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Preparation method of carbon-containing macroporous alumina carrier

A technology of alumina carrier and macroporous alumina, which is applied in the direction of catalyst carrier, chemical instruments and methods, chemical/physical processes, etc., and can solve the problems that the interaction needs to be further improved and the influence of carrier strength, etc.

Active Publication Date: 2017-10-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, adding a physical pore-enlarging agent often affects the strength of the carrier
In addition, the interaction between the alumina carrier and the active component prepared by the prior art needs to be further improved

Method used

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  • Preparation method of carbon-containing macroporous alumina carrier
  • Preparation method of carbon-containing macroporous alumina carrier
  • Preparation method of carbon-containing macroporous alumina carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 200g of pseudoboehmite dry rubber powder (produced by Wenzhou Jingjing Alumina Co., Ltd.) and place it in a round bottom flask, add 600g of deionized water to the flask for beating, and add an appropriate amount of nitric acid to the above slurry with a molar concentration of 3mol / L, the mixed acid solution whose molar concentration of acetic acid is 1mol / L, the pH value of the slurry is controlled to be 3 and heated to reflux at 40°C for 3 hours. The above slurry was transferred into an autoclave, 20 g of urea was added to the mixed material, and the autoclave was sealed and heat treated at 140° C. for 6 hours. After cooling to room temperature, the mixed slurry was filtered, washed, and dried at 120° C. for 8 hours to obtain pseudo-boehmite. The treated pseudo-boehmite is fully mixed with 8 g of scallop powder, and an appropriate amount of aqueous solution dissolved in 4 g of acetic acid is added to the above materials, kneaded evenly, and extruded into cylindr...

Embodiment 2

[0035] With embodiment 1, just the add-on of deionized water is 1400 grams. The mixed acid is a mixed acid dissolved with 4 mol of sulfuric acid and 1 mol of oxalic acid, the pH value of the slurry is controlled to be 2, and the temperature of heating and refluxing is 30°C for 5 hours. The addition amount of urea is 30 grams, and hydrothermal treatment temperature is 120 ℃, and hydrothermal treatment is 8 hours. The alumina carrier is in the shape of clover strips. For the first spray and impregnation, use 30ml of an aqueous solution of sorbitol with a mass concentration of 30%, and for the second spray and impregnation, use 50ml of an aqueous solution of sorbitol with a mass concentration of 10%. In the first spraying and impregnation, 20ml of sorbitol aqueous solution with a mass concentration of 5% was used. The temperature of carbonization treatment was 200°C and the carbonization time was 8 hours to obtain alumina carrier S2. The properties of the carrier are shown in Tab...

Embodiment 3

[0037] With embodiment 1, just the add-on of deionized water is 2000 grams. The mixed acid is a mixed acid dissolved with 6mol / L sulfuric acid and 1mol / L citric acid, the pH value of the slurry is controlled to be 5, the heating reflux temperature is 60°C, and the reflux time is 1 hour. The amount of urea added was 40 grams, the hydrothermal treatment temperature was 160° C., and the hydrothermal treatment time was 4 hours. The pseudo-boehmite was impregnated with a mixed aqueous solution of glucose and ribose with a mass ratio of 1:1 at a mass concentration of 30% for 5 hours. The carbonization treatment temperature is 120° C., and the carbonization treatment time is 16 hours. Adopt four times of spray impregnation, use 20ml mass concentration to be the aqueous solution of mannitol of 50% when spraying and impregnating for the first time, use 40ml mass concentration to be the aqueous solution of sorbitol of 30% when spraying and impregnating for the second time, the third ti...

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Abstract

The invention provides a preparation method of a carbon-containing macroporous alumina carrier. The preparation method comprises the following contents: (1) mixing and pulping pseudo-boehmite and deionized water, adding a proper amount of mixed acid solution of an organic acid and an inorganic acid to the slurry and carrying out heating reflux treatment; (2) adding a proper amount of urea for hydro-thermal treatment, carrying out washing and drying, and molding, drying and roasting the treated pseudo-boehmite to obtain an alumina carrier; (3) preparing at least two polyol and / or monosaccharide water solutions of different concentration, spraying the water solutions to the alumina carrier obtained in the step (2) according to the concentration order from high to low; and (4) carrying out hydrothermal carbonization treatment on the alumina carrier dipped in the step (3) and then drying to obtain the carbon-containing macroporous alumina carrier. The alumina carrier prepared through the method has relatively large pore volume and pore diameter, the carbon content is in uneven distribution in the radial direction of the carrier, and the carrier is suitable for the field of preparation of heavy oil or residual oil hydrodemetallization catalysts.

Description

technical field [0001] The invention relates to a method for preparing an alumina carrier, in particular to a method for preparing a carbon-containing alumina carrier with relatively large pore volume and pore diameter. Background technique [0002] At present, in the production process of heavy oil hydrodemetallization, because the raw oil contains a certain amount of impurities such as vanadium, sulfur, arsenic, nickel, etc., it is easy to form deposits, thereby blocking the pores of the catalyst, resulting in a rapid decline in catalyst activity, and even Inactivation affects industrial applications. Catalysts with larger pore volume and larger pore diameter have strong metal and carbon storage capacity, which can slow down the deactivation of the catalyst and prolong the operation period of the catalyst. The pore structure of the catalyst is determined by the carrier that constitutes the catalyst. Therefore, the preparation of a carrier with a larger pore volume and lar...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J21/18B01J35/10
CPCB01J21/18B01J35/695B01J35/635B01J35/647B01J35/615
Inventor 佟佳吕振辉
Owner CHINA PETROLEUM & CHEM CORP
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