Preparation method of modified mesoporous silicon-aluminum material

A mesoporous silica-alumina, modified technology, applied in chemical instruments and methods, catalyst carriers, catalysts for physical/chemical processes, etc., can solve the problem of poor hydrothermal stability, weak acidity of mesoporous molecular sieves, catalyst production stability and life. And other issues

Active Publication Date: 2015-12-09
QINGDAO HUICHENG PETROCHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high content of macromolecular hydrocarbons and high nitrogen, sulfur and metal content in heavy oil, the existing catalysts are seriously affected in terms of production stability and service life. Catalyst activity decline or deactivation caused by coking and coking, urgently require the carrier widely used in the petroleum processing industry to have the characteristics of large pore volume and high specific surface, so as to improve the ability of the device to process inferior raw material oil
[0003] Mesoporous molecular sieves have a large specific surface area, which can effectively solve the diffusion limitation of microporous zeolites, and provide favorable spatial configurations for the catalysis, adsorption and separation of macromolecules. However, mesoporous molecular sieves have weak acidity and are hydrothermally stable Poor sex

Method used

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  • Preparation method of modified mesoporous silicon-aluminum material
  • Preparation method of modified mesoporous silicon-aluminum material
  • Preparation method of modified mesoporous silicon-aluminum material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add (calculated as alumina) 10% pseudo-boehmite slurry into 50% phosphoric acid solution, control the reaction temperature at 50°C, and react for 10 hours, wherein P 2 o 5 / Al 2 o 3 =2.0 (this ratio is relatively low, need to increase the reaction temperature), recorded as solution A.

[0028] (2) The concentration is 45g / l (as Al 2 o 3 meter) aluminum chloride solution with a concentration of 55g / l (as SiO 2 In the water glass solution, control the pH=10.3, the temperature is 10 ℃, static aging for 1 hour, record it as solution B.

[0029] (3) Mix solution A with a concentration of 85g / l (with Al 2 o 3 In terms of) aluminum chloride as P 2 o 5 :Al 2 o 3 =0.06 was added into solution B, the pH was controlled to be 3.4, and the temperature was 10°C, which was recorded as solution C.

[0030] (4) Add the lanthanum chloride solution in solution C in a certain proportion, control lanthanum:aluminum=0.02, record it as solution D.

[0031] (5) Add 5% ammonia ...

Embodiment 2

[0035] (1) Add (calculated as alumina) 20% pseudoboehmite slurry into 60% phosphoric acid solution, control the reaction temperature at 60°C, and react for 15 hours, wherein P 2 o 5 / Al 2 o 3 =3.0, recorded as solution A.

[0036] (2) The concentration is 50g / l (as Al 2 o 3 meter) of aluminum sulfate solution with a concentration of 60g / l (as SiO 2 In the alkaline silica sol solution, the pH is controlled at 10.4, the temperature is 20° C., and the static aging is 1.5 hours, which is recorded as solution B.

[0037] (3) Mix solution A with a concentration of 90g / l (with Al 2 o 3 In terms of aluminum sulfate in P 2 o 5 :Al 2 o 3 =0.08 into solution B, control pH=3.5, temperature 20°C, record as solution C.

[0038] (4) Add the lanthanum chloride solution in solution C in a certain proportion, control lanthanum:aluminum=0.03, record it as solution D.

[0039] (5) Add 5% sodium hydroxide to solution D to control pH=8.2.

[0040] (6) Wash and filter with chemical wat...

Embodiment 3

[0043] (1) Add (calculated as alumina) 30% pseudo-boehmite slurry into 70% phosphoric acid solution, control the reaction temperature at 70°C, and react for 20 hours, wherein P 2 o 5 / Al 2 o 3 =4.0, recorded as solution A.

[0044] (2) The concentration is 50g / l (as Al 2 o 3 The concentration of sodium metaaluminate solution added is 60g / l (as SiO 2 In the water glass solution, control the pH=10.5, the temperature is 30 ℃, static aging for 2 hours, record it as solution B.

[0045] (3) Mix solution A with a concentration of 90g / l (with Al 2 o 3 In terms of) sodium metaaluminate dissolved in P 2 o 5 :Al 2 o 3 =0.10 was added to solution B, the pH was controlled to be 3.6, the temperature was 30°C, and it was recorded as solution C.

[0046] (4) Add the lanthanum chloride solution in solution C in a certain proportion, control lanthanum:aluminum=0.04, record it as solution D.

[0047] (5) Add 5% ammonia water to the solution D to control the pH=8.4.

[0048](6) Was...

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Abstract

The invention discloses a preparation method of a modified mesoporous silicon-aluminum material. The modified mesoporous silicon-aluminum material has a pseudo-boehmite physical structure. The anhydrous chemical formula of the material by the weight of oxides is (0-8)P2O5(0-0.1)Na2O*(20-30)SiO2*(70-80)Al2O3(0-1.0)RE2O3. The specific area is 200 to 500 m2/g, and the pore volume is 0.5 to 1.5 mL/g. The preparation method comprises the following steps: step one, adding a low-concentration aluminum source into a silicon source solution, controlling the pH in a range of 10.3 to 10.8, and carrying out stationary aging for 0.5 to 3 hours; step two, adding phosphor-aluminum gel and a high-concentration aluminum source into the previous solution according to a certain ratio, and controlling the pH in a range of 3.4 to 3.8; step three, adding a rare earth solution according to a certain ratio; step four, adjusting the pH of the previous slurry to 8.0-9.0 by an alkaline solution; step five, filtering the slurry, and washing the solids by deionized water and ammonium salt. The provided modified mesoporous silicon-aluminum material can be used as the carrier of FCC catalyst, has a proper pore volume and acidic property, and is capable of performing pre-cracking on macromolecular raw oil. RE2O3 exists in a deposited state of oxides and can prevent the metal pollution, so the provided material can improve the heavy oil cracking performance of FCC catalyst, moreover, the hydrothermal stability of FCC catalyst is good, and the coke selectivity is excellent.

Description

technical field [0001] The invention relates to a modified mesoporous silicon-aluminum material, in particular to an FCC catalyst modified mesoporous silicon-aluminum material carrier with large pore volume and suitable pore structure. Background technique [0002] Due to the increasingly inferior quality of petroleum resources and environmental regulations, the requirements for the content of sulfur, olefins and aromatics in gasoline and diesel for vehicles are becoming more and more stringent. Due to the high content of macromolecular hydrocarbons and high nitrogen, sulfur and metal content in heavy oil, the existing catalysts are seriously affected in terms of production stability and service life. Catalyst activity decline or deactivation caused by coking and coking, etc., urgently require the carrier widely used in the petroleum processing industry to have the characteristics of large pore volume and high specific surface area, so as to improve the ability of the device...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J32/00B01J35/10
Inventor 李凤高明军叶红李正刘惠娟杨海龙张新功
Owner QINGDAO HUICHENG PETROCHEM TECH
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