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A rapid synthesis method and application of cobalt-based metal-organic framework materials

A technology of organic framework and synthesis method, which is applied in the field of preparation of inorganic non-metallic catalytic materials, can solve the problems of unreported methods for rapidly synthesizing organic framework MOFs materials, increase production cost, and long preparation time, so as to shorten synthesis time and avoid Good effect of waste and fluidity

Active Publication Date: 2020-07-03
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN104086594A discloses a method for rapidly synthesizing metal-organic framework material MIL-101 (Cr). This invention rapidly synthesizes MIL-101 through the induction of carbon nanomaterials, which solves the shortcoming of long preparation time of traditional methods and realizes the metal Rapid and controllable preparation of organic framework materials MIL-101 materials
However, this patent uses Lewis acid as a catalyst. During the preparation process, the material is treated with hydrochloric acid solution to dissolve and remove the catalyst. The catalyst is directly lost, which increases the production cost.
[0005] Although a series of rapid synthesis methods for metal-organic framework materials published above have successfully synthesized organic framework materials with different structures, the method for rapidly synthesizing organic framework MOFs materials through rotational crystallization has not been reported yet, and the above-mentioned The application of the materials synthesized in the patent in catalytic reactions, especially in the epoxidation of olefins, has not been reported.

Method used

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  • A rapid synthesis method and application of cobalt-based metal-organic framework materials
  • A rapid synthesis method and application of cobalt-based metal-organic framework materials
  • A rapid synthesis method and application of cobalt-based metal-organic framework materials

Examples

Experimental program
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Embodiment 1

[0033] (1) The rapid synthesis method of cobalt-based metal-organic framework material, comprises the following steps:

[0034] Add 1.494g of cobalt acetate, 0.3g of hydrofluoric acid, and 1.0g of terephthalic acid into a beaker, and add 60g of deionized water (metal cobalt salt: hydrofluoric acid: terephthalic acid: water in a molar ratio of 1 :1:1:556), stirred and mixed at room temperature on a magnetic stirrer, and the mixing time was 15 minutes at room temperature to obtain a uniformly mixed pre-reaction precursor solution. Then add the pre-reaction precursor solution into a 100mL airtight reactor, seal the reactor and put it into a rotary crystallization device, rotate the airtight reactor around a horizontal axis and rotate the crystallization reaction at 200°C and 150r / min for 3h; After the end, the reaction kettle was quickly taken out and cooled down to room temperature, and then subjected to the first suction filtration, the filter cake was washed with deionized wat...

Embodiment 2~14

[0039] In Examples 2-14, according to the technical solution provided by the present invention, the ratio of raw materials is adjusted within the given range, and the performance of the obtained products is equivalent. The implementation process is the same as in Example 1 except for the following differences. The relevant results are shown in Table 1 for the formulations of Examples 1 to 14 and Table 2 for the formulation and test results of catalytic α-pinene and air epoxidation.

[0040] Table 1

[0041]

[0042] Table 2

[0043]

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Abstract

The invention discloses a quick synthetic method and application of a cobalt-based metal-organic framework material. The synthetic method comprises the following steps of firstly, adding a metal cobalt salt, hydrofluoric acid, benzendicarboxylic acid and water into a container, and fully mixing and stirring to react to obtain a pre-reaction precursor solution; secondly, adding the pre-reaction precursor solution into a sealed reaction still, placing the sealed reaction still into a rotary crystallization device to perform rotary crystallization reaction, after reaction, taking the reaction still out, and quenching the reaction still to room temperature to obtain reaction-formed liquid; and finally, performing suction filtration on the reaction-formed liquid for a first time, and sequentially performing flushing treatment and hot washing treatment on a filter cake, performing suction filtration for a second time, and sequentially performing washing and drying on a filter cake to obtain the cobalt-based metal-organic framework material. As a rotary crystallization mode is adopted by the synthetic method, the synthetic time is greatly shortened; in addition, the obtained cobalt-based metal-organic framework material is controllable in shape and high in catalytic activity.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic non-metallic catalytic materials, in particular to a rapid synthesis method of a cobalt-based metal-organic framework material and its application. Background technique [0002] Metal-organic frameworks (MOFs) are unique self-assembled metal ions or clusters of metal ions and suitable multidentate bridging ligands through covalent bonds or ion-covalent bonds. A class of inorganic-organic hybrid porous materials with controllable size and morphology has attracted more and more attention. The most commonly used organic linking ligands are rigid ligands containing N, O and other atoms that can provide lone pairs of electrons, such as polycarboxylic acid, polyphosphoric acid, polysulfonic acid, pyridine, pyrimidine, etc. Central metal ions cover almost all transition metal ions, even tetravalent metal ions. Due to the selection of different metal ions and organic ligands and a varie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J31/22C07D301/06C07D303/04
CPCB01J31/1691C07D301/06C07D303/04C08G83/008
Inventor 何杰鲁新环黄锋锋沈艳夏清华
Owner HUBEI UNIV