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Process for preparing diesel oil hydrog-refining catalyst using TiO2-SiO2 compound oxide as carrier

A composite oxide and hydrofining technology, which is applied in the direction of physical/chemical process catalysts, catalyst carriers, chemical instruments and methods, etc., can solve the problems of low specific surface area, poor thermal stability, and no obvious increase in the acidity of the carrier surface. Achieve the effects of easy vulcanization, good thermal stability and crystal form stability, and good diesel hydrotreating activity

Inactive Publication Date: 2006-06-07
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

γ-Al 2 o 3 The content of titanium oxide in the medium is 5-30wt%. The catalyst has a low specific surface area and the surface acidity of the support has not been significantly improved, so the denitrification effect is not obvious.
[0006] WO96 / 14152 and CN1212992A disclose a hydrogenation dearsenization catalyst with titanium dioxide mixed with alumina as a carrier, a carrier and a preparation method thereof. The catalyst has high low-temperature dearsenic activity and low content of active components, and can meet the requirements of ethylene cracking feedstock oil. The need for arsenic removal, but due to the poor thermal stability and higher Lewis acid and lower Brnsted acid brought about by its carrier mechanical compounding, it cannot be used for hydrogenation of heavier petroleum distillates
[0007] When the existing diesel refining catalysts supported by alumina or modified alumina are used for hydrogenation reaction, it is difficult to have good hydrodesulfurization, denitrogenation and dearomatization performance at the same time, so a single catalyst cannot realize the performance of diesel oil. deep refinement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of TiO by Sol-Gel Method 2 -SiO 2 Complex oxide carrier

[0017] Dissolve the metered tetrabutyl titanate and ethyl orthosilicate in ethanol respectively, and then mix them uniformly to obtain solution A; mix a certain amount of water, acetic acid and anhydrous ethanol to obtain solution B; under strong stirring conditions, mix the solution B is dropped into A for the reaction; after a certain time of reaction, a sol is obtained, and the sol is aged under natural conditions for a certain period of time to obtain TiO 2 -SiO 2 gel. Gel by CO 2 Supercritical drying to obtain white TiO 2 -SiO 2 Ultrafine powder, the powder is calcined at 500 ℃ in an air atmosphere and then pressed into a tablet, and the particles with a particle size of 3-3.6 mm are ground and used as the carrier for preparing the catalyst. The optimized molar ratio of raw materials in the above-mentioned sol preparation process is: (butyl titanate+ethyl orthosilicate): ethanol: water: ac...

Embodiment 2

[0020] Preparation of TiO by Particle Hydrolysis Coating 2 / SiO 2 Complex oxide carrier

[0021] At room temperature, silica gel particles with a particle size of 1.3-2.7 mm were immersed in butyl titanate solution for 2 hours, dried at 120 °C for 2 hours, and then calcined at 500 °C for 2 hours in an air atmosphere to obtain coated TiO 2 / SiO 2 Complex oxide carrier. The amount of titanium dioxide coated by the silica gel particles can be controlled by repeating the above coating process. The optimized coated TiO of the present invention 2 / SiO 2 The composite oxide carrier is preferably coated three times. Table 2 is the specific surface and pore volume data of carriers with different coating times.

[0022] sample

[0023] Secondary coating of TiO 2 / SiO 2

Embodiment 3

[0025] Preparation of TiO by Mixed Sol Method 2 -SiO 2 Complex oxide carrier

[0026] 8~20g Ti (SO 4 ) 2 Dissolve in 20~60ml of water to obtain solution A, mix 20g of NH 4 HCO 3 Dissolve in 100-200ml of water to obtain solution B, add solution B dropwise to solution A under stirring conditions for hydrolysis to obtain TiO 2 sol, then add 3-25ml of silica sol, stir the mixed sol for 1 h, wash with distilled water repeatedly until no sulfate radicals are detected (BaCl 2 method), dry at 120°C for 2h, or replace the water with ethanol at 40°C, 12.0MPa CO 2 The mixed sol-type TiO was obtained by drying for 2 h under supercritical conditions, and then calcining at 500 °C for 2 h in an air atmosphere. 2 -SiO 2 Complex oxide carrier. Table 2 is the TiO prepared by the mixed sol method 2 -SiO 2 Basic properties of complex oxide supports.

[0027] TiO 2 -SiO 2 complex oxide

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PUM

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Abstract

The diesel oil hydrorefining catalyst has composite oxide TiO2-SiO2 as carrier and active metal Co, Mo or Ni, and W components. The catalyst carrier is prepared through sol-gel process, granular hydrolyzing and coating process, or mixed sol process. The active metal components are supported onto the carrier through co-dipping or stepped dipping process. The composite TiO2-SiO2 hydrorefining catalyst has average pore diameter of 7-15 nm and pore volume of 0.2-0.7 ml / g, specific surface area of 100-300 sq m / g. The catalyst of the present invention has relatively high hydrodesulfurizing activity and dydrodenitrifying activity on different kinds of material.

Description

technical field [0001] The present invention relates to a kind of TiO 2 -SiO 2 The invention discloses a preparation method of a diesel hydrorefining catalyst with a composite oxide as a carrier. technical background [0002] At present, most of the diesel hydrofining catalysts used at home and abroad use alumina as the carrier and cobalt, molybdenum, nickel and tungsten as the active components. In recent years, in order to improve the performance of hydrogenation catalysts, some work has been carried out in the aspects of carrier modification, adoption of new materials and preparation methods. [0003] In the method for hydrotreating petroleum hydrocarbons proposed in USP4880524, a hydrogenation catalyst with high activity is used. The catalyst belongs to Ni-Mo / Al 2 O 3 It is prepared by gelation method, that is, water-soluble acidic aluminum salt is titrated with water-soluble alkali metal aluminide to form a hydrogel precipitate, ageing under certain conditions, was...

Claims

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Application Information

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IPC IPC(8): C10G45/08B01J32/00
Inventor 孙发民周亚松王甫村李颖冯秀芳张绍金葛冬梅袁大辉于静梁景程姚彤王忠德
Owner PETROCHINA CO LTD
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