Preparation method of graded hollow silica confined cuprous oxide visible light catalyst

A technology of silica and cuprous oxide, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, catalyst activation/preparation, preparation of organic compounds, etc. It can solve the problem of inability to realize efficient and selective hydrogenation of nitroaromatics, etc. problem, to achieve the effect of increasing photon yield, uniform shell thickness, and improving photon quantum yield

Active Publication Date: 2022-07-22
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The task of the present invention is to find a visible light catalyst with simple preparation, low cost and excellent performance, so that it can realize the efficient and selective hydrogenation of nitroaromatics into the corresponding aniline under the action of visible light. With photocatalysts under the action of visible light and pure water system, it is impossible to realize the technical problem of efficient and selective hydrogenation of nitroaromatics into corresponding anilines

Method used

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  • Preparation method of graded hollow silica confined cuprous oxide visible light catalyst
  • Preparation method of graded hollow silica confined cuprous oxide visible light catalyst
  • Preparation method of graded hollow silica confined cuprous oxide visible light catalyst

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Embodiment 1

[0044] (1) Preparation of cationic template CPS: set up the experimental device and introduce nitrogen into the system, add 72 mL of water to the four-necked flask, heat the water bath to 70°C, and sequentially add 0.16 g of initiator and 7.5 g of styrene to start the stirring reaction 1.5h, then add the modifier methacryloyloxyethyltrimethylammonium chloride aqueous solution, the first three injections are one injection every half an hour (10 μl per injection), and then two injections are injected, one injection every hour, every Needle is (50 μl). The remaining solution is then injected every 3 minutes, each injection (10 μl), until all remaining methacryloyloxyethyltrimethylammonium chloride (DMC) has been injected, and the injection is 1.1 g. After the injection of the mixed solution obtained by methacryloyloxyethyltrimethylammonium chloride and 1.2 g of deionized water was completed, the polymerization was extended for another 12 hours to make it fully polymerized. After...

Embodiment 2

[0050] SiO 2 -Cu 2 O@SiO 2 The photocatalyst reduces o-chloronitrobenzene;

[0051] Pour 20 mL (1 mg / mL) of the prepared o-chloronitrobenzene deionized aqueous solution into the reactor, add 25 mg of catalyst and 27 mg of formic acid, and study its photocatalytic behavior under the action of visible light. Samples were taken every 30 minutes and analyzed by high performance liquid chromatography to obtain the reduction changes of o-chloronitrobenzene at different reduction times, and finally the conversion rate and selectivity of o-chloronitrobenzene were calculated according to the obtained data. The results show that the photocatalyst of the present invention can realize the complete conversion of o-chloronitrobenzene under visible light.

Embodiment 3

[0053] SiO 2 -Cu 2 O@SiO 2 The photocatalyst reduces o-chloronitrobenzene;

[0054] 40 mL (1 mg / mL) of the prepared o-chloronitrobenzene deionized aqueous solution was poured into the reactor, 25 mg of catalyst and 54 mg of formic acid were added, and its photocatalytic behavior was studied under the action of visible light. Samples were taken every 30 minutes and analyzed by high performance liquid chromatography to obtain the reduction changes of o-chloronitrobenzene at different reduction times, and finally the conversion rate and selectivity of o-chloronitrobenzene were calculated according to the obtained data. The results show that the photocatalyst of the present invention can realize the complete conversion of o-chloronitrobenzene under visible light.

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Abstract

The invention relates to a visible light catalyst, in particular to a preparation method of a graded hollow silica confined cuprous oxide visible light catalyst. Firstly, copper ions were uniformly loaded on CPS@SiO by adsorption-evaporation-drying method. 2 surface, and then with CPS@SiO 2 ‑Cu 2+ As a template, SiO was prepared 2 Outer layer (CPS@SiO 2 ‑Cu 2+ @SiO 2 ), then calcined at high temperature to remove the CPS template, and finally adjusted the temperature and adjusted the temperature in Ar / H 2 The copper oxide is reduced to cuprous oxide under the atmosphere. The visible light catalyst prepared by the invention is used to realize the purpose of efficiently and selectively reducing nitroaromatics to corresponding anilines, so as to solve the technical problem that the existing photocatalysts cannot realize the efficient and selective reduction of nitroaromatics in the visible light and pure water system.

Description

technical field [0001] The invention relates to a visible light catalyst, in particular to a simple preparation technology of a novel confinement visible light catalyst, in particular to a preparation method of a graded hollow silica confinement cuprous oxide visible light catalyst, which is a A carrier, a preparation method using cuprous oxide as a semiconductor catalyst and the application of the visible light catalyst in the visible light catalytic reduction of nitroaromatics. Background technique [0002] Aromatic amines are important industrial raw materials and organic intermediates, which are widely used in medicine, pesticides, dyes and other fields (P.Zhou, et al, High performance of a cobalt-nitrogen complex for thereduction and reductive coupling of nitro compounds). into amines and their derivatives. Sci. Adv. 2017, 3, e1601945). Therefore, how to realize the efficient conversion of p-nitroaromatics is extremely important. At present, traditional thermal cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72B01J35/08B01J35/10B01J37/08B01J37/18C07C209/36C07C211/52C07C211/45
CPCB01J23/72B01J35/004B01J35/10B01J35/08B01J37/0018B01J37/18C07C209/325C07C211/52C07C211/45
Inventor 尹正亮曹顺生陈刚肖颖冠时庆叶张宣宣
Owner JIANGSU UNIV
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