Preparation method of hydrodemetallization catalyst

A hydrodemetallization and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problem of further improvement of the interaction between active components and supports, pore volume and macropore content Lowering, collapse, etc.

Active Publication Date: 2019-08-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the molding process of the alumina carrier, it is necessary to knead pseudo-boehmite dry rubber powder, extrusion aids, peptizers, etc. The macropores of the body itself partially collapse, so that the pore volume and macropore content of the final carrier are greatly reduced
In addition, the interaction between the active ingredient and the carrier needs to be further improved

Method used

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  • Preparation method of hydrodemetallization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 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.

[0037] Weigh 200 g of the above-mentioned pseudo-boehmite and place it in a beaker, add 400 mL of xylitol aqueous solution with a mass concentration of 25% to the beaker and soak for 4 hours. The impregnated material is ...

Embodiment 2

[0041] 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 pseudo-boehmite was impregnated with a mixed aqueous solution of sorbitol and mannitol with a mass concentration of 40% and a mass ratio of 1:1 for 3 hours. The carbonization treatment temperature is 130°C, and the treatment time is 14 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 impregnat...

Embodiment 3

[0043] 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 discloses a preparation method of a hydrodemetallization catalyst. The preparation method comprises the following steps: (1) mixing pseudo-boehmite with deionized water, mashing, adding a mixed acid solution of organic acid and inorganic acid into the size, and carrying out heating reflux treatment; adding urea into the size, and carrying out hydrothermal treatment; (2) impregnating pseudo-boehmite dry glue powder obtained in the step (1) with an aqueous solution containing polyalcohol and / or carbohydrate, and carrying out hydrothermal carbonization treatment; (3) preparing at least two kinds of polyalcohol and / or monosaccharide aqueous solution with different concentrations, spraying and impregnating onto an alumina carrier obtained in the step (2) in a sequence from high concentration to low concentration, and carrying out hydrothermal carbonization treatment on the impregnated alumina carrier; and (4) loading a hydrogenation active component to the carrier, so that the hydrodemetallization catalyst product is obtained. The hydrodemetallization catalyst prepared by adopting the preparation method has an appropriate porous structure, effects of the active component and the carrier are moderate, and the hydrodemetallization catalyst has higher demetallization activity and activity stability in heavy and residual oil hydrogenation reaction.

Description

technical field [0001] The invention relates to a preparation method of a hydrodemetallization catalyst. 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. During the calcination process after loading the active component, the active metal component is easy to react with the alumina carrier to form a strong M-O-Al bond, which causes the active component to form a spinel phase and lose its activity, or the active component cannot be com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/19C10G45/08
CPCB01J27/19C10G45/08C10G2300/205
Inventor 季洪海王少军凌凤香沈智奇杨卫亚王丽华郭长友
Owner CHINA PETROLEUM & CHEM CORP
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