MOFs desulfurizer based on organic amine in-situ modification and preparation and application thereof

An in-situ modification and desulfurization agent technology, applied in the direction of refined hydrocarbon oil, other chemical processes, chemical instruments and methods, etc., can solve the problem of single interaction of active components, insufficient exposure of active components, and limited utilization of active sites The synthesis method is simple, convenient and quick, saves the time of organic amine modification, and helps dissociation and diffusion.

Active Publication Date: 2021-07-09
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, H under static conditions 2 S pressure swing adsorption is not easy to meet the dynamic industrial desulfurization process; the active components of MOFs materials are single or the interaction is weak, making the desulfurization performance relatively poor
As another example, the pore structure of MOFs materials is mainly micropores, the active components are not fully exposed, and the mass transfer is relatively slow, which limits the utilization of active sites.

Method used

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  • MOFs desulfurizer based on organic amine in-situ modification and preparation and application thereof
  • MOFs desulfurizer based on organic amine in-situ modification and preparation and application thereof
  • MOFs desulfurizer based on organic amine in-situ modification and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 0.524g of trimesic acid, add it into 15ml of anhydrous methanol, stir and dissolve at room temperature to obtain solution A.

[0037] Weigh 1.872g of copper nitrate trihydrate, add it into 15ml of deionized water, stir and dissolve at room temperature to obtain solution B.

[0038] The above-mentioned solution A was added to the solution B, and stirred for 15 minutes to maintain a homogeneous phase to obtain a mixed solution.

[0039] Continue to add 0.667ml of n-butylamine to the mixed solution, stir at room temperature for 24h, filter with suction, wash the precipitate with ethanol solution, and dry at 120°C for 12h to obtain BA-Cu-BTC desulfurizer modified in situ with n-butylamine .

[0040] The specific surface area of ​​the above-mentioned BA-Cu-BTC desulfurizer is 1011.9m² / g, the total pore volume is 0.69cm³ / g, of which the micropore volume is 0.41cm³ / g, and the mesopore volume is 0.28cm³ / g. After testing, the calculated breakthrough sulfur capacity of th...

Embodiment 2

[0042] Weigh 0.524g of trimesic acid, add it into 15ml of anhydrous methanol, stir and dissolve at room temperature to obtain solution A.

[0043] Weigh 1.872g of copper nitrate trihydrate, add it into 15ml of deionized water, stir and dissolve at room temperature to obtain solution B.

[0044] The above-mentioned solution A was added to the solution B, and stirred for 15 minutes to maintain a homogeneous phase to obtain a mixed solution.

[0045] Continue to add 0.727ml triethylamine to the mixed solution, stir at room temperature for 24h, filter with suction, rinse the precipitate with ethanol solution, and dry at 120°C for 12h to obtain TEA-Cu-BTC desulfurizer modified in situ with triethylamine .

[0046] The specific surface area of ​​the above-mentioned TEA-Cu-BTC desulfurizer is 1094.9m² / g, the total pore volume is 0.68cm³ / g, of which the micropore volume is 0.46cm³ / g, and the mesopore volume is 0.23cm³ / g. After testing, the calculated breakthrough sulfur capacity of ...

Embodiment 3

[0048] Weigh 0.524g of trimesic acid, add it into 15ml of anhydrous methanol, stir and dissolve at room temperature to obtain solution A.

[0049] Weigh 1.872g of copper nitrate trihydrate, add it into 15ml of deionized water, stir and dissolve at room temperature to obtain solution B.

[0050] The above-mentioned solution A was added to the solution B, and stirred for 15 minutes to maintain a homogeneous phase to obtain a mixed solution.

[0051] Continue to add 0.891ml of triethanolamine to the mixed solution, stir at room temperature for 24 hours, filter with suction, rinse the precipitate with ethanol solution, and dry at 120°C for 12 hours to obtain TEOA-Cu-BTC desulfurizer modified in situ with triethanolamine.

[0052] The specific surface area of ​​the above-mentioned TEOA-Cu-BTC desulfurizer is 607.2m² / g, the total pore volume is 0.59cm³ / g, of which the micropore volume is 0.26cm³ / g, and the mesopore volume is 0.33cm³ / g. After testing, the calculated breakthrough sul...

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Abstract

The invention discloses an MOFs desulfurizer based on organic amine in-situ modification and a preparation method thereof. The preparation method comprises the following steps: preparing an MOF material Cu-BTC by using copper salt and trimesic acid as raw materials, adding small-molecule organic amine for in-situ modification, and preparing the organic amine in-situ modification MOFs desulfurizer A-Cu-BTC by using a solution diffusion method. The MOFs crystal structure is improved through in-situ preparation, the grain size of MOFs is reduced, and organic amine molecules are introduced to increase adsorption active site components, generate abundant stacked mesoporous apertures and increase the alkalinity of the material surface, so that the adsorption and dissociation performance on H2S is improved, and the sulfur capacity of the MOFs desulfurizer is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of desulfurizer preparation, and relates to a metal organic framework material desulfurizer, in particular to a metal organic framework material desulfurizer modified by organic amine, and a preparation method of the desulfurizer. Background technique [0002] Hydrogen sulfide (H 2 S) is a poisonous gas with a disgusting smell that is extremely threatening to humans and the environment, and is mainly derived from the chemical production process of coal, oil, and natural gas processing. h 2 The existence of S will corrode equipment and pipelines, poison catalysts and reduce production efficiency, and emit SO into the air. 2 , forming acid rain and damaging the environment. So, H 2 The removal of S is very necessary for the pollution control and operation safety of industrial production process. [0003] Adsorption method is a desulfurization technology that is widely studied at present. Its operation pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C10L3/10C10G25/00B01D53/02
CPCB01J20/226B01J20/22C10L3/103C10G25/003B01D53/02B01D2257/304
Inventor 樊惠玲王业双杨超梁丽彤杨颂寇佳伟林建英
Owner TAIYUAN UNIV OF TECH
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