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Preparation method of mesoporous active material

An active material and mesoporous technology, which is applied in the field of preparation of mesoporous active materials, can solve the problems of high price and stability of organic silicon, uneven distribution of silicon and aluminum, low impurity content, etc., and achieve smooth pores and strong conversion capacity of heavy oil , the effect of small granularity

Active Publication Date: 2017-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

US4,003,825 discloses a method for preparing silicon-aluminum materials by hydrolysis of organosilicon compounds in an aqueous solution of aluminum nitrate, but organosilicon is expensive and has certain stability problems
US5,045,519 discloses a method for preparing a silicon-aluminum material by mixing and hydrolyzing alkoxy aluminum and orthosilicic acid in an aqueous medium. The material obtained by this method has a pseudo-boehmite structure, low impurity content, and thermal stability Well, more acidic, but less even distribution between silicon and aluminum

Method used

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  • Preparation method of mesoporous active material
  • Preparation method of mesoporous active material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This example illustrates the preparation method of the mesoporous active material provided by the present invention.

[0023] Take Al 2 (SO 4 ) 3 Solution (concentration 90gAl 2 o 3 / L) and ammonia (mass fraction 25%) are reaction raw materials. Using the method of co-flow gelation, under vigorous stirring, the Al 2 (SO 4 ) 3 Solution and ammoniacal liquor are mixed into gel, 40 DEG C of gel forming temperature, and gel forming pH value is 9.0, simultaneously the water glass solution (concentration 100gSiO 2 / L) mixed with the above-mentioned colloidal slurry in parallel flow to realize the online addition of silicon source. After collecting a certain amount of mixed slurry, raise the temperature to 70°C and age for 2 hours; Base: HCl: H 2 The weight ratio of O=1:0.1:10 was exchanged at 30°C for 0.5 hours, filtered and washed with water to obtain a mesoporous active material, which was designated as SM-1.

[0024] SM-1 has a pseudo-boehmite crystal phase struc...

Embodiment 2

[0026] This example illustrates the preparation method of the mesoporous active material provided by the present invention.

[0027] Take Al 2 (SO 4 ) 3 The solution and ammonia water are used as the reaction raw materials, and the Al 2 (SO 4 ) 3 The solution and ammonia water are mixed to form a gel, the gelation temperature is 30°C, and the pH value of the gelation is 10.0. At the same time, the metered water glass solution and the above-mentioned gelling slurry are mixed in parallel to realize the online addition of silicon sources. A large amount of mixed slurry was heated to 60°C and aged for 2 hours; after filtration, the obtained solid precipitate was calculated according to the dry basis of the precipitate: HCl: H 2 The weight ratio of O=1:0.08:15 was exchanged at 50°C for 0.3 hours, filtered and washed with water, and the exchange was repeated once. After filtration, the mesoporous active material was obtained, which was designated as SM-2.

[0028] SM-2 has a p...

Embodiment 3

[0030] This example illustrates the preparation method of the mesoporous active material provided by the present invention.

[0031] Take Al 2 (SO 4 ) 3 solution and NaAlO 2 Solution (concentration 190gAl 2 o 3 / L) is the reaction raw material, co-flow gel at room temperature and control the gel pH value to be 10.5, and simultaneously mix the water glass solution and the colloid slurry in proportion to realize the online addition of silicon source, and then the collected The slurry is heated to 60°C and aged for 4 hours; after filtration, the obtained solid precipitate is calculated on a dry basis of the precipitate: H 2 SO 4 :H 2 The weight ratio of O=1:0.12:15 was exchanged at room temperature for 1 hour, filtered and washed with water to obtain a mesoporous active material, which was designated as SM-3.

[0032] SM-3 has a pseudo-boehmite crystal phase structure, and its X-ray diffraction pattern has the characteristics of the attached figure; the chemical compositi...

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Abstract

The invention relates to a preparation method of a mesoporous active material. The preparation method is characterized by comprising the following steps: mixing an aluminum source and an alkaline solution at the temperature from room temperature to 85 DEG C to form gel, controlling a pH value of the formed gel to be 7-11, adding a needed silicon source in gel formation slurry in a flow combination manner at the same time in the gel formation process, ageing and filtering a mixture, carrying out exchange on obtained solid precipitates for at least 0.2h at the temperature from the room temperature to 100 DEG C according to the weight ratio of dry basis to acid to H2O is 1 to (0.03-0.30) to (5-30), and washing the exchanged solid precipitates until the content of sodium oxide is 0.2 percent or below, wherein the weight ratio of the silicon source (by SiO2) to the aluminum source (by Al2O3) is 1 to (0.6-9). The mesoporous active material prepared by the method is small in particle size, more unobstructed in channel, obvious in mesoporous characteristics, higher in ratio of B acid and L acid sites and improved in heavy oil conversion ability.

Description

technical field [0001] The invention relates to a preparation method of a mesoporous active material, in particular to a preparation method of a mesoporous material with smaller particle size, unobstructed mesoporous channels, higher B-acid ratio and higher heavy oil conversion capacity. Background technique [0002] Catalytic cracking is a very important process in the petroleum refining process. It is widely used in the petroleum processing industry and occupies a pivotal position in the refinery. In the catalytic cracking process, heavy fractions such as vacuum distillates or residues of heavier components are reacted in the presence of a catalyst to convert gasoline, distillate and other liquid cracking products and lighter gaseous cracking of up to four carbons products, catalytic materials with high acidity and high cracking activity are usually required to be used in these reaction processes. [0003] Microporous molecular sieve materials are widely used in petroleum...

Claims

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Application Information

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IPC IPC(8): B01J23/04B01J21/12C10G11/04
CPCC10G11/04B01J21/12B01J23/002B01J23/04B01J2523/00C10G2300/70B01J35/647B01J35/615B01J2523/12B01J2523/22B01J2523/31
Inventor 王成强郑金玉罗一斌
Owner CHINA PETROLEUM & CHEM CORP
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