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Co-N-C catalyst, and preparation method and applications thereof

A catalyst and compound technology, applied in the field of catalyst preparation and application, can solve the problems such as the catalyst cannot be recycled, the added value of the product is reduced, and the product selectivity is not high, and the effect of excellent cycle performance, low cost and broad application prospects can be achieved.

Active Publication Date: 2017-02-15
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are problems such as low conversion rate of raw materials, low product selectivity and inability to realize the cycle of the catalyst in the direct oxygen oxidation of ethylbenzene. At the same time, there are also problems such as the need to add solvents, phase transfer substances or hydrogen transporters. The addition of these substances, a On the one hand, it increases pollution, on the other hand, it increases the cost of production and reduces the added value of products

Method used

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  • Co-N-C catalyst, and preparation method and applications thereof
  • Co-N-C catalyst, and preparation method and applications thereof
  • Co-N-C catalyst, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under room temperature conditions, accurately weigh 3g melamine and 1.85g cobalt nitrate hexahydrate (m 三聚氰胺 :m Co 2+ =8:1), put the two in a mortar and grind them thoroughly to obtain a blue-green solid powder with uniform color, and obtain the Co-N-C catalyst 1.

[0029] Catalyst 1 prepared by grinding was used to catalyze the conversion of ethylbenzene to acetophenone.

[0030]

[0031] The specific experimental steps are as follows: add 1 mL of ethylbenzene to a 25 mL sealed tube, add 0.5 mol% of Co-N-C catalyst 1, seal it with a rubber stopper, and after purging with oxygen, insert an oxygen balloon to provide oxygen. The reaction was stirred for 20 h under the condition, and the conversion rate of ethylbenzene was 89% and the selectivity of acetophenone was 95% as detected by gas chromatography.

Embodiment 2

[0033] In this example, except that the mass ratios of melamine and cobalt nitrate hexahydrate are different, other parameters and steps for preparing the Co-N-C catalyst 1 are the same as in Example 1, and the specific test results are shown in Table 1.

[0034] Table 1 mass ratio is (1-20): 1 the data of catalyst 1 catalyzing the oxidation of ethylbenzene prepared by the grinding method of melamine and cobalt nitrate hexahydrate

[0035] different ratios 1：1 2：1 3：1 4：1 5：1 6：1 7：1 8：1 9：1 10：1 Conversion rate(%) 83 82 85 84 86 80 82 89 68 62 Selectivity (%) 77 83 84 90 94 92 92 95 96 95 different ratios 11：1 12：1 13：1 14：1 15：1 16：1 17：1 18：1 19：1 20：1 Conversion rate(%) 54 58 55 51 46 42 40 35 37 34 Selectivity (%) 98 96 96 96 98 97 95 98 97 96

Embodiment 3

[0037] By the method of ball milling, at room temperature, accurately weigh 3g melamine and 1.85g cobalt nitrate hexahydrate (m 三聚氰胺 :m Co 2+ =8:1), the two are placed in a ball mill jar, high-energy ball milling, the rotating speed is 200r / min, and the ball milling time is 240min to obtain a blue-green solid powder with uniform color, and obtain the Co-N-C catalyst 2.

[0038] like figure 1 as well as figure 2 As shown, the prepared Co-N-C catalyst 2 was characterized by scanning electron microscope and XRD. It can be seen from the electron microscope that the catalyst is flake-shaped; from the XRD data, it is shown that the original crystal form of the original cobalt nitrate hexahydrate and melamine was destroyed, and a new crystal form appeared.

[0039] The Co-N-C catalyst 2 prepared by ball milling was used to catalyze the conversion of ethylbenzene to acetophenone.

[0040]

[0041] The specific experimental steps are as follows: add 1mL ethylbenzene to a 25mL ...

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Abstract

The invention discloses a Co-N-C catalyst. According to a preparation method of the Co-N-C catalyst, the Co-N-C catalyst is prepared at room temperature via grinding, or ball milling, or grinding-sintering of a cyanamide compound and a cobalt salt at a mass ratio of (1-20):1. The invention also discloses applications of the Co-N-C catalyst. In applications, the Co-N-C catalyst is mainly used for selective oxidation of the benzyl positions of aromatic hydrocarbons and the allyl position C-H bonds of olefins. The synthesis process of the Co-N-C catalyst is simple, is easy to control, and is safe; and at the same time, coordination of the cyanamide compound with the cobalt salt is firm, the cost of metal Co is relatively low, requirements on equipment used in catalyst synthesis are simple, the equipment is easily available; efficiency is high; no additive is added; no solvent is added; conditions of the Co-N-C catalyst in application process are mild; and cycling performance is excellent.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and application, and in particular relates to a Co-N-C catalyst, its preparation method and application. Background technique [0002] In recent years, with the continuous development of science and technology, more and more new catalysts have come into people's sight, and the appearance of these catalysts has greatly improved the efficiency of chemical reactions. Among them, the emergence of new carbon-nitrogen materials and its application in oxidation reactions have attracted widespread attention. There are more and more reports on carbon-nitrogen materials. The environment is non-polluting and meets the requirements of green chemistry; moreover, it has good thermal stability and can exhibit extremely strong catalytic performance in the reaction. Zhigang Liu (Journal of Molecular Catalysis A: Chemical 2015, 408, 91), Runliang Zhu (RSC Adv. 2016, 6, 19482), Baojiao Gao (Applied Surface Scien...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J31/28C07C45/36C07C49/78
CPCB01J27/24B01J31/28B01J2231/70C07C45/36C07C49/78
Inventor 姚小泉聂守杰黄翔许定健王军
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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