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Synthesis method of mesoporous TiO2-Al2O3 composite carrier

A technology of tio2-al2o3, synthesis method, applied in catalyst carriers, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as insufficient uniformity, and achieve the effects of uniform distribution, high specific surface area, and narrow pore size distribution

Active Publication Date: 2015-04-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, because the hydrolysis speeds of organic titanium salts and organic aluminum salts are very different, titanium alkoxides with fast hydrolysis speeds will inevitably undergo titanium aggregation after hydrolysis, and the ratio of titanium oxide phase and aluminum oxide phase in the resulting composite support Separation is still relatively obvious, not uniform enough

Method used

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  • Synthesis method of mesoporous TiO2-Al2O3 composite carrier
  • Synthesis method of mesoporous TiO2-Al2O3 composite carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At room temperature, under magnetic stirring conditions, 54 g of aluminum sec-butoxide was mixed with 300 mL of benzyl alcohol solvent. After stirring for 20 minutes, add 63 g of titanium isopropoxide; stir for 20 minutes, add 160 mL of oleylamine, and stir for 4 hours. Transfer the solution to a static reaction kettle, seal it tightly, and place it in a dry box. The temperature of the drying oven was set at 180° C., and after 24 hours of constant temperature, it was taken out and cooled naturally. The prepared solution was washed with absolute ethanol and centrifuged three times, and the collected solid powder was dried in a drying oven at 70° C. for 24 hours. Part of the solid powder was dispersed in absolute ethanol for high-resolution observation. Then, the temperature was raised to 500° C. at a rate of 3° C. / min in an air atmosphere, and then calcined at a constant temperature for 6 hours to obtain a Ti-Al composite oxide carrier A.

Embodiment 2

[0031] At room temperature, under the condition of magnetic stirring, 73g of aluminum sec-butoxide was mixed with 300mL of benzyl alcohol solvent. After stirring for 20 minutes, add 42 g of titanium isopropoxide; stir for 20 minutes, add 160 mL of oleylamine, and stir for 3 hours. Transfer the solution to a static reaction kettle, seal it tightly, and place it in a dry box. The temperature of the drying oven was set at 180° C., and after 16 hours of constant temperature, it was taken out and cooled naturally. The prepared solution was washed with absolute ethanol and centrifuged three times, and the collected solid powder was dried in a drying oven at 70° C. for more than 24 hours. Part of the solid powder was dispersed in absolute ethanol for high-resolution observation. Then, the temperature was raised to 500° C. at a rate of 3° C. / min in an air atmosphere, and then calcined at a constant temperature for 6 hours to obtain a Ti-Al composite oxide carrier B.

Embodiment 3

[0033] At room temperature, under the condition of magnetic stirring, 194g of aluminum sec-butoxide was mixed with 300mL of benzyl alcohol solvent. After stirring for 20 minutes, add 28 g of titanium isopropoxide; stir for 20 minutes, add 160 mL of oleylamine, and stir for 4 hours. Transfer the solution to a static reaction kettle, seal it tightly, and place it in a dry box. The temperature of the drying oven was set at 200° C., and after 12 hours of constant temperature, it was taken out and cooled naturally. The prepared solution was washed with absolute ethanol and centrifuged three times, and the collected solid powder was dried in a drying oven at 70° C. for more than 24 hours. Part of the solid powder was dispersed in absolute ethanol for high-resolution observation. Then, the temperature was raised to 500° C. at a rate of 3° C. / min in an air atmosphere, and then calcined at a constant temperature for 6 hours to obtain a Ti-Al composite oxide carrier C.

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Abstract

The invention discloses a synthesis method of a mesoporous TiO2-Al2O3 composite carrier. The method consists of: employing a solvothermal method to dissolve a titanium oxide precursor and an alumina precursor in an organic solvent, and under the action of a protective agent, performing an etherification reaction in a high temperature static reaction kettle, mixing the molecules of titanium oxide and alumina mutually to form a monomolecular layer compound, and carrying out roasting at 400DEG C-600DEG C to form a TiO2-Al2O3 composite oxide. The method provided in the invention uses a solvothermal process to synthesize the TiO2-Al2O3 composite carrier with a specific and novel layer structure for the first time. The composite carrier can be used as the carrier of a hydrofining catalyst, and is especially suitable to be used as the carrier of a heavy oil hydrodesulfurization catalyst.

Description

technical field [0001] The present invention relates to a kind of TiO 2 ·Al 2 o 3 The preparation method of the composite carrier is mainly used for the preparation method of the carrier in the hydrogenation refining catalyst. Background technique [0002] Heavy crude oil and strict quality requirements for petroleum products will be the problems that the petrochemical industry has been facing. Only continuous innovation in hydrotreating technology can meet the needs of market and social development. The improvement of the hydrofining process depends on the application of high-activity catalysts. In order to improve the activity of the catalysts, a lot of work has been done on the modification of the catalyst's alumina carrier in recent years. [0003] Using alumina-titania composite oxide as a carrier, the desulfurization ability of the original catalyst is significantly increased because the active phase interacts with titania to increase the number of active centers. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J32/00B01J35/10B01J21/06C10G45/04
Inventor 郭长友沈智奇凌凤香王少军杨卫亚季洪海王丽华
Owner CHINA PETROLEUM & CHEM CORP