MOF-derived cu@c catalyst and its preparation method and application

A catalyst and reaction technology, applied in the field of tetrahydroquinoline synthesis catalyst, can solve the problems such as the catalyst cannot be recycled for many times, the cost of the catalyst is high, and it is difficult to maintain long-term operation, and the catalyst is cheap, reproducible, and difficult to maintain. High catalytic activity

Active Publication Date: 2021-11-23
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Because many existing technologies use precious metals as active components, the cost of catalysts remains high, and due to the high activity of precious metal catalysts, the catalyst cannot be recycled multiple times and has poor stability in terms of device start-up stability, operating flexibility and long-term performance of the catalyst. , Precious metals are easily poisoned, making it difficult to maintain long-term operation and other problems

Method used

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  • MOF-derived cu@c catalyst and its preparation method and application
  • MOF-derived cu@c catalyst and its preparation method and application
  • MOF-derived cu@c catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035](1) A preparation method of Cu@C catalyst derived from MOF, comprising the steps of:

[0036] 1) Dissolve 0.58mmol trimesic acid (BTC) in 34.8mmol ethanol, 1.12mmol copper nitrate in 89.6mmol water, then mix the above two solutions and stir for 10min, then add 0.0025mmol sodium fluoride and mix Stir at room temperature for 0.5h to carry out pre-synthesis of self-assembly to obtain solution A;

[0037] 2) Add solution A to the polytetrafluoroethylene lining and put it into a stainless steel airtight reaction kettle, then put the sealed reaction kettle into an oven, turn on the heating to 170°C, start the turning mode of the reaction kettle to carry out the rotation crystallization reaction, The turning rate of the reaction kettle is 150rpm / min, and the reaction time is 2h. After the reaction, the reaction kettle is taken out to cool naturally, and the product B is obtained after the kettle is opened;

[0038] 3) The reaction product B was suction-filtered using a Buchner...

Embodiment 2

[0045] (1) A preparation method of Cu@C catalyst derived from MOF, comprising the steps of:

[0046] 1) Dissolve 1.16mmol trimesic acid (BTC) in 58mmol methanol, 3.36mmol copper acetate in 235mmol water, then mix the above two solutions and stir for 30min, then add 0.005mmol potassium fluoride, mix and stir at room temperature 1h for self-assembly pre-synthesis to obtain solution A;

[0047] 2) Add solution A to the polytetrafluoroethylene lining and put it into a stainless steel airtight reaction kettle, then put the sealed reaction kettle into an oven, turn on the heating to 120°C, start the turning mode of the reaction kettle to carry out the rotation crystallization reaction, The turning rate of the reaction kettle is 200rpm / min, and the reaction time is 2h. After the reaction, the reaction kettle is taken out to cool naturally, and the product B is obtained after the kettle is opened;

[0048] 3) The reaction product B was suction-filtered using a Buchner funnel, and the...

Embodiment 3

[0052] (1) A preparation method of Cu@C catalyst derived from MOF, comprising the steps of:

[0053] 1) Dissolve 5.8mmol of 1,2,4-benzenetricarboxylic acid (BTC) in 232mmol of isopropanol and 8.96mmol of copper chloride in 538mmol of water, then mix the above two solutions and stir for 60min, then add 0.025 After mixing mmol ammonium fluoride, stir at room temperature for 2 hours to carry out self-assembly pre-synthesis to obtain solution A;

[0054] 2) Add solution A to the polytetrafluoroethylene lining and put it into a stainless steel airtight reaction kettle, then put the sealed reaction kettle into an oven, turn on the heating to 170°C, start the turning mode of the reaction kettle to carry out the rotation crystallization reaction, The turning rate of the reaction kettle was 56rpm / min, and the reaction time was 2h. After the reaction, the reaction kettle was taken out to cool naturally, and the product B was obtained after the kettle was opened;

[0055] 3) The reactio...

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Abstract

The invention discloses a Cu@C catalyst derived from MOF and its preparation method and application. The preparation method comprises the following steps: after fully mixing the mixed solution of benzenetricarboxylic acid and alcohol, the mixed solution of copper salt and water, adding fluorinated The salt is mixed and stirred for self-assembly pre-synthesis to obtain a solution A; then, the solution A is subjected to a rotational crystallization reaction, and after the reaction is finished, it is naturally cooled to obtain a product solution B; then, the product solution B is sequentially purified and dried to obtain Cu‑MOF metal-organic framework; finally, Cu‑MOF metal-organic framework 2 After pyrolysis treatment, the Cu@C catalyst derived from MOF can be obtained. In the present invention, the copper organic framework material is first obtained by rotational crystallization reaction, and then MOF-derived Cu@C catalyst with high catalytic activity is obtained by pyrolysis treatment, and the MOF-derived Cu@C catalyst is applied to catalyze quinolines and H 2 In the selective hydrogenation reaction to prepare tetrahydroquinoline compounds, the conversion rate of quinoline and the yield of tetrahydroquinoline are greatly improved.

Description

technical field [0001] The invention relates to the field of tetrahydroquinoline synthesis catalysts, in particular to a MOF-derived Cu@C catalyst and its preparation method and application. Background technique [0002] 1,2,3,4-Tetrahydroquinoline compound is the structural unit of many quinoline alkaloids, which are widely used in the synthesis of fine chemicals and pharmaceutical intermediates, and have anti-vasodilation, anti-arrhythmic and anti-tumor activities . At present, the methods for industrially synthesizing 1,2,3,4-tetrahydroquinoline compounds mainly include chemical synthesis and catalytic hydrogenation of quinoline. The preparation of 1,2,3,4-tetrahydroquinoline compound by catalytic hydrogenation of quinoline is a relatively simple and feasible way, with few reaction steps and low raw material cost. However, the use of large-scale homogeneous catalysts has problems such as harsh reaction conditions, difficult separation of products and catalysts, and ungu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D215/06C07D215/26C07D215/20C07D215/38C07D215/18C07D215/50
Inventor 鲁新环潘海军夏清华
Owner HUBEI UNIV
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