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Preparation method and application of supported cobalt/carbon nano tube material derived from zeolite imidazole framework material

A zeolite imidazole framework and carbon nanotube technology, which is applied in the preparation of carbon-based compounds, the preparation of organic compounds, the preparation of oxidation reactions, etc., can solve the problem of low conversion rate KA oil selectivity, unsatisfactory value, low catalytic performance, etc. problem, to achieve the effect of good industrial application prospect, low synthesis cost and simple preparation method

Active Publication Date: 2020-06-23
YANGZHOU UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, most of the catalysts used in cyclohexane oxidation reaction have defects such as high preparation cost, low catalytic performance and poor stability
In addition, the conversion rate of the catalytic cyclohexane oxidation reaction and the selectivity of KA oil are low, which cannot reach the ideal value

Method used

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  • Preparation method and application of supported cobalt/carbon nano tube material derived from zeolite imidazole framework material
  • Preparation method and application of supported cobalt/carbon nano tube material derived from zeolite imidazole framework material
  • Preparation method and application of supported cobalt/carbon nano tube material derived from zeolite imidazole framework material

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preparation example Construction

[0038] Supported Co-Co with controllable cobalt valence state derived from zeolite imidazole framework material x o y The preparation method of / CN material specifically comprises the following steps:

[0039] Step (1), take a certain amount of cobalt nitrate and dissolve it in water and mark it as A solution, take a certain amount of dimethylimidazole and triethylamine and dissolve it in water and mark it as B solution, A solution and B solution are uniformly mixed, Wherein the mass ratio of cobalt nitrate, dimethylimidazole, triethylamine and water in the mixed solution=1.0:2.3:2.5:69.7, stirred at room temperature for 12-36 hours; centrifuged, washed; the obtained precipitate was dried and obtained Zeolite imidazole framework material;

[0040] Step (2), dissolving cobalt nitrate in water to prepare a precursor solution; impregnating the zeolite imidazole framework material prepared in step (1) in the precursor solution, stirring overnight, then drying, and roasting at 50...

Embodiment 1

[0046] Take a certain amount of cobalt nitrate and dissolve it in water and mark it as A solution, take a certain amount of dimethylimidazole and triethylamine and dissolve it in water and mark it as B solution, and A solution and B solution are uniformly mixed, wherein the mixed solution Cobalt nitrate, dimethylimidazole, triethylamine, water mass ratio = 1:2.3:2.5:69.7, stirred at room temperature for 24 hours; centrifuged, washed; the obtained precipitate was dried to obtain the zeolite imidazole framework material;

[0047] figure 1 According to the XRD pattern of the prepared zeolite imidazole framework material, it can be confirmed that the zeolite imidazole framework material has been synthesized. figure 2 From the SEM image of the prepared zeolite imidazole framework material, it can be seen that the surface of the prepared material is relatively smooth, polyhedral, and uniform in size, with an average size of about 300 nm.

Embodiment 2

[0049] The zeolite imidazole framework material prepared in Example 1 was placed in a tube furnace and calcined at 500°C, 700°C, 800°C, and 900°C respectively at a heating rate of 5°C / min for 3 hours to obtain Co-Co x o y / CN material. It is used in cyclohexane oxidation reaction, the activity data is listed in Table 1, it can be seen that the material performance is the best when calcined at 900°C, so 900°C is the best calcining temperature. image 3 Co-Co obtained as a zeolite imidazole framework material at different calcination temperatures x o y / CN XRD pattern, it can be seen that the existence of metal Co in Co-Co x o y / CN material. No Co x o y The corresponding diffraction peaks, which may be due to the Co x o y The high degree of dispersion may be due to its amorphous structure. Figure 4 For the prepared Co / Co x o y / NC material SEM image, it can be seen that the prepared Co / Co x o y The / NC material is in the shape of a sea urchin, with a size of abou...

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Abstract

The invention belongs to the field of material preparation, and discloses a preparation method and application of a supported cobalt / carbon nano tube material (Co-CoxOy / CN) with a controllable cobaltvalence state derived from a zeolite imidazole framework material. The preparation method comprises the following steps: taking a zeolite imidazole framework material as a precursor, impregnating theframework material to load cobalt ions, performing high-temperature in-situ selective reduction in nitrogen to prepare a cobalt-valence-controllable supported Co-CoxOy / CN material, and applying the cobalt-valence-controllable supported Co-CoxOy / CN material to a reaction for preparing cyclohexanol and cyclohexanone (KA oil) by catalyzing cyclohexane oxidation. The preparation method is simple, green, and environment-friendly, and the nano tube material is high in activity, good in stability, low in price and easy to obtain, can efficiently catalyze cyclohexane oxidation to prepare KA oil, and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the field of material preparation, in particular to a loaded cobalt / carbon nanotube material (Co-Co x o y / CN) and its application in cyclohexane oxidation. Background technique [0002] The selective oxidation of cyclohexane to cyclohexanol and cyclohexanone (KA oil) is a very typical carbon-hydrogen bond activated oxidation reaction. Cyclohexanol and cyclohexanone (KA oil) can be used to prepare caprolactam and adipic acid to obtain nylon-6 and nylon-66. Like most selective oxidations of alkanes, this reaction also has the following problems, such as low conversion rate, complex reaction, poor selectivity, and high energy consumption. At present, in the industry, cyclohexane oxidation uses soluble cobalt salt as a catalyst. This type of cyclohexane oxidation process has low conversion rate (3.5%-4%), general selectivity (80-85%), and high energy consumption. , a large amount of lye is needed in the process of processing, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C07C29/50C07C35/08C07C49/403C07C45/33
CPCB01J27/24C07C29/50C07C45/33B01J35/394B01J35/615C07C35/08C07C49/403
Inventor 袁恩先顾明晴菅盘铭
Owner YANGZHOU UNIV
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