An organic porous framework material with adsorption and desulfurization performance and its preparation method

A porous skeleton, adsorption desulfurization technology, applied in chemical instruments and methods, refined hydrocarbon oil, inorganic chemistry, etc., can solve problems such as intolerance to strong acid and strong alkali, difficult regeneration, poor thermal stability, etc.

Active Publication Date: 2022-05-20
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commercial zeolites and activated carbons have the advantages of low cost and easy availability, but the strong acid sites in zeolites have strong interactions with sulfides, making their regeneration difficult
Due to the lack of suitable adsorption sites in activated carbon materials, the selective adsorption of thiophene sulfur is relatively poor.
MOFs materials have also been widely used in adsorption desulfurization research in recent years, and have shown excellent adsorption effects. However, MOFs materials have poor thermal stability and are not resistant to strong acids and alkalis, so they are limited in application range and reusability.

Method used

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  • An organic porous framework material with adsorption and desulfurization performance and its preparation method
  • An organic porous framework material with adsorption and desulfurization performance and its preparation method
  • An organic porous framework material with adsorption and desulfurization performance and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Step 1: Add 2mol of 1,3,5-benzenetricarbaldehyde and 3mol of 1,4-benzenediacetonitrile into the reactor, then add 1L of 1,4-dioxane and 1L of 1,3, 5 Trimethylbenzene solvent, after stirring evenly, add 0.2L of 6mol / L DBU (1,8-diazabicyclo[5.4.0]undec-7-ene) solution as a catalyst, and react at 150°C for 72h to obtain a mixed liquid;

[0047] Step 2: Cool the mixture obtained in Step 1 to room temperature, and pour it into the material barrel, during which time the residue in the kettle can be washed with deionized water. The obtained mixture was subjected to suction filtration, and deionized water and methanol were used as washing solvents, each washing three times to obtain a filter cake. Put the filter cake into a beaker filled with DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then carry out suction filtration. The obtained product was subjected to Soxhlet extraction with methanol reagent for 24 hours to further remove impurities, and the Soxhlet...

Embodiment 2

[0053] Step 1: Add 2mol monomer 1,3,5-benzenetricarbaldehyde and 3mol 1,4-benzenediacetonitrile into the reaction kettle, then add 2L of N,N-dimethylformamide solvent, stir well Add 0.2L of 6mol / L sodium hydroxide solution as a catalyst, and react at 100°C for 72h to obtain a mixed solution;

[0054] Step 2: Cool the mixture obtained in Step 1 to room temperature, and pour it into the material barrel, during which time the residue in the kettle can be washed with deionized water. The obtained mixture was subjected to suction filtration, and deionized water and methanol were used as washing solvents, each washing three times to obtain a filter cake. Put the filter cake into a beaker filled with DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then carry out suction filtration. The obtained product was subjected to Soxhlet extraction with methanol reagent for 24 hours to further remove impurities, and the Soxhlet-extracted solid was vacuum-dried at 100° C. for 1...

Embodiment 3

[0064] Step 1: Add 2mol of monomer 1,3,5-benzenetricarbaldehyde and 3mol of 1,4-benzenediacetonitrile into the reaction kettle, then add 2L of dichlorobenzene solvent, stir well and add 0.2L of 6mol / L of potassium carbonate solution was used as a catalyst, and reacted at 120°C for 72 hours to obtain a mixed solution;

[0065] Step 2: Cool the mixture obtained in Step 1 to room temperature, and pour it into the material barrel, during which time the residue in the kettle can be washed with deionized water. The obtained mixture was subjected to suction filtration, and deionized water and methanol were used as washing solvents, each washing three times to obtain a filter cake. Put the filter cake into a beaker filled with DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then carry out suction filtration. The obtained product was subjected to Soxhlet extraction with methanol reagent for 24 hours to further remove impurities, and the Soxhlet-extracted solid was va...

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Abstract

The invention discloses an organic porous framework material with adsorption and desulfurization performance and a preparation method thereof. Based on the Knoevenagel reaction principle, an aldehyde-based compound is used to undergo a condensation reaction with a cyano-based compound having an active α-hydrogen atom under weakly alkaline conditions. , and finally obtain a graphene-like organic porous framework material product connected by carbon-carbon double bonds between the reaction monomers. The material prepared by the invention has a large-area conjugated structural unit, and this structural feature makes it have a more significant adsorption effect on aromatic thiophene sulfur compounds than alkane compounds.

Description

technical field [0001] The invention belongs to the field of preparation of organic porous framework materials, and in particular relates to an organic porous framework material with adsorption desulfurization performance and a preparation method thereof. Background technique [0002] Fossil fuels (gasoline, diesel, kerosene, etc.) provide important support for the rapid development of society and people's lives, but also cause inevitable damage to our surrounding environment. Sulfur-containing compounds in fuel oil, such as thiophene sulfur, sulfide, etc., are burned to produce sulfur dioxide, which will cause serious pollution to the environment. Therefore, the laws and regulations of various countries in the world have strict restrictions on the sulfur content in fuel oil. With the improvement of environmental protection requirements, it is imminent to produce high-clean hydrocarbon fuels with ultra-low sulfur content. At present, most of the desulfurization of fuel oil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C10G25/00
CPCB01J20/22B01J20/28011B01J20/2808B01J20/28061B01J20/3085B01J20/3071C10G25/003C10G2300/202
Inventor 马和平陈姝晖张文祥
Owner XI AN JIAOTONG UNIV
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