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Visible light catalyst containing copper oxide and application thereof

A copper oxide, visible light technology, used in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problem of high energy consumption, difficult catalyst recovery, and toxic solvents and other problems, to achieve the effects of high yield, excellent photocatalytic efficiency, and easy separation and recovery.

Active Publication Date: 2018-05-04
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above defects or improvement needs of the prior art, the present invention provides a copper-containing oxide visible light catalyst and its application in the catalytic synthesis of 1,3-butadiyne, the purpose of which is to provide a copper-containing oxide catalyst It is used to catalyze the coupling of terminal alkynes to synthesize 1,3-butadiyne compounds under visible light catalysis. It can be efficiently carried out at room temperature, normal pressure, ethanol solvent, alkali-free, visible light or sunlight irradiation, and the catalyst can be reused after recovery , thereby solving the technical problems of high energy consumption, use of toxic solvents, and difficult recovery of catalysts in the existing synthesis methods of 1,3-butadiyne compounds

Method used

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  • Visible light catalyst containing copper oxide and application thereof
  • Visible light catalyst containing copper oxide and application thereof
  • Visible light catalyst containing copper oxide and application thereof

Examples

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preparation example Construction

[0036] The preparation method of this visible light catalyst comprises the steps:

[0037] (1) Using salt compounds containing copper and the above-mentioned A and / or B elements as raw materials, such as using copper-containing chlorides, nitrates, etc., and using chlorides and nitric acid containing the above-mentioned A metal elements and B metal elements Salt and the like are used as raw materials, and the salts of A and B can be selected from one of the two, or can be selected at the same time, and the copper-containing metal oxide is prepared by co-precipitation method, hydrothermal method, low-temperature combustion method or sol-gel method;

[0038] (2) Place the copper-containing metal oxide described in step (1) under a hydrogen atmosphere, and activate it at 150-300° C. for 0.5-5 hours to obtain the A x B y Cu z o n . After hydrogen reduction, the low-valence species in the variable-valence metal elements increase, which can improve the catalytic efficiency. Var...

Embodiment 1

[0045] Preparation of CuAl by Co-precipitation 2 o 4 For visible light catalyzed phenylacetylene coupling reaction. Weigh 4.83g of copper nitrate and 15.01g of aluminum nitrate, dissolve them in 60mL of deionized water and place them in a 100mL constant pressure dropping funnel, weigh 6.5g of sodium hydroxide and dissolve them in 60mL of deionized water and place them in another 100mL constant pressure dropping funnel Measure 60mL of deionized water into a 250mL three-necked round-bottomed flask and place it in a 50°C water bath for electromagnetic stirring. At the same time, add the mixed salt solution and alkali solution dropwise into the three-necked flask, and control the dropping speed so that the pH of the precipitation slurry remains constant at ~11. After the dropwise addition, continue to stir for 3 hours, after cooling, filter with suction, wash with a large amount of deionized water until the pH of the filtrate is ~7, dry the filter cake at 110°C overnight, grind i...

Embodiment 2

[0048] Preparation of CuCr by Co-precipitation 2 o 4 For visible light catalyzed phenylacetylene coupling reaction. Weigh 4.83g copper nitrate and 16.0g chromium nitrate, dissolve them in 60mL deionized water and place them in a 100mL constant pressure dropping funnel, weigh 6.5g sodium hydroxide and dissolve them in 60mL deionized water and place them in another 100mL constant pressure dropping funnel Measure 60mL of deionized water into a 250mL three-necked round-bottomed flask and place it in a 50°C water bath for electromagnetic stirring. At the same time, add the mixed salt solution and alkali solution dropwise into the three-necked flask, and control the dropping speed so that the pH of the precipitation slurry remains constant at ~11. After the dropwise addition, continue to stir for 3 hours, after cooling, filter with suction, wash with a large amount of deionized water until the pH of the filtrate is ~7, dry the filter cake at 110°C overnight, grind it and roast it i...

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Abstract

The invention belongs to the field of photocatalysis organic synthesis and more in particular relates to a visible light catalyst containing copper oxide and application thereof to catalytic synthesisof 1,3-butadiyne. The catalyst is AxCuyBzOn, wherein A is a non-valence-variable metal ion and B is a valence-variable metal ion; in a preparation process, hydrogen treatment is carried out for 0.5 to 5h at 150 to 300 DEG C so that a Cu<+> active center is enriched on the surface of the catalyst; under the irradiation of visible light, room-temperature, alkali-free and efficient photocatalysis terminal alkyne with the repeatedly usable catalyst is coupled to synthesize a 1,3-butadiyne compound. The method is simple to operate; when the photocatalyst is used, the terminal alkyne, which is cheap and easy to obtain, is subjected to photocatalytic oxidation to obtain the 1,3-butadiyne compound with high yield under conditions of room temperature, normal oxygen atmosphere, ethanol solvent andirradiation of the visible light or sunlight; alkali does not need to be additionally added in reaction so that the visible light catalyst is green and environmentally friendly, and large-scale production is easy to realize.

Description

technical field [0001] The invention belongs to the field of photocatalytic organic synthesis, and more specifically relates to a visible light catalyst containing copper oxide and its application in catalytic synthesis of 1,3-butadiyne. Background technique [0002] Alkyne compounds widely exist in nature. Diynes and their derivatives are one of the most important classes and have high application value. In the field of medicine, 1,3-diyne has significant anticancer, antibacterial, anti-inflammatory and anti-HIV biological activities; in the field of organic synthesis, it is an important intermediate in organic synthesis and the basic skeleton of physiologically active compounds and natural products ; It also has a very wide range of applications in the fields of supramolecular, polymer chemistry and nanomaterials. Due to the high rigidity of 1,3-diyne rod-shaped molecules, it plays an important role in the construction of molecular complexes. It is used as a linker in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/745B01J23/86C07C2/84C07C15/54C07C11/22C07C17/269C07C25/24C07C41/30C07C43/215C07B37/00
CPCC07B37/00C07C2/84C07C17/269C07C41/30B01J23/002B01J23/72B01J23/745B01J23/868C07C2523/72C07C2523/745C07C2523/86B01J2523/00B01J35/39C07C15/54B01J2523/17B01J2523/22B01J2523/842C07C11/22C07C25/24C07C43/215
Inventor 刘鹏朱莹
Owner HUAZHONG UNIV OF SCI & TECH
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