and other problems, to achieve the effect of improving activity and selectivity, improving mass transfer capacity, and high specific surface area

Active Publication Date: 2011-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the aluminum oxide precursor, aluminum nitrate, has undergone a sol process in this method, the hydrolysis-polymerization process of the aluminum oxide precursor is rapid and difficult to control.
Therefore, in this method, the size of the alumina microscopic particles obtained through the hydrolysis-polymerization process of aluminum nitrate using ammonia as a catalyst is also uneven, and the formed larger inter-particle gaps will cause the loss of the specific surface area of ​​the material.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthesis of Monodisperse Polymer Microspheres. Get an appropriate amount of twice-distilled water and heat it to boil for 10 minutes to reduce the dissolved oxygen content in the water. After natural cooling of distilled water, 135 mL was added to a three-necked flask, and then the flask was placed in a water bath and heated to 75°C. Add 0.1011 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. Add 0.0496 g of sodium p-styrene sulfonate (NaSS) and stabilize for 10 minutes, then add 29.4 mL of styrene monomer (St) and stabilize for 30 minutes. Finally, the 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 reacting for 20 hours, it was observed that there were basically no oil droplets on the wall of the three-necked flask. It can be considered that the conversion of styrene monomer ...

Embodiment 2～5

[0032] According to the method of Example 1, polystyrene emulsion particles with different particle sizes can be synthesized by changing the dosage of each reagent. The test results are shown in Table 1. figure 1 The SEM image of the polystyrene colloidal crystal template with a particle size of 240 nm prepared for Example 3 of the present invention shows a wide range of (111) planes in the crystal face-centered cubic structure.

[0033] Table 1 Polystyrene microspheres synthesized by styrene-free emulsion polymerization

[0034]

[0035] *The emulsifier used in this example is sodium dodecyl sulfate

Embodiment 6

[0037] Assembly of polystyrene colloidal microspheres and sintering of templates. Assembled by natural deposition method.

[0038] Measure 150 mL of the polystyrene microsphere emulsion obtained in Example 2, ultrasonically disperse it for 10 minutes, place it in a flat-bottomed sedimentation tank, settle naturally at room temperature, and dry it at room temperature for 3 to 7 days. After the liquid is completely volatilized, the thickness is about 1.5 mm colloidal crystal PS2.

[0039] Heat treatment of colloidal crystals: The colloidal crystals PS2 are slightly sintered at a temperature of 100° C., and the sintering time is 5 minutes. After the sintering treatment, the polymer colloidal crystal template PL2 used for preparing the porous alumina of the present invention is obtained.

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Abstract

The invention provides a three-dimensional ordered macroporous alumina and a preparation method thereof, wherein the method comprises the following steps of: assembling polymer microspheres which are singly dispersed to form a colloidal crystal template, filling the alumina sol which is prepared by means of a special method into the template, and drying and roasting to obtain macroporous alumina. The method provided by the invention has the advantages that the alumina sol and the compounding process of the alumina sol and the polymer microspheres can be controlled well, the network structure of the alumina sol is protected possibly, the alumina which is prepared by means of the method not only has three-dimensional ordered macroporous channels but also has a high specific surface area. Furthermore, the macropores within the material are communicated to the surrounding macropores by means of 12 small window holes, and the window holes are formed by sintering the template properly. The alumina prepared by means of the method provided by the invention is suitable for being used as a catalyst carrier of heavy oil and an adsorption and separation material of organic macromolecule. The alumina prepared by means of the method which is provided by the invention is suitable for improving the mass transfer capability of the material within the catalyst and is suitable for improving the activity and the selectivity of the catalyst during the application process as a catalyst carrier.

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] In recent years, with the increasingly heavy and inferior quality of crude oil resources, the petrochemical industry will face more and more processing problems of macromolecular hydrocarbons. Making full use of heavy oil resources and converting them into light fuels as much as possible is one of the important goals of the current oil refining industry. In addition, due to the continuous improvement of environmental protection regulations, the control of the content of impurities such as sulfur, nitrogen, aromatics and metals in vehicle fuels has become more stringent. Therefore, in order to make full use of heavy oil resources and convert them into clean fuels that meet environmental protection requirements, it is extremely important to use hydrogenation tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02B01J20/08B01J20/30
Inventor 杨卫亚沈智奇凌凤香王丽华季洪海王丽君孙万付
Owner CHINA PETROLEUM & CHEM CORP
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