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N, n'-bis(salicyloyl) terephthalic hydrazide manganese polymer and its synthesis method and application

A technology of manganese phthaloyl hydrazide and manganese phthaloyl hydrazide, which is applied in the field of N,N'-diterephthalic hydrazide manganese polymers and their synthesis, can solve the problems of few three-dimensional MOFs and achieve good Adsorption, low cost, good repeatability

Active Publication Date: 2020-11-13
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these polymers have a one-dimensional or two-dimensional structure, and there are few three-dimensional MOFs constructed by the ligand itself. So far, no N,N'-bis(salicyloyl)terephthalic hydrazide (L) Three-dimensional polymers with holes synthesized as ligands [Mn III 10 mn II 5 (L) 6 (μ 3 -O) 2 (Py) 12 (H 2 O) 3 ] n related reports

Method used

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  • N, n'-bis(salicyloyl) terephthalic hydrazide manganese polymer and its synthesis method and application
  • N, n'-bis(salicyloyl) terephthalic hydrazide manganese polymer and its synthesis method and application
  • N, n'-bis(salicyloyl) terephthalic hydrazide manganese polymer and its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh the ligand (0.025mmol, 0.0108g), Mn(OAc) 2 4H 2 O (0.05mmol, 0.0125g) and NaN 3 (0.01mmol, 0.065g,), they were added to a Pyrex tube with a length of 22cm and one end was closed, then a mixed solvent consisting of 0.9mLDMF and 0.3mL methanol was added, and 4 drops of pyridine were added dropwise, and shaken evenly (at this time The pH of the solution = 6.1). Vacuum the Pyrex tube, seal the other port, place it at 60°C for 72 hours, take it out, then place it at 80°C for 120 hours, take it out, cool it to room temperature, and black quadrangular block crystals precipitate out. Yield: 60%. Elemental analysis (%), theoretical value: C, 53.73; H, 3.94; N, 12.00; experimental value: C, 53.80; H, 3.90; N, 12.05.

[0035] The product obtained in Example 1 is characterized:

[0036] 1) Infrared characterization:

[0037] Use American Nicolet 360FT-IR type Fourier transform infrared spectrometer (KBr tablet), carry out infrared analysis to the product that present em...

Embodiment 2

[0063] Repeat Example 1, the difference is:

[0064] 1) N,N'-bis(salicyloyl)terephthalic hydrazide, Mn(OAc) 2 4H 2 O and NaN 3 The ratio of the amount of substances is changed to 1:3:0.2;

[0065] 2) In the mixed solvent, change the volume ratio of DMF and methanol to 2:1;

[0066] 3) Adjust the pH value of the solution to 6.3.

[0067] The Pyrex tube was taken out and cooled to room temperature, and black quadrangular block crystals were precipitated at the bottom of the Pyrex tube. Yield 56%.

[0068] The resulting product was characterized for its structure, and it was determined that the product was the target product [Mn III 10 mn II 5 (L) 6 (μ 3 -O) 2 (Py) 12 (H 2 O) 3 ] n , where L represents N, N'-bis(salicyloyl) terephthalic hydrazide, which removes six protons during the coordination process to form a negative charge with six units.

[0069] Characterization of the magnetic properties of the obtained product shows that there is antiferromagnetic exch...

Embodiment 3

[0072] Repeat Example 1, the difference is:

[0073] 1) N,N'-bis(salicyloyl)terephthalic hydrazide, Mn(OAc) 2 4H 2 O and NaN 3 The ratio of the amount of substances is changed to 1:4:1;

[0074] 2) In the mixed solvent, change the volume ratio of DMF and methanol to 1:1;

[0075] 3) Put the mixed solution with adjusted pH value at 40° C. for 48 hours, and then at 80° C. for 24 hours.

[0076] The Pyrex tube was taken out and cooled to room temperature, and black quadrangular block crystals were precipitated at the bottom of the Pyrex tube. Yield 55%.

[0077] The resulting product was characterized for its structure, and it was determined that the product was the target product [Mn III 10 mn II 5 (L) 6 (μ 3 -O) 2 (Py) 12 (H 2 O) 3 ] n , where L represents N,N'-bis(salicyloyl)terephthalic hydrazide, which removes six protons during the coordination process to form a negative charge with six units.

[0078] Characterization of the magnetic properties of the obta...

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Abstract

The invention discloses an N,N'-bis(salicyloyl)terephthaloyl hydrazine manganese polymer as well as a synthesis method and application thereof. A chemical formula of the polymer is [Mn<III>10Mn<II>5(L)6(mu 3-O)2(Py)12(H2O)3]n, wherein L represents N,N'-bis(salicyloyl)terephthaloyl hydrazine, and six protons of the L are removed in a process of participating in a coordination process, so that negative charge with six units is formed. The synthesis method of the polymer comprises the following steps: taking the N,N'-bis(salicyloyl)terephthaloyl hydrazine, Mn(OAc)2.4H2O and NaN3, and dissolving by utilizing a mixed solvent; regulating the pH (Potential of Hydrogen) of a system by utilizing pyridine; firstly, enabling the system to react under a relatively low temperature condition; then enabling the system to react under a relatively high temperature condition; cooling a reactant and separating out a crystal to obtain the polymer. According to the polymer disclosed by the invention, manganese ions in a polymer molecule have an anti-ferromagnetic exchange effect, so that the polymer has a very good adsorption effect on carbon dioxide gas.

Description

technical field [0001] The invention relates to a manganese N,N'-di(salicyloyl)terephthaloyl hydrazide polymer, a synthesis method and an application thereof, and belongs to the technical field of magnetic materials. Background technique [0002] Metal-organic frameworks (MOFs) functional coordination polymers are a class of organic-inorganic hybrid materials that are connected by metal ions or metal cluster units through organic ligands with coordination bonds. Recognition, heterogeneous catalysis, new optoelectronic devices, magnetic materials, biomedicine and many other aspects have shown unique properties, and are one of the frontier research fields in the field of inorganic chemistry. As a class of multidentate ligands containing O and N electron donors, the number of protons removed by N-acylated salicylhydrazide ligands is different under different reaction conditions, forming anions with different valence states, and the coordination modes are flexible and diverse. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C08L87/00B01J20/26B01J20/30B01D53/02
CPCB01D53/02B01D2253/202B01D2257/504B01J20/262C08G83/008C08L87/00Y02C20/40Y02P20/151
Inventor 邹华红凌晓梁福沛
Owner GUANGXI NORMAL UNIV