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Supramolecular microporous framework material supported by functionalized caged borane anion pillars and its preparation method and application

A technology of anion column and frame material, which is applied in separation methods, chemical instruments and methods, adsorption purification/separation, etc., can solve the problems that need to be studied in application, achieve good structural stability, and realize the effect of selective separation

Active Publication Date: 2020-06-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of caged borane anions with functional group modifications to construct porous framework materials has never been reported, and its application remains to be studied.

Method used

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  • Supramolecular microporous framework material supported by functionalized caged borane anion pillars and its preparation method and application
  • Supramolecular microporous framework material supported by functionalized caged borane anion pillars and its preparation method and application
  • Supramolecular microporous framework material supported by functionalized caged borane anion pillars and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In a 50mL round-bottomed flask, 242mg (1mmol) of Cu(NO 3 ) 2 ·3H 2 O and 314mg (1mmol) of Na 2 B 12 H 11 I was dissolved in 10 ml of water. In another 25 mL round bottom flask, 360 mg (2 mmol) of 4,4'-dipyridine acetylene was dissolved in 15 mL methanol. The methanol solution was slowly added to the aqueous solution and stirred at 25°C for 24 hours to obtain a grayish purple solid precipitate, which was filtered and washed with methanol. Replace the above solid in anhydrous methanol 3 times with an interval of 12 hours each time to remove the water molecules in the material pores, and then vacuum and degas at 70℃ for 10 hours to obtain activated functionalized cage-like dodecaborane anion supramolecules Microporous frame material, named BSF-20.

[0036] The self-assembly behavior of BSF-20 is as figure 1 Shown. First, the metallic copper ion is coordinated to four different pyridine rings in the horizontal direction, and to the B-H of two different caged boranes in the ...

Embodiment 2

[0054] In a 50mL round-bottomed flask, 242mg (1mmol) of Cu(NO 3 ) 2 ·3H 2 O and 314mg (1mmol) of Na 2 B 12 H 11 I was dissolved in 10 ml of water. In another 25 mL round bottom flask, 312 mg (2 mmol) of bipyridine was dissolved in 15 mL methanol. The methanol solution was slowly added to the aqueous solution and stirred at 25°C for 2 hours to obtain a grayish purple solid precipitate, which was filtered and washed with methanol. Replace the above solid in anhydrous methanol 3 times with an interval of 12 hours each time to remove the water molecules in the material pores, and then vacuum degas and activate at 80°C for 5 hours to obtain activated functionalized caged dodecaborane anion supramolecules The microporous frame material is named BSF-21.

Embodiment 3

[0056] In a 50mL round-bottomed flask, 242mg (1mmol) of Cu(NO 3 ) 2 ·3H 2 O and 314mg (1mmol) of Na 2 B 12 H 11 I was dissolved in 10 ml of water. In another 25 mL round bottom flask, 464 mg (2 mmol) of bipyridinebenzene was dissolved in 15 mL of methanol. The methanol solution was slowly added to the aqueous solution and stirred at 25°C for 48 hours to obtain a grayish purple solid precipitate, which was filtered and washed with methanol. Replace the above solid in anhydrous methanol 3 times with an interval of 8 hours each time to remove the water molecules in the material pores, and then vacuum degas and activate for 10 hours at 100°C to obtain activated functionalized cage-like dodecaborane anion supramolecules The microporous frame material is named BSF-22.

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Abstract

The invention discloses a functional cage borane anion-pillared supramolecular microporous framework material. Metal Cu<2+> ions coordinate with organic nitrogen-containing ligand L to form a two-dimensional plane structure, which is then bridged to iodine-substituted functional cage dodecaborane anion[B12H11I]<2-> to form a three-dimensional layered columnar framework structure. The functional cage borane anion-pillared supramolecular microporous framework material provided by the invention can be used for selective purification of methane, specifically in high selective adsorption and separation of propylene / methane, propane / methane, ethane / methane, ethylene / methane, and acetylene / methane, and the obtained high purity methane gas and recovered low-carbon hydrocarbon of C2-C3 can be usedfor selective adsorption and separation of natural gas, biogas, pyrolysis gas and other industrial mixed gas containing a lot of methane.

Description

Technical field [0001] The invention relates to the technical field of synthesis of porous materials and gas adsorption and separation, in particular to a functionalized cage-shaped borane anion pillared supramolecular microporous framework material and a preparation method and application thereof. Background technique [0002] Adsorption separation is a relatively energy-saving and efficient separation technology, which has the advantages of simple operation and high removal depth. With the development of porous materials such as molecular sieves, porous polymers (PCPs), and metal-organic frameworks (MOFs), adsorption and separation technology has received widespread attention in recent years, but traditional adsorbents have separation options Shortcomings such as low performance and insufficient processing capacity. Designing a new type of adsorbent to improve adsorption capacity and selectivity is the key to the application of adsorption separation technology to gas separatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/02C10L3/10C08G83/00C07C7/12C07C9/04
CPCB01D53/02B01D2256/245B01D2257/7022B01J20/226B01J2220/4806B01J2220/4812C07C7/12C08G83/008C10L3/10C07C9/04Y02P30/40
Inventor 邢华斌张袁斌崔希利赵宁
Owner ZHEJIANG UNIV
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