Cd-MOF based on 4,4'-dicarboxydiphenyl ether and preparation method thereof

A technology of dicarboxydiphenyl ether and repeating unit is applied in the directions of non-active ingredient medical preparations, active ingredients-containing medical preparations, pharmaceutical formulas, etc. The effect of wide source of raw materials and mild reaction conditions

Active Publication Date: 2017-03-08
广东优农品科技有限公司
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This shortcoming greatly hinders the practical application of M

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  • Cd-MOF based on 4,4'-dicarboxydiphenyl ether and preparation method thereof
  • Cd-MOF based on 4,4'-dicarboxydiphenyl ether and preparation method thereof
  • Cd-MOF based on 4,4'-dicarboxydiphenyl ether and preparation method thereof

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Example Embodiment

[0038] Example 1

[0039] 1. Preparation of Cd-MOF based on 4,4’-dicarboxydiphenyl ether

[0040] The preparation method includes the following steps:

[0041] (1) Dissolve 4,4'-dicarboxydiphenyl ether (0.063g, 0.3mmol) in 10mL water under heating, and adjust the pH to 7-8 with NaOH;

[0042] (2) Dissolve dmbpy (0.028g, 0.15mmol) ligand in 5mL ethanol solution, then add Cd(NO 3 ) 2 ·4H 2 O (0.093g, 0.3mmol);

[0043] (3) Add the substances in steps 1 and 2 to a 23mL polytetrafluoroethylene reactor, keep at 130°C for 72 hours under autogenous pressure, and then reduce to room temperature at a rate of 5°C / h;

[0044] (4) Filter the product obtained in step 3, collect crystals, wash with absolute ethanol and dry to obtain colorless crystals (calculated yield based on oba: 48%).

[0045] 2. Identification of Cd-MOF based on 4,4’-dicarboxydiphenyl ether

[0046] Through the following elemental analysis, IR spectroscopy and X-ray single crystal diffraction analysis, the colorless crystal obtaine...

Example Embodiment

[0057] Example 2: Thermal stability and chemical stability experiment

[0058] In this example, the 4,4'-dicarboxydiphenyl ether-based Cd-MOF obtained in Example 1 was used to study the thermal stability and chemical stability.

[0059] 1. Research on the thermal stability of Cd-MOF based on 4,4’-dicarboxydiphenyl ether

[0060] Weigh 3 mg of the prepared Cd-MOF and the activated (vacuum dried at 130°C for 12h) Cd-MOF, and measure their thermal stability in the range of 25-800°C at a heating rate of 10°C / min.

[0061] The experimental results are as figure 2 Shown: when Cd-MOF is around 200℃, it loses 2 ethanol molecules and 4 lattice water molecules in the coordination environment, and the mass loss is about 15.1%; at 200-250℃, it loses one coordination water molecule, The mass loss is about 1.75%; after about 380°C, the frame structure of Cd-MOF begins to decompose and eventually becomes metal oxide CdO. The activated Cd-MOF can exist stably at 380°C.

[0062] 2. The chemical stabi...

Example Embodiment

[0068] Example 3

[0069] In this example, the 4,4'-dicarboxydiphenyl ether-based Cd-MOF obtained in Example 1 was used to study the encapsulation and sustained release of 5-fluorouracil. The specific research methods are as follows:

[0070] 1. Determination of the porosity of Cd-MOF based on 4,4’-dicarboxydiphenyl ether

[0071] At 77K, the activated Cd-MOF and the Cd-MOF vs. N after immersion for 3 days and 5-Fu loading were measured. 2 The adsorption isotherm.

[0072] N 2 The adsorption isotherm shows the type I characteristics of microporous materials ( Figure 5 a) The specific surface area of ​​the pores of the activated Cd-MOF is 775m by theoretical calculation 2 g -1 . At the same time, the specific surface area of ​​Cd-MOF is basically unchanged after being immersed in water for 3 days (775-740m 2 g -1 ), therefore, the porous structure of Cd-MOF is stable in water, indicating that the hydrophobic group methyl in the Cd-MOF framework is very close to the center of the cadm...

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Abstract

The invention relates to Cd-MOF based on 4,4'-dicarboxydiphenyl ether, wherein MOF is a cadmium metallic coordination polymer of which a repeating unit is [Cd2(oba)2(dmbpy)(H2O)].2(EtOH).4(H2O); oba in the chemical formula [Cd2(oba)2(dmbpy)(H2O)].2(EtOH).4(H2O) is 4,4'-dicarboxydiphenyl ether ligand; dmbpy is 3,3'-dimehtyl-4,4'-bipyridine; EtOH is an ethanol molecule. The Cd-MOF provided by the invention can be used as a drug carrier for effectively loading 5-fluorouracil, and can be also used as a gas adsorbing material for selectively adsorbing the molecule of a CO2 gas.

Description

technical field [0001] The present invention relates to microporous metal-organic frameworks (MOFs), in particular to a Cd-MOF based on 4,4'-dicarboxydiphenyl ether and a preparation method thereof. Background technique [0002] Due to the role of microporous metal-organic frameworks (MOFs) in gas adsorption and separation [1] ,catalytic [2] ,magnetic [3] , fluorescent probe [4] , drug loading and sustained release [5] And other aspects have potential application value, and have received extensive attention in the past ten years. However, some reports have shown that many cadmium or zinc-based MOFs are structurally unstable and rapidly lose their structural integrity and high specific surface area when exposed to air. [6] . This is due to the relatively weak metal-oxygen bonds within the framework that are easily attacked by water molecules and lose their structure [7] . This shortcoming greatly hinders the practical application of MOFs because moisture is ubiquitous...

Claims

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Application Information

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IPC IPC(8): C08G83/00A61K47/34A61K31/513
CPCA61K9/0002A61K31/513A61K47/34C08G83/008
Inventor 马德运郭海福覃亮雷佳眉谢佳敏朱致卫
Owner 广东优农品科技有限公司
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