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A nanoscale aluminum-based metal-organic framework material and its preparation method

An organic framework, nanoscale technology, applied in the fields of magnetism, nanotechnology, organic chemistry, etc.

Inactive Publication Date: 2016-03-16
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method usually forms large single crystals with larger particles, and it is difficult to obtain micron or nanoscale materials, and traditional inorganic aluminum sources are easily hydrolyzed to form aluminum hydroxide precipitation, making it difficult to efficiently and controllably synthesize nano / micron crystalline materials

Method used

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  • A nanoscale aluminum-based metal-organic framework material and its preparation method
  • A nanoscale aluminum-based metal-organic framework material and its preparation method
  • A nanoscale aluminum-based metal-organic framework material and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0022] Aluminum isopropoxide was used as the organic aluminum source (0.706g, 3.46mmol) and 1,4-BDC (0.287g, 1.73mmol) (molar ratio Al:1,4-BDC=2:1), and the weighed medicine and 5mL of water was mixed, stirred evenly, and placed in a polytetrafluoroethylene reactor. The experiment adopted a temperature-programmed method of 3°C / min. The reaction temperature was 210°C, and the holding time was 72 hours. After the reaction was completed, the temperature was lowered to room temperature and then taken out. The reaction solution was washed with deionized water and ethanol in sequence, and dried at room temperature to finally obtain a light yellow powder.

[0023] Take some samples for XRD characterization, such as figure 1 As shown, it can be seen that the synthesized product and the standard XRD spectrum (MichaelMaes, FrederikVermoortele, LucAlaerts, SarahCouck, ChristineE.A.Kirschhock, JoeriF.M.Denayer, and DirkE .DeVos, J.Am.Chem.Soc., 2010, 132(43), 15277–15285; Fajula and Gé...

Embodiment 2

[0026] Aluminum isopropoxide is used as the organic aluminum source (0.706g, 3.46mmol) and 1,4-BDC (0.287g, 1.73mmol), (molar ratio Al: 1,4-BDC = 2: 1), the weighed drug Mix it with 4mL water + 1mL ethanol, stir evenly, and place it in a polytetrafluoroethylene reactor. The experiment adopts the method of temperature programming at 3°C / min, the reaction temperature is 210°C, and the holding time is 72 hours. After the reaction was completed, the temperature was lowered to room temperature and then taken out. The reaction solution was washed with deionized water and ethanol in sequence, and dried at room temperature to finally obtain a light yellow powder. Take some samples for XRD characterization, such as figure 1 As shown, it can be seen that the synthesized product matches the MIL-53 (Al) standard XRD spectrum; from image 3 It can be seen that the products synthesized under this condition are still dominated by rod-like structures, but accompanied by the formation of nano...

Embodiment 3

[0028] Aluminum isopropoxide was used as the organic aluminum source (0.706g, 3.46mmol) and 1,4-BDC (0.287g, 1.73mmol) (molar ratio Al:1,4-BDC=2:1), and the weighed medicine and 2.5mL water + 2.5mL ethanol were mixed, stirred evenly, and placed in a polytetrafluoroethylene reactor. The experiment adopted a 3°C / min temperature programming method, the reaction temperature was 210°C, and the holding time was 72 hours. After the reaction was completed, the temperature was lowered to room temperature and then taken out. The reaction solution was washed with deionized water and ethanol in sequence, and dried at room temperature to finally obtain a light yellow powder.

[0029] Some samples were taken for XRD characterization, from figure 1 It can be seen that the synthesized products are consistent with the MIL-53 (Al) standard XRD spectrum, the crystallinity is good, and the samples are pure. And by comparing the XRD spectra of the two, it can be seen that the (1,0,1) plane is wea...

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Abstract

A nanoscale aluminium-based metal-organic framework structure material and its preparation method belong to the field of new material technology. The preparation method comprises the following steps: weighing an organic aluminum source and 1,4-terephthalic acid and putting them in a teflon reaction vessel, adding a solvent, and uniformly mixing by stirring, ultrasound or concussion, wherein the molar ratio of aluminium in the organic aluminum source to 1,4-terephthalic acid is 1.5-4:1 and the solvent is a mixture of water and ethanol which accounts for 0-50% (vol) of the mixed solvent; sealing the reaction vessel, reacting at 200-220 DEG C for 60-80 hours, and cooling to room temperature; and filtering the above reaction liquid, washing precipitates with deionized water and ethanol respectively, drying at room temperature to obtain a light yellow powdery product, namely the nanoscale aluminium-based metal-organic framework structure material. By the above method, release speed of aluminium ion can be controlled effectively, and controllable synthesis of the MIL-53(Al) material can be realized at micro-level by changing the aluminium source.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a nanoscale aluminum-based metal-organic framework structure material and a preparation method thereof. Background technique [0002] Metal-organic framework materials are a kind of coordination polymers that have been developed rapidly in recent decades. Usually, metal ions or metal ion clusters are used as connection points, and organic ligands are used as three-dimensional structures in space. They are zeolites and carbon nanotubes. Another important new class of porous materials. Compared with traditional porous materials, metal-organic framework materials not only have the characteristics of infinite extension, but also exist metal-heteroatom bonds. Based on the above two structural characteristics, metal-organic framework materials also have corresponding physical and chemical properties, such as good thermal stability due to their stable spatial structur...

Claims

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Application Information

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IPC IPC(8): C07F5/06B01J31/22B01J20/22H01L51/54H01F1/42B82Y40/00
Inventor 戴昉纳张建光刘丹丹王文范卫东
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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