Preparation method of metal organic framework/nanofiber with bead-like structure

A metal-organic framework and nanofiber technology, which is applied in the direction of fiber type, fiber treatment, fiber chemical characteristics, etc., can solve the problem of not controlling the crystal structure and morphology well, maintaining the polyhedral structure of MOF derivatives, and reducing the utilization rate of metal salts and other problems, to achieve the effect of solving difficult integrated utilization, improving physical and chemical properties, and improving utilization efficiency

Active Publication Date: 2021-06-18
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

However, the current way of combining ZIF and nanofibers is generally to mix and spin metal salts and polymer molecules, resulting in part of the metal salts being wrapped inside the fibers by the polymers and unable to combine with organic ligands, resulting in a decrease in the utilization of the metal salts. Very good control of crystal structure and morphology, not conducive to maintaining the polyhedral structure of MOF derivatives

Method used

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  • Preparation method of metal organic framework/nanofiber with bead-like structure
  • Preparation method of metal organic framework/nanofiber with bead-like structure
  • Preparation method of metal organic framework/nanofiber with bead-like structure

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preparation example Construction

[0024] The invention provides a method for preparing a metal organic framework / nanofiber with a beaded structure.

[0025] Such as figure 1 As shown, the method includes the following steps:

[0026] (1) Preparation of metal / PAN spinning solution: first, add DMF organic solvent in a glass bottle, under the condition of uniform stirring, add metal salt to the solvent, after the metal salt is dissolved, slowly add PAN, at a speed of 200 Stir evenly in a magnetic stirrer at ~1000rpm for 8~24h to obtain metal / PAN spinning solution;

[0027] (2) Synthesis of metal / PAN nanofibers by electrospinning technology: transfer the metal / PAN spinning solution obtained in step (1) to the syringe, adjust the advancing speed, receiving distance and electrospinning voltage, and perform double-needle spinning, The metal / PAN nanofiber membrane is obtained by electrospinning technology, and the obtained nanofiber membrane is dried in a vacuum oven at 50-100°C for 12-24 hours;

[0028] (3) Obtain...

Embodiment 1

[0032] A ZIF / PAN nanofiber electrode material with beaded structure based on candied haws and a preparation method thereof, comprising the following steps:

[0033] ZIF-67 / PAN nanofiber composites with "dotted" distribution were prepared by one-time growth of in-situ metal salts:

[0034] (1) Preparation of Co 2+ / PAN / spinning solution: 0.5g cobalt nitrate (Co(NO 3 ) 2 ·6H 2 O) and 0.9g PAN were dissolved in 10mL DMF, stirred evenly at room temperature for 12h to obtain Co 2+ / PAN spinning solution;

[0035] (2) Preparation of Co 2+ / PAN / nanofiber composite film: the resulting Co 2+ The / PAN spinning solution was transferred to two 5mL syringes for double-needle spinning, the advancing speed was 0.08mm / min, the receiving distance was 15cm, and the voltage was 17kV. The obtained nanofibers were dried in a vacuum oven at 80 °C for 12 h to obtain Co 2+ / PAN / nanofiber membrane;

[0036] (3) Preparation of a methanol solution of 2-methylimidazole: add 6.6 g of 2-methylimid...

Embodiment 2

[0039] A grape-type beaded structure ZIF / PAN nanofiber material and a preparation method thereof, comprising steps as follows:

[0040] The ZIF-67-ZIF-8 bimetallic ZIF material with "dotted" distribution was prepared by in situ mixed metal salt growth method:

[0041] (1) Preparation of Co 2+ -Zn 2+ / PAN spinning solution: 0.25g Co(NO 3 ) 2 ·6H 2 O, 0.25g zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) and 0.9g PAN were dissolved in 10mL DMF, stirred evenly at room temperature for 12h to obtain Co 2+ -Zn 2+ / PAN spinning solution;

[0042] (2) Preparation of Co 2+ -Zn 2+ / PAN nanofiber composite film: the resulting Co 2+ -Zn 2+ The / PAN spinning solution was transferred to two 5mL syringes for double-needle spinning, the advancing speed was 0.08mm / min, the receiving distance was 15cm, and the voltage was 17kV. The obtained nanofibers were dried in a vacuum oven at 80 °C for 12 h to obtain Co 2+ -Zn 2+ / PAN nanofiber membrane;

[0043] (3) Preparation of a methanol solution...

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Abstract

The invention provides a preparation method of a metal organic framework/nanofiber with a bead-like structure, and belongs to the technical field of nano material preparation. The method includes the following steps: firstly, bridging metal salt nodes on the surfaces of metal/PAN nanofibers with 2-methylimidazole in a solution for coordination, and generating ZIF particles distributed along the nanofibers in an in-situ one-time growth manner; and then adding a metal salt solution, wherein metal ions enriched on the surfaces of the fibers and the organic ligands are subjected to a strong cross-linking effect, and a ZIF/PAN nanofiber composite material with a layered heterostructure is obtained through in-situ secondary growth. The method can promote the uniform growth of ZIF particles along the orientation of the nanofibers, so that more crystal face positions are exposed, the crystal face utilization of the ZIF is maximized, the specific surface area and the activity are greatly improved, and the application field of the ZIF is expanded. The method is simple, the process is controllable, the problems of MOF particle aggregation, MOF derivative structure collapse and the like are greatly solved, the method can be applied to the field of fuel cell catalysis, and the catalytic activity and stability are improved.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a preparation method of a metal organic framework / nanofiber with a beaded structure. Background technique [0002] Metal-organic framework (MOF) is a periodic porous material constructed by self-assembly of metal ions and organic linkers. It has designable tailoring, rich pore structure and high specific surface area. Among them, zeolite imidazolate framework material (ZIF) is a kind of MOF material with imidazole and its derivatives as ligands, which combines the advantages of zeolite and MOF materials, such as: outstanding structural stability and adjustable function In addition, carbon materials and metal compounds prepared with ZIF as precursors have excellent electrical conductivity, rich pore structure and more active sites of metals and heteroatoms. Therefore, ZIF materials and their derivatives are widely used in gas sensing , catalysis, energy storage a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M15/37D01F6/54D01F1/10D04H1/728D06M101/28
CPCD06M15/37D01F6/54D01F1/10D04H1/728D06M2101/28
Inventor 张秀玲李从举郭仕权李曈
Owner UNIV OF SCI & TECH BEIJING
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