Zirconium-based metal organic frameworks UiO-66 and application thereof

An organic framework, uio-66 technology, applied in the direction of analysis of materials, other chemical processes, preparation of test samples, etc., to achieve the effect of wide application range, reliable measurement results, and simple operation

An organic framework, uio-66 technology, applied in the direction of analysis of materials, other chemical processes, preparation of test samples, etc., to achieve the effect of wide application range, reliable measurement results, and simple operation

CN108854967AActive Publication Date: 2018-11-23HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Zirconium-based metal organic frameworks UiO-66 and application thereof
  • Zirconium-based metal organic frameworks UiO-66 and application thereof
  • Zirconium-based metal organic frameworks UiO-66 and application thereof

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preparation example Construction

[0040] A zirconium-based metal-organic framework material UiO-66, the preparation method of which comprises the following steps:

[0041] Step A, use acetic acid of 4.5~72mmoL, 30mL of N,N-dimethylformamide (DMF), the ratio of the terephthalic acid of 0.45mmoL according to every 0.45mmoL zirconium tetrachloride, zirconium tetrachloride and acetic acid Dissolve in N,N-dimethylformamide, add terephthalic acid and stir evenly to obtain a transparent mixed reaction solution.

[0042] Step B. Transfer the mixed reaction solution to a polytetrafluoroethylene-lined reactor, seal the reactor and place it in an oven at 120°C for 7 to 24 hours; cool to room temperature after the reaction, And carry out solid-liquid separation to remove the solvent, and then wash and dry the solid obtained after solid-liquid separation, so as to prepare regular octahedral zirconium-based metal organic framework material UiO-66 with a particle size of 500-600 nm.

[0043] Among them, the above steps use ...

Embodiment 1

[0068] A kind of UiO-66 liquid binding phase, its preparation method comprises the following steps:

[0069] Step a. Dissolve 0.45mmol of zirconium tetrachloride and 72mmol of acetic acid in 30mL of N,N-dimethylformamide, add 0.45mmol of terephthalic acid and stir evenly to obtain a transparent mixed reaction solution.

[0070] Step b. Transfer the mixed reaction solution to a reaction kettle with a polytetrafluoroethylene liner of 50mL, seal the reaction kettle and place it in an oven at 120°C for 24 hours; cool to room temperature after the reaction, and centrifuge Filter to remove the solvent, and then use N,N-dimethylformamide to wash the solid obtained after centrifugal filtration to wash off unreacted solutes, and then use methanol for 3 days of activation treatment at 60°C. The N,N-dimethylformamide in the pore structure of the product UiO-66 was removed by replacement, methanol was removed by centrifugation, and then vacuum-dried at 60°C for 12 hours to obtain a regula...

Embodiment 2

[0091] A UiO-66 liquid binding phase, the preparation method of which is basically the same as that of the UiO-66 liquid binding phase in Example 1 of the present invention, the only difference being that in step a, in Example 2 of the present invention, 0.45mmoL Zirconium tetrachloride and 4.5mmol of acetic acid were dissolved in 30mL of N,N-dimethylformamide, and 0.45mmol of terephthalic acid was added and stirred evenly to obtain a transparent mixed reaction solution.

[0092] Specifically, Example 2 of the present invention also provides a method for determining active phosphorus in water based on DGT, which is basically the same as the method for determining active phosphorus in water based on DGT in Example 1 of the present invention, and the only difference is that in the assembly of the DGT device In Example 2 of the present invention, the UiO-66 liquid binding phase prepared in Example 2 of the present invention is used as the binding phase of the DGT device; in the pl...

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Abstract

The invention discloses zirconium-based metal organic frameworks UiO-66 and application thereof, and further discloses a preparation method. The preparation method comprises the steps that zirconium tetrachloride and acetic acid are dissolved in N, N-dimethylformamide, terephthalic acid is added, and uniform stirring is carried out so as to obtain a mixed reaction solution; and the mixed reactionsolution is transferred into a reaction kettle and is placed at the temperature of 120 DEG C for reaction for 7-24 hours, then cooling is carried out to reach room temperature, solid-liquid separationis carried out, and then solid obtained after solid-liquid separation is cleaned and dried so as to obtain the zirconium-based metal organic frameworks UiO-66. The zirconium-based metal organic frameworks UiO-66 can serve as a liquid binding phase of a DGT(diffusive gradients in thin-films) device and are used for measuring the active phosphorus of a water body; and the zirconium-based metal organic frameworks UiO-66 have good binding capacity for the phosphorus and can be applied to the DGT(diffusive gradients in thin-films) device as the liquid binding phase, so that in-situ collection andrapid detection can be carried out on the active phosphorus of the water body, in addition, the operation is simple, the accuracy is high, the stability is good, and the the zirconium-based metal organic frameworks UiO-66 are suitable for long-term storage and large-scale production.

Description

technical field [0001] The invention relates to the field of zirconium-based metal organic framework materials, in particular to a zirconium-based metal organic framework material UiO-66 and its application. Background technique [0002] Phosphorus is the most important source of primary productivity and food chain, and it is also an important limiting nutrient for the outbreak of cyanobacteria blooms in water bodies. Accurate and reliable monitoring of active phosphorus in water bodies is of great significance for early warning of eutrophication in water bodies and control of cyanobacteria blooms. For a long time, the detection of active phosphorus concentration in water mainly adopts active sampling technology, but what it obtains is only the concentration level of phosphorus at the moment of sampling, and cannot represent the actual pollution level of phosphorus in a period of time, which makes active sampling very random. Therefore, the development of in-situ passive sam...

Claims

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Application Information

Patent Timeline
23 Nov 2018
Publication
CN108854967A
IPC
B01J20/22; B01J20/30; G01N1/40; G01N21/25
CPC
B01J20/226; G01N1/34; G01N1/4005; G01N21/25
Inventors
秦文秀; 张云霞