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A kind of macroporous alumina with dual pore distribution and preparation method thereof

A technology of macroporous alumina and double pores, applied in chemical instruments and methods, alumina/aluminum hydroxide, catalyst supports, etc., can solve the problems of carrier material porosity decrease, unfavorable macromolecular mass transfer, poor spatial continuity, etc. , to achieve the effect of reducing the degree of solid-liquid phase separation, improving mechanical strength and maintaining integrity

Active Publication Date: 2020-02-14
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 50-10000nm 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. quality
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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  • A kind of macroporous alumina with dual pore distribution and preparation method thereof
  • A kind of macroporous alumina with dual pore distribution and preparation method thereof
  • A kind of macroporous alumina with dual pore distribution and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0036] At room temperature (20°C), mix water, absolute ethanol, aluminum chloride, polyethylene glycol, and formamide evenly, and then add pyridine. The contents of each component of the mixture are by weight: water 23%, ethanol 22% , aluminum chloride 20%, polyethylene glycol (viscosity average molecular weight 1 million) 0.3%, formamide 1%, pyridine 33.7%. After mixing evenly, the obtained gel is aged at 45°C for 48 hours, and then soaked in a mixture of ethanol and water for 48 hours. After soaking and removing the liquid phase, dry it at 40°C until the product no longer occurs. Visible weight loss. Then it was calcined at 550°C for 7 hours, and then cooled to room temperature to obtain the macroporous alumina. The total porosity is 81%, and the pores have a double pore distribution. Among them, the macropores are evenly distributed, the average pore size of the macropores is 400nm, and the macropore porosity accounts for 60%; the mesopore diameter is 4~6nm, and the mesopo...

Embodiment 2

[0038] At room temperature (20°C), mix water, absolute ethanol, aluminum chloride, polyethylene glycol, and formamide evenly, and then add pyridine. The contents of each component of the mixture are by weight: water 31%, ethanol 29% , aluminum chloride 16%, polyethylene glycol (viscosity average molecular weight 2 million) 0.5%, formamide 3.5%, pyridine 20%. After mixing evenly, the obtained gel was aged at 60°C for 24 hours, and then soaked in ethanol for 48 hours. After soaking and removing the liquid phase, it was dried at 50°C until the product no longer lost weight. Then bake at 650° C. for 5 hours, and then cool to room temperature to obtain the macroporous alumina of the present invention. The total porosity is 75%, and the pores have a double pore distribution. Among them, the macropores are evenly distributed. The average pore size of the macropores is 207nm, and the macropore porosity accounts for 43%. The mesopore diameter is 9~12nm, and the mesopore porosity accoun...

Embodiment 3

[0040] At room temperature (20°C), mix water, absolute ethanol, aluminum sulfate, polyethylene glycol, and N,N-dimethylformamide evenly, and then add pyridine. The contents of each component of the mixture are, by weight, water 48%, ethanol 38%, aluminum chloride 10%, polyethylene glycol (viscosity average molecular weight 300,000) 0.78%, N,N-dimethylformamide 3.22%, pyridine 10%. After mixing evenly, the obtained gel product is aged at 80°C for 24 hours, and then soaked in ethanol for 48 hours. After soaking and removing the liquid phase, dry it at 50°C until the product no longer loses weight . Then calcined at 850°C for 5 hours, and then cooled to room temperature to obtain macroporous alumina. The total porosity is 67%, and the pores have a double pore distribution. Among them, the macropores are evenly distributed. The average pore size of the macropores is 709nm, and the macropore porosity accounts for 43%. The mesopore diameter is 14~20nm, and the mesopore porosity acc...

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Abstract

The invention discloses a macroporous alumina with dual pore distribution and a preparation method thereof. The macroporous alumina of the present invention has high porosity, in which the porosity proportion of 5 to 20 nm pores is 15% to 55%, and the porosity proportion of 100 to 1000 nm macropores is 40% to 75%. The macropores are evenly distributed and three-dimensionally connected. The method is to thoroughly mix aluminum source, polyethylene glycol, organic matter containing amide groups and selected low-carbon alcohol aqueous solution, add pyridine into the mixture, and then undergo aging, soaking, drying and roasting to obtain macroporous alumina. The method of the invention can meet the existing heterogeneous catalytic strength requirements and is suitable as a good carrier for the catalyst.

Description

technical field [0001] The invention relates to a macroporous alumina and a preparation method thereof, in particular to a macroporous alumina with double pore distribution and a preparation method thereof, belonging to the field of inorganic material preparation. Background technique [0002] Activated alumina As a good hydrogenation catalyst support material, alumina has been widely used in the oil refining industry. In actual industrial catalytic applications, in addition to reactive pores of appropriate size (5-20nm), some large pores (above 100nm) are required as efficient macromolecular mass transfer pores. [0003] Acta Physicochemical Sinica, 2005, 21 (02): 221-224., with aluminum nitrate as precursor, ethanol as solvent, formamide as drying control chemical additive, pyridine as gel network inducer, prepared by sol-gel method Alumina gel, light, massive alumina airgel with concentrated mesoporous distribution can be obtained under normal pressure and drying conditi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/02B01J21/04B01J35/10B01J32/00
CPCC01F7/02B01J21/04C01P2004/03C01P2006/17C01P2006/16C01P2006/14C01P2006/12B01J35/617B01J35/638B01J35/651B01J35/635B01J35/615B01J35/647
Inventor 杨卫亚凌凤香沈智奇郭长友季洪海王丽华王少军张会成
Owner CHINA PETROLEUM & CHEM CORP