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A method for preparing modified alumina carrier by using water-reactive halide

A technology of alumina carrier and alumina, which is applied in the direction of catalyst carrier, chemical instruments and methods, silicon compounds, etc., can solve the problems of complicated mechanism of action, difficulty in large-scale industrial production, destruction, etc., and achieve low cost and easy large-scale The effect of popularization and application and simple operation process

Active Publication Date: 2016-05-11
FUZHOU UNIV
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Problems solved by technology

[0003] The pore size distribution adjustment in the carrier synthesis and molding stages is mainly realized by adjusting the size and packing mode of the pore-forming particles. The pore size distribution can be adjusted by adding suitable templates and / or adjusting suitable preparation conditions, but these methods have Its shortcomings cannot be ignored, such as high synthesis cost, serious pollution of template agent, and it is not easy to realize large-scale industrial production.
The pore size distribution of the formed carrier can be adjusted by appropriate chemical treatment (acid treatment, alkali treatment, water vapor treatment, etc.), hydrothermal treatment and other post-treatment methods, but these methods will cause certain damage to the structure of the carrier itself. Such as the reduction of crushing strength, etc., and there are problems to be solved urgently such as the generation of a large amount of waste water, the complex mechanism of action, and the difficulty in realizing industrialization (D.L.Trimm, et al., Appliedcatalysis, 1986, 21(2), 215-238.)
[0004] Water-reactive halides can react with water and / or hydroxyl groups to form corresponding oxides (or hydroxides). The chemical vapor deposition reaction of water vapor and water-reactive halides has been used to modify porous membrane materials, and certain achievements have been made. Progress (M.Niwa, et al., Journal of Physics and Chemistry of Solids, 1989,50(5):487-496.), but this method usually needs to be carried out under vacuum conditions, and there are problems such as difficult control of the amount of water vapor, which is difficult Realize controllable modulation of pore structure properties and surface properties of porous supports
Some progress has been made in surface modification of porous supports by using high-temperature reactions (higher than 300°C) between water-reactive halides and porous supports such as molecular sieves (M.W.Anderson, et al., Zeolites, 1986, 6 (6 ):455-466.), but the reaction at high temperature will lead to serious damage to the framework of the porous support, such as dealumination, etc., it is difficult to achieve controllable modulation of the pore structure and surface properties of the porous support
Utilize the reaction of water generated during the roasting process of water-reactive halides (silicon tetrachloride, titanium tetrachloride, etc.) A method to simultaneously realize the modulation of the pore size distribution and surface properties of porous alumina supports has not been reported

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  • A method for preparing modified alumina carrier by using water-reactive halide

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Embodiment 1

[0028] Example 1: Fill 0.5kg of pseudo-boehmite (produced by Aluminum Corporation of China Shandong Branch, P-DF-03, ignition loss ≤ 24%) in a glass-lined fixed-bed reactor, and use dry nitrogen at 40°C Under purge for 0.2h, the space velocity of nitrogen is 300h -1 ; With dry nitrogen as the purge gas, the reactor pressure is 0.1MPa (absolute pressure), the fixed bed reactor is heated at a rate of 2°C / min, and when the reactor temperature rises to 50°C, nitrogen is used to bubble The method carries water-reactive halide silicon tetrachloride to interact with pseudoboehmite, the temperature of the bubbler is 35°C, and the space velocity of nitrogen is 300h -1 ; when the reactor temperature rises to 120°C, switch to dry nitrogen for purging; when the reactor temperature rises to 450°C, stop heating up, and after roasting at 450°C for 5 hours, cool to room temperature to obtain a concentrated pore size distribution The porous alumina carrier, its pore structure parameters are s...

Embodiment 2

[0029] Example 2: Fill 0.5kg boehmite (manufactured by Zibo Baida Chemical Co., Ltd., BD-BS03, alumina content ≥ 83%) into a glass-lined fixed-bed reactor, blow with dry nitrogen at 35°C Sweep for 0.5h, the space velocity of nitrogen is 400h -1 ; With dry nitrogen as the purge gas, the reactor pressure is 0.12MPa (absolute pressure), the fixed bed reactor is heated at a rate of 4°C / min, and when the reactor temperature rises to 60°C, nitrogen bubbles are used The method carries the water-reactive halide titanium tetrachloride to interact with boehmite, the temperature of the bubbler is 35 ℃, and the space velocity of nitrogen is 400h -1 ; When the reactor temperature rises to 130°C, switch to dry nitrogen for purging; when the reactor temperature rises to 550°C, stop heating up, and after roasting at 350°C for 8 hours, cool to room temperature to obtain a concentrated pore size distribution The porous alumina carrier, its pore structure parameters are shown in Table 1.

Embodiment 3

[0030] Example 3: Pack 0.5kg of boehmite (manufactured by Zibo Baida Chemical Co., Ltd., BD-BS03, with alumina content ≥ 83%) in a glass-lined fixed-bed reactor, and purge with dry nitrogen at 40°C 0.5h, the space velocity of nitrogen is 300h -1 ; With dry nitrogen as the purge gas, the reactor pressure is 0.15MPa (absolute pressure), the fixed bed reactor is heated at a rate of 10°C / min, and when the reactor temperature rises to 50°C, nitrogen is used to bubble The way to carry the water-reactive halide tin tetrachloride to interact with boehmite, the temperature of the bubbler is 50 ℃, and the space velocity of nitrogen is 600h -1 ; when the reactor temperature rises to 150°C, switch to dry nitrogen for purging; when the reactor temperature rises to 550°C, stop heating, and after roasting at 550°C for 4 hours, cool to room temperature to obtain a concentrated pore size distribution The porous alumina carrier, its pore structure parameters are shown in Table 1.

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Abstract

The invention discloses a method for preparing modified aluminum oxide by treating pseudo-boehmite through a water-reactive halide. The method comprises the following steps: in the temperature-programmed calcination process of the pseudo-boehmite, introducing 0.1-30 percent by volume of the water-reactive halide by adopting an inert gas bubbling way for reacting with water produced during calcination of the pseudo-boehmite; and drying and sintering a reaction product to prepare the modified aluminium oxide which is controllable in the pore diameter distribution and surface property. The method disclosed by the invention is simple in process, is low in cost, meets the practical production requirements, and has a wide application prospect in the field of material preparation. By adopting the method, controllable modulation of the pore diameter distribution and the surface property of the aluminum oxide can be realized at the same time.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing modified alumina with concentrated pore size distribution by utilizing water-reactive halides. Background technique [0002] Porous supports are widely used in high-tech fields such as adsorption, catalysis, separation and microelectronics. The pore size distribution of the porous carrier is a key factor affecting the diffusion of the medium in the pores. In the field of catalytic materials, it has an important impact on the activity, selectivity and thermal stability of the catalyst, and also has an important impact on the separation performance of separation materials such as adsorbents. Therefore, developing an efficient, stable, and simple method for regulating the pore size distribution is a core challenge in this field. [0003] The pore size distribution adjustment in the carrier synthesis and molding stages is mainly realiz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J32/00B01J21/12B01J21/06B01J23/14B01J20/08B01J20/10
Inventor 陈晓晖许承志肖益鸿魏可镁
Owner FUZHOU UNIV