Preparation method of gallium-containing zeolite and application to coal pyrolysis volatile matter transformation

A technology of zeolite and gallium source is applied in the field of preparation of gallium-containing zeolite to achieve the effects of promoting conversion, simple synthesis method and mild conditions

Active Publication Date: 2019-03-08
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no literature and patent reports on the application of gallium-containing zeolite in coal pyrolysis volatile modification

Method used

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  • Preparation method of gallium-containing zeolite and application to coal pyrolysis volatile matter transformation
  • Preparation method of gallium-containing zeolite and application to coal pyrolysis volatile matter transformation
  • Preparation method of gallium-containing zeolite and application to coal pyrolysis volatile matter transformation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] (1) Under stirring conditions, first take 10.58g TPAOH and 0.233mL 10mol / L NaOH solution and add them to 10.81g water, then add 1.97g TPOAC to form a transparent solution A;

[0063] (2) Add 12.5g LUDOX HS-40 dropwise to solution A, stir for 1h after the dripping, add 0.21g gallium nitrate hydrate and 0.35g aluminum isopropoxide, and stir for 0.5h for aging;

[0064] (3) Transfer the solution obtained from step (2) room temperature aging to a stainless steel reactor with PTFE lining, crystallize at 140°C for 4 days, filter and wash with suction, dry at 105°C, and then roast at 550°C 6h;

[0065] (4) The solid obtained in step (3) is ion-exchanged with ammonium nitrate, exchanged three times, washed, dried, and calcined at 550° C. for 6 hours to obtain a multi-porous micron-scale framework-containing gallium molecular sieve with MFI framework structure.

[0066] See Figure 5 The molecular sieve prepared by this method obviously has intracrystalline mesopores formed by the remov...

Embodiment 2

[0068] (1) Under stirring conditions, first take 10.58g TPAOH and 0.233mL 10mol / L NaOH solution and add them to 10.81g water, then add 1.97g TPOAC to form a transparent solution A;

[0069] (2) Add 12.5g LUDOX HS-40 dropwise to A, stir for 1h, add 0.21g gallium nitrate hydrate and 0.087g aluminum isopropoxide, stir for 0.5h;

[0070] (3) Transfer the solution obtained from step (2) room temperature aging to a stainless steel reactor with PTFE lining, crystallize at 140°C for 4 days, filter and wash with suction, dry at 105°C, and then roast at 550°C 6h;

[0071] (4) The solid obtained in step (3) is ion-exchanged with ammonium nitrate, exchanged three times, washed, dried, and calcined at 550° C. for 6 hours to obtain a multi-porous micron-scale framework-containing gallium aluminum molecular sieve with MFI framework structure.

[0072] See Image 6 The molecular sieve prepared by this method can also observe the mesopores formed by the accumulation of particles on the surface and the...

Embodiment 3

[0074] (1) Under stirring conditions, first take 10.58g TPAOH and 0.233mL 10mol / L NaOH solution and add them to 10.81g water, then add 1.97g TPOAC to form a transparent solution A;

[0075] (2) Add 12.5g LUDOX HS-40 dropwise to A, stir for 1h, add 0.21g gallium nitrate hydrate and 0,17g aluminum isopropoxide, and stir for 0.5h;

[0076] (3) Transfer the solution obtained from step (2) room temperature aging to a stainless steel reactor with PTFE lining, crystallize at 140°C for 4 days, filter and wash with suction, dry at 105°C, and then roast at 550°C 6h;

[0077] (4) The solid obtained in step (3) is ion-exchanged with ammonium nitrate, exchanged three times, washed, dried, and calcined at 550° C. for 6 hours to obtain a multi-porous micron-scale framework-containing gallium aluminum molecular sieve with MFI framework structure.

[0078] See Figure 7 Obvious intracrystalline and intercrystalline mesopores can also be observed when synthesizing molecular sieves by this method. The ...

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Abstract

The invention discloses a preparation method of gallium-containing zeolite and an application to coal pyrolysis volatile matter transformation. A solution is prepared from water, a microporous template agent, NaOH and a mesoporous template agent, a silicon source is added dropwise, stirring is performed after addition of the silicon source, a gallium source and an aluminum source are added after the silicon source is hydrolyzed and dispersed, an obtained mixture is crystallized for 2-6 days at 100-180 DEG C after aging, ammonium nitrate ion exchange is performed after crystallization and roasting, roasting is performed again after drying, and hierarchically porous gallium-containing zeolite with an MFI skeleton is obtained. According to gallium-containing zeolite, carbon deposition inactivation of a catalyst can be reduced to a certain degree; aiming at various substances contained in coal pyrolysis volatile matter, a weak acid site formed by skeleton gallium and gallium outside the skeleton can be subjected to concerted catalysis with Si-OH-Al (a strong B acid site) in a molecular sieve, dehydrogenation, pyrolysis, oligomerization and aromatization of macromolecular alkane can bepromoted, CH4 can be activated by formed olefins under the action of Ga2O3, and methane is promoted to be converted into long-chain olefins and arenes.

Description

Technical field [0001] The invention relates to a preparation method of gallium-containing zeolite and its application in coal pyrolysis volatile matter upgrading. Background technique [0002] Coal occupies a dominant position in my country's energy structure, accounting for about 70% of primary energy production and consumption. Clean and efficient use of coal is the focus of coal chemical technology. The coal pyrolysis process is to extract the hydrogen-rich components of coal in the form of liquid or gas under anaerobic conditions before coal gasification, combustion or other methods are used. The liquid product obtained from coal pyrolysis, namely coal tar, is an important chemical raw material. Coal tar contains a large amount of aromatic hydrocarbons, phenols and other compounds, which can be used as raw materials for fine chemicals and new chemical materials, and has extremely high economic efficiency. value. However, the quality of tar in the traditional pyrolysis proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/06C10C1/20
CPCC10C1/20C01B39/065C01P2004/03C01P2004/62C01P2004/61
Inventor 陈汇勇毕晨瑶王晓宵尤晴王旭张建波郝青青马晓迅
Owner NORTHWEST UNIV(CN)
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