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Rapid synthesis method of cyclodextrin-metal organic framework material

A metal-organic framework and cyclodextrin technology, which is applied in the direction of non-active components of polymer compounds, can solve problems such as difficult industrial production and long reaction time, and achieve a good protective effect

Active Publication Date: 2017-09-12
SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

But above-mentioned method reaction time is long, continues several days, is difficult to industrialized production

Method used

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  • Rapid synthesis method of cyclodextrin-metal organic framework material
  • Rapid synthesis method of cyclodextrin-metal organic framework material
  • Rapid synthesis method of cyclodextrin-metal organic framework material

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preparation example Construction

[0149] A preferred preparation method based on cyclodextrin-metal organic framework includes the following steps: after mixing the metal salt solution with the cyclodextrin aqueous solution, pre-adding a part of organic solvent, at a certain temperature (higher than room temperature), passing solvent vapor Diffusion method, react for a certain period of time, and then add a size regulator to obtain the metal organic framework material based on cyclodextrin; or mix the metal salt solution with the cyclodextrin aqueous solution, add a part of the organic solvent in advance, and use solvent heat / microwave / Ultrasonic vibration of the reaction medium, so that the reactants react quickly, and after a certain period of time, a size regulator is added to obtain the cyclodextrin-based metal-organic framework material.

[0150] Wherein, the cyclodextrin includes α-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, hydroxypropyl-β-cyclodextrin, sulfobutyl-β-cyclodextrin, methyl-β - cyclodext...

Embodiment 1

[0174] Preparation of first-stage CD-MOF crystals by solvothermal evaporation

[0175] Dissolve 163.0 mg of γ-CD and 56.0 mg of KOH mixture (the molar ratio of γ-CD and KOH is 0.125) in 5 mL of water, sonicate for 10 minutes to fully dissolve, and filter through a 0.45 μm filter. Then pre-add 0.5mL methanol to the mixed solution of γ-CD and KOH, heat the methanol in a closed container at 50°C (the whole closed container is heated), and evaporate the methanol vapor into the mixed system of γ-CD and KOH. After 6 hours of reaction, a small amount of crystals began to be produced. After 24 hours of reaction, a large amount of colorless transparent crystals were obtained. The supernatant was discarded, centrifuged at 3000rpm for 5 minutes, washed with ethanol (10mL×3), and the obtained crystals were vacuum-dried at 50°C for 12 hours. DEK's first-stage CD-MOF crystals (CD-MOF I), which can be stored for a long time, have a size of 40-500 μm, such as figure 1 and Figure 5 , and th...

Embodiment 2

[0177] Preparation of second-stage micron-sized CD-MOF crystals by solvothermal evaporation

[0178]Weigh 163.0 mg of γ-CD and 56.0 mg of KOH mixture (the molar ratio of γ-CD and KOH is 0.125) and dissolve it in 5 mL of water, sonicate for 10 minutes to fully dissolve, and filter through a 0.45 μm filter membrane. Then pre-add 0.5mL methanol to the mixed solution of γ-CD and KOH, heat the methanol in a closed container at 50°C (the whole closed container is heated), and evaporate the methanol vapor into the mixed system of γ-CD and KOH. After reacting for 6 hours, take out the supernatant, add PEG 20000 at the ratio of 8mg / mL supernatant, let stand for half an hour, centrifuge at 3000rpm for 5min, wash with ethanol (10mL×2) and dichloromethane (10mL×2) respectively After washing, the resulting crystals were vacuum-dried at 50°C for 12 hours to obtain the second-stage micron-sized CD-MOF crystals (CD-MOF II) that can be stored for a long time, with a size of 1-10 μm, such as ...

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Abstract

The invention provides a rapid synthesis method of a cyclodextrin-metal organic framework material, and concretely provides a method for rapidly synthesizing a cyclodextrin (CD)-based cyclodextrin-metal organic framework (CD-MOFs) material by using a solvothermal volatilization / solvothermal / microwave / ultrasonic wave assisting technology. The method comprises the following steps: preparing an aqueous solution of metal salt and cyclodextrin, and adding a part of an organic solvent in advance; carrying out the solvothermal volatilization / solvothermal / microwave / ultrasonic wave assisting technology to rapidly react reactants; and taking the obtained supernatant after the reaction is carried out for a certain time, and adding a dimension regulator in order to obtain the cyclodextrin-metal organic framework material. The method has the advantages of fastness, simplicity, safety, high yield, cheap and easily available raw materials and solvents, facilitation of industrial production, and wide application prospect of the obtained CD-MOFs in the fields of catalysis, adsorption, drug carriers and the construction of nanometer devices.

Description

technical field [0001] The invention relates to the field of biomaterials, and more particularly relates to a method for rapidly synthesizing cyclodextrin-based cyclodextrin-metal organic framework materials using solvothermal volatilization / solvothermal / microwave / ultrasonic assisted methods. Background technique [0002] Metal-organic frameworks (MOFs) are crystalline materials in which inorganic metal centers are connected by organic bridging ligands through coordination bonds to form an infinitely extended network structure. Due to the ultra-high porosity and huge specific surface area of ​​MOFs, as well as its structure composed of different inorganic and organic components, its structure is diverse and adjustable, making MOFs have potential in many fields such as gas storage, catalysis, and drug carriers. Value. [0003] Cyclodextrin is a general term for a series of cyclic oligosaccharides produced by amylose under the action of glucosyltransferase, usually containing...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08B37/16A61K47/40
CPCA61K47/40C08B37/0012C08G83/008B01J20/226B01J20/24B01J20/3078B01J20/3085
Inventor 张继稳刘波涛李海燕吕娜娜伍丽郭桢
Owner SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI
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