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A kind of highly thermally stable porous zinc-based MOF material and its preparation method and application

A high thermal stability, zinc-based technology, applied in the direction of luminescent materials, analytical materials, material excitation analysis, etc., can solve the problems of unpredictable topological structure performance, poor thermal stability of MOF, etc., and achieve mild preparation conditions and thermal stability high effect

Active Publication Date: 2022-04-05
CHONGQING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the microscopic reaction process, topological structure, and performance are difficult to predict, and most porous MOFs have poor thermal stability, it is a challenging task to prepare porous MOFs with novel topological structures and high thermal stability.
On the other hand, flexible or semi-rigid organofunctional ligands generally only produce non-porous or interpenetrating dense structures, so the preparation of porous MOFs based on semi-rigid organofunctionality is a challenging subject.

Method used

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  • A kind of highly thermally stable porous zinc-based MOF material and its preparation method and application
  • A kind of highly thermally stable porous zinc-based MOF material and its preparation method and application
  • A kind of highly thermally stable porous zinc-based MOF material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take the material according to the following specific mass or volume: H 3 tcpb (12.1mg, 0.025mmol), bpeb (8.5mg, 0.03mmol), Zn (NO 3 ) 2 ·6H 2 O (30.0 mg, 0.1 mmol), CH 3 CN (5mL), H 2 O (5mL), HNO 3 solution (20 μL, 7 mol / L, 0.14 mmol). Put the above material in 25mL polytetrafluoroethylene liner, stir for about 0.5h, seal it in a stainless steel reaction kettle, place the reaction kettle in an electric blast oven and raise the temperature to 140°C, after 4 days of reaction, cool naturally to room temperature, A bulk crystal sample was obtained, which was filtered from the mother liquor, washed with distilled water, and dried naturally in air at room temperature.

[0037] To the prepared crystal sample, carry out powder diffraction test with Shimadzu XRD-6100 type X-ray diffractometer (see image 3 , abscissa—angle; ordinate—diffraction intensity), the peaks of the test spectrum and the peaks of the crystal structure simulation spectrum (software Mercury) can be...

Embodiment 2

[0053] Take the material according to the following specific mass or volume: H 3 tcpb (12.1mg, 0.025mmol), bpeb (8.5mg, 0.03mmol), Zn(NO 3 )2 ·6H 2 O (30.0 mg, 0.1 mmol), CH 3 CN (5mL), H 2 O (5mL), HNO 3 solution (10 μL, 7 mol / L, 0.07 mmol). Put the above material in 25mL polytetrafluoroethylene liner, stir for about 10min, seal it in a stainless steel reaction kettle, place the reaction kettle in an electric blast oven and raise the temperature to 160°C, react for 4 days, and naturally cool to room temperature to obtain Block crystal samples were filtered from the mother liquor, washed with distilled water, and dried naturally in air at room temperature.

[0054] Product powder X-ray diffraction characterization, obtains data similar to embodiment 1 (see image 3 ). It shows that the crystal structure prepared by Example 2 does not change, and the product has a higher purity. This embodiment is repeated many times, and Zn is actually obtained 3 -The quality of MOF i...

Embodiment 3

[0056] Take the material according to the following specific mass or volume: H 3 tcpb (12.1mg, 0.025mmol), bpeb (8.5mg, 0.03mmol), Zn(NO 3 ) 2 ·6H 2 O (30.0 mg, 0.1 mmol), CH 3 CN (5mL), H 2 O (5mL), HNO 3 (30 μL, 7 mol / L, 0.21 mmol). Put the above material in 25mL polytetrafluoroethylene liner, stir for about 20min, seal it in a stainless steel reaction kettle, place the reaction kettle in an electric blast oven and raise the temperature to 120°C, react for 4 days, and naturally cool to room temperature to obtain Block crystal samples were filtered from the mother liquor, washed with distilled water, and dried naturally in air at room temperature.

[0057] Product powder X-ray diffraction characterization, obtains data similar to embodiment 1 (see image 3 ). It shows that the crystal structure prepared by Example 3 does not change, and the product has a higher purity. This embodiment is repeated many times, and Zn is actually obtained 3 -The mass of MOF is kept at ...

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Abstract

The invention provides a highly thermally stable porous zinc-based MOF material and its preparation method and application. The general chemical formula is [Zn 3 (tcpb) 2 (bpeb)] n , belongs to the triclinic system, the space group is P‑1, and the unit cell parameter component tcpb 3‑ is a semi-rigid ternary organic carboxylic acid H 3 tcpb removes 3 protons, H 3 tcpb is shown in formula I; the component bpeb is shown in formula II. The triple interpenetrated porous MOF material provided by the present invention has high thermal stability and can exist stably in solvents such as water and acetonitrile; the preparation conditions are mild and the yield is the highest It can reach 76.3%; the theoretical porosity is 31.3%, and the calculated density is 1.173g / cm 3 , is a typical porous material with low density; as a luminescent material, it can be used to identify the commonly used high boiling point solvent DMA, and to identify Fe 3+ Qualitative and quantitative fluorescence detection.

Description

technical field [0001] The invention belongs to the field of advanced porous materials, in particular to a highly thermally stable triple interpenetrating porous zinc-based metal-organic framework Zn 3 -MOF new materials and their preparation methods and applications. Background technique [0002] Generally speaking, porous materials are solid substances with gaps, such as sponges, crater zeolites, etc.; limited by natural resources, artificial synthesis has become an important source of porous new materials. Since the middle of the last century, the inorganic porous Materials (such as silicate molecular sieves, aluminum phosphate AlPO-5, etc.), metal-organic frameworks (Metal-Organic Frameworks, MOFs, such as MOF-5) and porous organic framework materials (Porous Organic Frameworks, POFs) stage, these new materials It has been extensively researched and applied in gas storage, catalytic reaction, sensor, drug sustained release, etc. [0003] The most favored MOFs are organ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06G01N21/6428G01N2021/6432C09K2211/1425C09K2211/1433C09K2211/1466
Inventor 黄坤林夏刚陈新张愿胡敏吴越
Owner CHONGQING NORMAL UNIVERSITY
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