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Phosphorus-and potassium-containing aluminum oxide carrier and preparation method thereof

A technology of alumina carrier and alumina phosphorus oxide, which is applied in the direction of catalyst carrier, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of small pores and underutilized pores, and achieve large pores and extended operation Period, effect of increasing deposition amount

Active Publication Date: 2013-01-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] CN1123309A discloses a preparation method of a residual oil demetallization catalyst. The selected alumina carrier has a pore volume of 0.45-0.8ml / g, and the edge of the catalyst is passivated by potassium, but this catalyst does not have fully utilized pore channels
[0009] CN1123196A discloses a preparation method of residual oil demetallization catalyst, which uses potassium dihydrogen phosphate to prevent potassium loss, but this invention also has the disadvantage of too small pores

Method used

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  • Phosphorus-and potassium-containing aluminum oxide carrier and preparation method thereof

Examples

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Embodiment 1

[0046] 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 30g of binder pseudo-boehmite; mix 2.6g of dilute nitric acid (mass concentration 17%), 18g of water and 1g of cosolvent ethanol, and mix the two mixtures Uniform, and then shaped in the extruder, the pressure is controlled 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 alumina carrier A1. 4ml containing 0.5g KH 2 PO 4 The solution was sprayed on the above-...

Embodiment 2

[0048] 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. Spray the mixed aqueous solution of 0.2...

Embodiment 3

[0050] 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, 110 g of liquid ammonia at 50° C. was added to the supersolubilizing colloid, and reacted 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. Spray the solution of 0.1g phosphoric acid and 0.1g potassium nitrate on the above-mentioned 100g A3 carrier in an atomized manner, dry at 100°C for 3 hours, and bake at 550°C for 4 hours to obtain the potassium and phosphorus-containing alumina carrier of the present invention KA3.

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Abstract

The invention discloses a phosphorus- and potassium-containing aluminum oxide carrier and a preparation method thereof. The aluminum oxide carrier is prepared by molding an aluminum oxide carrier by using aluminum hydroxide gel, which is prepared by a molten-salt super-solubility micelle method, as a raw material at first and then loading potassium and phosphorus on the aluminum dioxide carrier in a spraying and soaking mode. In a process of preparing the carrier, the aluminum hydroxide gel has a surfactant and hydrocarbon components, so that after the aluminum hydroxide gel is molded and roasted, aluminum oxide nanoparticles formed by dewatering the polymerized aluminum oxide still have a rod-like basic structure; the aluminum oxide nanoparticles are stacked into a framework structure in a disordered way, so that the carrier has a large pore volume, a large aperture, a high porosity, a large outer surface orifice and high duct penetrability; and after the surface acidity of the carrier is reduced by the potassium and the phosphorus, the surface activity of a catalyst is reduced, so that asphaltene micelles tend to disperse into the inner part of the carrier to undergo a reaction. Thus, a hydrocracking reaction is restrained, the generation of carbon deposit is prevented, a residual hydrodemetalization reaction is carried out smoothly, and the capability of dissolving metals is improved.

Description

technical field [0001] The invention relates to an alumina carrier containing phosphorus and potassium and a preparation method thereof, in particular to an alumina carrier used as a residual oil demetallization catalyst and a preparation method thereof. Background technique [0002] At present, hydroprocessing is still the most important means to produce high-quality, environment-friendly petroleum products. The core of hydroprocessing technology is the catalyst, and the performance of the carrier is the key to preparing a hydroprocessing catalyst with excellent properties. For the heavy components of petroleum (such as VGO, especially residual oil), the pore size and pore volume of the carrier will directly affect the catalyst activity. [0003] So far, the catalyst carrier used in the fixed bed of residual oil is still the classic alumina carrier. High-temperature roasting method, pH value swing method and steam treatment can all obtain macroporous alumina suitable for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/14B01J32/00B01J21/04B01J35/10B01J37/00C10G45/04
Inventor 王鼎聪刘纪端
Owner CHINA PETROLEUM & CHEM CORP