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Preparation method of titanium-aluminum composite oxide with large specific surface and small aperture

A composite oxide and large specific surface technology, applied in chemical instruments and methods, chemical/physical processes, catalyst carriers, etc., can solve problems such as high production costs, unsuitable for industrial scale-up, organic ammonia nitrogen pollution, etc., and achieve easy control, Effect of reducing activation energy and improving hydrodesulfurization performance

Active Publication Date: 2015-04-01
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method can prepare TiO with partial titanium oxide composition 2 -Al 2 o 3 Composite support, the specific surface area and pore size are larger than that of TiO alone 2 It needs to be large, but the preparation of raw materials requires the use of expensive organic titanium sources or organic alkali sources, the production cost is high, it is not suitable for industrial scale-up, and there is a problem of organic ammonia nitrogen pollution

Method used

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  • Preparation method of titanium-aluminum composite oxide with large specific surface and small aperture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolving the mixed solution (TiO 2 Concentration is 20%, Al 2 o 3 Concentration is 30%) solution, 6.3g sodium perfluorononenylbenzene sulfonate, after stirring evenly, solution A is obtained. Prepare 5kg of sodium hydroxide solution (concentration is 15%), stir evenly to obtain solution B.

[0031] Slowly add solution B to solution A at 40°C and 320rpm stirring. After gelation, control the end point pH to 5, stir for 1 hour, age at 90°C for 3 hours, and wash with deionized water until neutral. The obtained filter cake was directly dried at 120° C. for 3 hours. Using a heating rate of 10° C. / min, holding at 200° C. for 2 hours and at 600° C. for 2 hours to obtain titanium-aluminum composite oxide powder. Powdered TiO 2 / Al 2 o 3 The ratio and pore structure data are listed in Table 1.

Embodiment 2

[0033] Dissolving the mixed solution (TiO 2 Concentration is 20%, Al 2 o 3 Concentration is 30%) solution, obtain solution A after stirring evenly. Prepare 5kg of sodium hydroxide solution (concentration is 15%), stir evenly to obtain solution B.

[0034] Slowly add solution B to solution A at 40°C and 320rpm stirring, control the end point pH value to 5 after gelation, stir for 1 hour after neutralization, add ammonia water to adjust the pH of the solution to 9,90°C Aged for 3 hours, washed with deionized water until neutral. The obtained filter cake is beaten and then spray-dried, the inlet temperature is controlled at 220°C, and the feed rate is adjusted so that the outlet temperature is maintained at about 100°C. Using a heating rate of 10° C. / min, holding at 200° C. for 2 hours and at 600° C. for 2 hours to obtain titanium-aluminum composite oxide powder. Powdered TiO 2 / Al 2 o 3 The ratio and pore structure data are listed in Table 1.

Embodiment 3

[0036] Dissolving the mixed solution (TiO2) of 6.5kg titanyl sulfate and aluminum sulfate 2 The content is 1.5%, Al 2 o 3 Concentration is 30%), 10.5g sodium perfluorononenylbenzene sulfonate, after stirring evenly, solution A is obtained. Prepare 13kg of sodium hydroxide solution (concentration is 15%), stir evenly to obtain solution B.

[0037] Slowly add solution B to solution A at 40°C and 320rpm stirring. After gelation, control the end point pH to 5, age at 90°C for 3 hours, and wash with deionized water until neutral. The obtained filter cake was directly dried at 120° C. for 3 hours. Using a heating rate of 10° C. / min, holding at 200° C. for 2 hours and at 600° C. for 2 hours to obtain titanium-aluminum composite oxide powder. Powdered TiO 2 / Al 2 o 3 The ratio and pore structure data are listed in Table 1.

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Abstract

The invention relates to a preparation method of a titanium-aluminum composite oxide with large specific surface and small aperture. The method comprises the following steps: 1, uniformly mixing an inorganic titanium source with an acidic aluminum source, a surfactant and deionized water to obtain a solution A, and uniformly mixing an inorganic alkali source with deionized water to obtain a solution B; 2, pouring the solution A into a gel formation tank, heating to 20-60DEG C, adding the solution B into the gel formation tank under a certain flow, and controlling the pH value at the neutralization end point by adjusting the amount of the solution A and / or B; 3, reacting under stirring at a temperature controlled in step 2 for 0.5-3h; 4, adding a suitable concentration of the inorganic alkali source into the solution obtained in step 3, adjusting the pH value of the obtained system to a certain range, and ageing at 30-120DEG C for 2-8h; 5, carrying out solid-liquid separation on the solution obtained in step 4, and washing with water until neutrality; and 6, respectively carrying out spray drying and segmented roasting on the composite oxide obtained in step 5 to obtain titanium-aluminum composite oxide powder.

Description

Technical field: [0001] The invention relates to the field of preparation of catalysts and supports, and relates to a preparation method of titanium-aluminum composite oxide with large specific surface and small aperture. The invention aims to provide a green and environment-friendly catalyst carrier with small pore diameter, large specific surface, adjustable pore volume and titanium-aluminum ratio, simple preparation process, and low cost. The titanium-aluminum composite oxide of the invention is used as a carrier in the deep hydrotreating desulfurization catalyst of diesel oil, and has excellent desulfurization and denitrogenation performances. Background of the invention: [0002] The support has an important influence on the performance of supported catalysts. When the same catalytic reaction uses the same active components but uses different supports, the catalyst activity and product composition will also vary greatly. At present, most of the supports used in indust...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J35/10B01J21/06
Inventor 于海斌周鹏孙彦民谢献娜李晓云张永惠马月谦曾贤君隋云乐
Owner CNOOC TIANJIN CHEM RES & DESIGN INST