A kind of cd-mof based on 4,4'-dicarboxy diphenyl ether and preparation method thereof
A technology of dicarboxydiphenyl ether and repeating units, applied in medical preparations with non-active ingredients, medical preparations containing active ingredients, pharmaceutical formulations, etc., can solve problems that hinder the practical application of MOFs materials, and achieve easy access, The effect of mild reaction conditions and high purity
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Embodiment 1
[0039] 1. Preparation of Cd-MOF based on 4,4'-dicarboxydiphenyl ether
[0040] The preparation method comprises the following steps:
[0041] (1) Dissolve 4,4'-dicarboxydiphenyl ether (0.063g, 0.3mmol) in 10mL water by heating, and adjust the pH value 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 into a 23mL polytetrafluoroethylene reactor, keep at 130°C for 72 hours under autogenous pressure, and then cool down to room temperature at a rate of 5°C / h;
[0044] (4) The product obtained in step 3 was filtered, and the crystals were collected, washed with absolute ethanol and dried to obtain colorless crystals (calculated yield according to oba: 48%).
[0045] 2. Identification of Cd-MOF based on 4,4’-dicarboxydiphenyl ether
[0046] Through the following elemental analysis, IR spectrum and X-ray single crystal diffraction analys...
Embodiment 2
[0057] Embodiment 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 thermal stability and chemical stability.
[0059] 1. Research on thermal stability of Cd-MOF based on 4,4'-dicarboxydiphenyl ether
[0060] Weighed 3 mg of the prepared Cd-MOF and the activated Cd-MOF (vacuum dried at 130 °C for 12 h), and measured its thermal stability in the range of 25-800 °C at a heating rate of 10 °C / min.
[0061] Experimental results such as figure 2 Shown: Cd-MOF loses 2 ethanol molecules and 4 lattice water molecules in the coordination environment at about 200°C, and the mass loss is about 15.1%; at 200-250°C, one coordination water molecule is lost, The mass loss is about 1.75%; after about 380°C, the framework structure of Cd-MOF begins to decompose, and finally becomes the metal oxide CdO. The activated Cd-MOF can exist stably at 380°C.
[0062] 2. Chemical sta...
Embodiment 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 porosity of Cd-MOF based on 4,4'-dicarboxydiphenyl ether
[0071] At 77K, the activated Cd-MOF and the Cd-MOF after 3 days of water immersion and 5-Fu loading were measured against N2 isothermal adsorption.
[0072] N 2 The adsorption isotherm shows a type I characteristic of the microporous material ( Figure 5 a), through theoretical calculation, the specific surface area of the pores of the activated Cd-MOF is 775m 2 g -1 . At the same time, the specific surface area of Cd-MOF remained basically unchanged after being immersed in water for 3 days (775-740m 2 g -1 ), so the porous structure of Cd-MOF is stable in water, indicating that the hydrophobic group methyl group in the Cd-MOF framework is very close to the cadmium met...
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