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Macroporous aluminium oxide carrier and preparation method thereof

A technology of alumina carrier and macroporous alumina, which is applied in catalyst carrier, chemical instrument and method, catalyst activation/preparation, etc., can solve the problems of low production efficiency, poor operating conditions for oil column forming, etc. Good pore penetration and the effect of increasing the amount of deposition

Active Publication Date: 2010-11-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, oil column forming has disadvantages such as harsh operating conditions and low production efficiency

Method used

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  • Macroporous aluminium oxide carrier and preparation method thereof
  • Macroporous aluminium oxide carrier and preparation method thereof

Examples

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Effect test

Embodiment 1

[0045] Under stirring conditions, 375g of aluminum nitrate nonahydrate and 90g of urea were mixed and heated to 100°C, and added to a mixture of 32g of polyisobutylene maleate triethanolamine maleate and 88g of 150HVI neutral oil at the same temperature to form supersolubilizing micelles , and then reacted at 100°C for 3 hours to obtain nano-aluminum hydroxide gel. Wash three times with 200ml of distilled water, and dry at 120°C for 10 hours. Mix 70g of nano-aluminum hydroxide gel dry powder with binder pseudo-boehmite 30g; 2.6g dilute nitric acid (mass concentration 17%), 18g water and 1g cosolvent ethanol are mixed uniformly, and then Molding in middle, control pressure at 10MPa. The molded product was dried at 100°C for 10 hours, calcined at 240°C for 3 hours, and then calcined at 850°C for 4 hours with a heating rate of 5°C / min to obtain the alumina carrier A1 of the present invention. Then impregnate A1 with 32 ml of aluminum nitrate aqueous solution with a weight conce...

Embodiment 2

[0047] Mix 90g minus three-line dewaxed oil and 70g SP-80, heat to dissolve at 80°C, and mix well; heat 620g of aluminum nitrate nonahydrate to 80°C to melt, slowly add to the above mixture, and mix for 20 minutes to form a uniform supersolubilized colloid. 220 g of saturated ammonia water at 20° C. was added dropwise and aged for 3 hours to obtain a nano-aluminum hydroxide gel. Wash three times with 200ml of distilled water, and dry at 120°C for 10 hours. Mix 70g of nano-aluminum hydroxide gel dry powder with 30g of binder pseudo-boehmite; 2g of dilute nitric acid (mass concentration 17%), 25g of water and 3g of cosolvent ethanol are mixed and added to the above mixture, and then Molding in extruder, control pressure at 23MPa. The molded product was dried at 100°C for 10 hours, calcined at 240°C for 3 hours, and then calcined at 850°C for 4 hours with a heating rate of 5°C / min to obtain the alumina carrier A2 of the present invention. Then use SiO 2 A2 was impregnated with...

Embodiment 3

[0049] Mix 20g of the fourth-line oil, 30g of the first-line oil, 25g of the second-line wax paste, and 15g of SP-80, heat to dissolve at 100°C, and mix well; heat 800g of aluminum nitrate nonahydrate to 100°C to melt, slowly add to the above mixture, and mix A uniform supersolubilized colloid was formed in 30 minutes. In a closed reactor, add 110 g of liquid ammonia at 50° C. to the supersolubilizing colloid, and react at 180° C. for 2 hours to obtain nanometer aluminum hydroxide gel. Wash three times with 200ml of distilled water, and dry at 120°C for 10 hours. Subsequent steps and conditions were the same as in Example 3 to obtain alumina carrier A3. Then adopt 50% zirconium oxychloride aqueous solution 23ml to impregnate A3, dry at 100 DEG C for 4 hours, and roast at 350 DEG C for 3 hours to obtain AA3.

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Abstract

The invention discloses macroporous aluminium oxide carrier and a preparation method thereof. The aluminium oxide carrier uses aluminium hydroxide gel prepared by molten salt super-solubility micelle method as raw material; the preparation method comprises the following steps: shaping, drying, roasting, and dipping precursor solution containing modifying agent to obtain the macroporous aluminium oxide carrier containing modifying agent. During the preparation process of the carrier, as aluminium hydroxide gel contains surfactant and hydrocarbon component, nanometer aluminium oxide particles still have stick-shaped basic structure, wherein after shaping and roasting, aluminium hydroxide is dewatered through polymerization so as to form nanometer aluminium oxide particles; and nanometer aluminium oxide particles are stacked randomly to form a frame structure, and modifying agent is used to block most of small pores, thus reducing the active metal amount of the dipped carrier and achieving the aim of reducing the production cost of catalyst. The obtained aluminium oxide carrier has large pore volume and bore size, high porosity, larger outer pore mouth and good pore passage penetrability, thus the deposition of impurities can be increased and the operating period of catalyst can be prolonged.

Description

technical field [0001] The invention relates to an alumina carrier and a preparation method thereof, in particular to a macroporous alumina carrier used as a residual oil hydrotreating catalyst and a preparation method thereof. Background technique [0002] So far, the catalyst carrier used in the fixed bed of residual oil is still the classic alumina carrier. High temperature calcination method, pH value swing method and water vapor treatment can all obtain macroporous alumina suitable for residual oil, the pore volume of which is concentrated at 8-15nm can reach more than 80%, and the catalyst has high initial activity. The pores of macroporous alumina are continuous through the residual oil molecules, but the pores are too concentrated at about 10nm-20nm, which is not conducive to the long-term operation of the catalyst. The blockage of the catalyst bed causes the shutdown of the device and the replacement of the catalyst. The main reason is that when the concentrated po...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J21/04B01J35/02B01J37/10B01J37/08C10G45/04
Inventor 王鼎聪刘纪端
Owner CHINA PETROLEUM & CHEM CORP
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