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Macroporous alumina and preparation method thereof

A macroporous alumina, pore size technology, used in alumina/hydroxide preparation, chemical instruments and methods, alumina/aluminum hydroxide, etc., can solve unfavorable catalytic applications, decrease in porosity of carrier materials, and decrease in mechanical strength And other issues

Active Publication Date: 2022-07-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is based on the content of polyethylene glycol to control the formation and pore size of macropores. Although macropores of 50nm-10000nm can be obtained, it has the following disadvantages: (1) It is easier to generate macropores larger than 1 μm, However, it is difficult to control the macropores smaller than 1 μm, and the macropores obtained in the actual preparation of the examples are all macropores above 1 μm; (2) The obtained macropores are apparently isolated and have poor spatial continuity, which is not conducive to the transmission of macromolecules. (3) The obtained material forms amorphous macroporous alumina at a lower calcination temperature (550-650°C), and this amorphous alumina material is not conducive to catalytic applications
If the macropore diameter in the catalyst is too large and the content is too large, the overall porosity of the carrier material will decrease, and the mechanical strength will also seriously decrease

Method used

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  • Macroporous alumina and preparation method thereof
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Examples

Experimental program
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Embodiment 1

[0033]At room temperature (about 25°C), water, anhydrous ethanol, aluminum chloride, polyethylene glycol, ultra-fine monodisperse SB powder (average particle size 10nm), and formamide are mixed uniformly, and then pyridine is added. By weight, the contents are: water 24%, ethanol 20%, aluminum chloride 19%, polyethylene glycol (viscosity average molecular weight 1 million) 0.3%, ultrafine SB powder 3%, formamide 1%, pyridine 32.7% . After mixing uniformly, the obtained gel was aged at 40°C for 48 hours, and then the aged mixture was soaked in a 55 wt% ethanol aqueous solution for 48 hours. After the soaking was completed and the liquid phase was removed, the gel was dried at 40°C until the product no longer appeared obvious. of weight loss. It was then calcined at 550°C for 3 hours and then cooled to room temperature to obtain the macroporous alumina. The XRD test shows that the sample is in a highly crystalline γ state, the total porosity is 76%, the macropores are uniforml...

Embodiment 2

[0035] At room temperature (about 25°C), water, anhydrous ethanol, aluminum chloride, polyethylene glycol, ultra-fine monodisperse SB powder (average particle size: 7nm), and acetamide were mixed uniformly, and then propylene oxide was added. By weight, the contents are: water 25%, ethanol 20%, aluminum chloride 22%, polyethylene glycol (viscosity average molecular weight 1 million) 0.5%, ultrafine SB powder (average particle size 10 nm) 1% , formamide 1.0%, propylene oxide 30.5%. After mixing uniformly, the obtained gel was aged at 40° C. for 48 hours, and then the aged mixture was soaked in ethanol for 48 hours. After soaking and removal of the liquid phase, drying was carried out at 40° C. until the product no longer lost significant weight. It was then calcined at 650°C for 5 hours and then cooled to room temperature to obtain the macroporous alumina. The XRD test shows that it has a good γ crystal state, the total porosity is 76%, the macropore distribution is uniform, a...

Embodiment 3

[0037] At room temperature (about 25°C), water, anhydrous ethanol, aluminum chloride, polyethylene glycol, ultra-fine monodisperse SB powder (average particle size 5nm), and N,N-dimethylformamide are mixed uniformly, and then added Pyridine, each component of the mixture is by weight, the contents are: water 22%, ethanol 20%, aluminum chloride 20%, polyethylene glycol (viscosity average molecular weight 1 million) 0.5%, ultrafine SB powder (average particle size 10 nm) 8%, formamide 2.5%, pyridine 27.0%. After mixing uniformly, the obtained gel was aged at 40°C for 48 hours, and then the aged mixture was soaked with 80 wt% ethanol aqueous solution for 72 hours. Lose weight. It was then calcined at 700°C for 3 hours and then cooled to room temperature to obtain the macroporous alumina. The XRD test shows that it has a good γ crystal state, the total porosity is 79%, the macropore distribution is uniform, and it has three-dimensional space connectivity. The size ratio is 3.4,...

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Abstract

The invention discloses a macroporous alumina and a preparation method thereof. The macroporous alumina of the present invention has the following properties: the macroporous alumina is in a γ crystal state, the total porosity is 60%-85%, the macropore diameter is 50nm-1000nm, and the ratio of the macropores to the total porosity is 40%-85%, preferably 50%-75%; macropores are evenly distributed and three-dimensionally through; the ratio of macropore wall thickness to aperture size is 3-10; lateral crushing strength is 10-35N / mm. In the present invention, macroporous alumina is prepared by sol-gel reaction of inorganic aluminum salts. The alumina macropores have three-dimensional permeability and high mechanical strength of the material, which can meet the strength requirements of the existing heterogeneous catalytic reaction, and can be used as a catalyst. carrier usage.

Description

technical field [0001] The invention relates to a macroporous alumina and a preparation method thereof, belonging to the field of inorganic material preparation. Background technique [0002] Activated Alumina Alumina, as a good hydrogenation catalyst carrier material, has a wide range of applications in the oil refining industry. In practical industrial catalysis applications, in addition to reactive pores of appropriate size (5 nm -20 nm), some large pores (above 100 nm) are also required as efficient macromolecular mass transfer channels. [0003] Acta Phys. Chem., 2005, 21 (02): 221-224., using aluminum nitrate as precursor, ethanol as solvent, formamide as drying control chemical additive, and propylene oxide as gel network inducer, through sol-gel Alumina gel was prepared by the method, and light and massive alumina aerogel with concentrated mesopore distribution was obtained under normal pressure drying conditions. However, the mesopores of this aerogel material are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/04B01J20/08B01J20/28C01F7/02C01F7/30C02F1/28C02F1/00
CPCB01J21/04B01J20/08B01J20/28085C01F7/02C02F1/281C02F1/00B01J2220/4806Y02P20/52
Inventor 杨卫亚凌凤香张会成王少军沈智奇
Owner CHINA PETROLEUM & CHEM CORP