Sulfonated graphene-based ru(bpy) 3 2+ Nano heterogeneous catalyst and preparation method thereof

A heterogeneous catalyst, sulfonated graphene technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalyst carrier, etc., can solve low light utilization efficiency, waste of resources, environment, Large mass transfer resistance and other problems, to achieve the effect of simple preparation process, wide application and low cost

Inactive Publication Date: 2016-08-24
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst has disadvantages such as high cost and difficulty in recycling, resulting in waste of resources and environmental pollution.
In order to overcome the above shortcomings, most of the current technologies use porous materials as carriers to prepare supported ruthenium pyridine photocatalysts, but these catalysts have the defects of large mass transfer resistance and low light utilization efficiency.

Method used

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  • Sulfonated graphene-based ru(bpy)  <sub>3</sub>  <sup>2+</sup> Nano heterogeneous catalyst and preparation method thereof
  • Sulfonated graphene-based ru(bpy)  <sub>3</sub>  <sup>2+</sup> Nano heterogeneous catalyst and preparation method thereof
  • Sulfonated graphene-based ru(bpy)  <sub>3</sub>  <sup>2+</sup> Nano heterogeneous catalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The preparation of embodiment 1 graphene oxide (GO) and reduced graphene (RGO):

[0062] Weigh 1g of natural graphite and 1g of anhydrous sodium nitrate respectively, mix well and slowly add 40ml of 98% concentrated sulfuric acid at a rate of 1ml / min, stir in an ice-water bath for 2 hours; Slowly add 5g of potassium permanganate to the solution at a rate of 0.1g / min. After the end, raise the temperature of the reaction system to 35°C and keep stirring for 2 hours; raise the temperature of the above reaction system to 60°C. Slowly add 100ml of 5% dilute sulfuric acid to the solution at a rate of 1 min, keep the temperature and stir for 1 hour after the end; raise the temperature of the above reaction system to 95°C, and slowly add 30ml of 30% sulfuric acid to the solution at a rate of 10ml / min after the temperature stabilizes Hydrogen peroxide and 1000ml of distilled water, keep the temperature and stir for 30 minutes after the end of the stirring; after the stirring, le...

Embodiment 2

[0064] Embodiment 2 sulfonated graphene-based Ru (bpy) 3 2+ Nano heterogeneous catalyst (Ru(bpy) 3 ClSO 3 -RGO) Preparation:

[0065] First weigh 5.2g of p-aminobenzenesulfonic acid and add it to 1mol / L HCl (300ml) solution under ice-water bath to disperse evenly, then under ice-water bath, add 33ml of 1mol / L NaNO 2 The solution was added dropwise to the reaction system, and the reaction system gradually changed from milky white to transparent. After the addition, a white precipitate was formed from the transparent solution after 30 minutes of reaction. The precipitate was filtered and dispersed into a mixture of 60ml ethanol and 60ml distilled water again. Then add 180mg of reduced graphene, then add 50wt% H 3 PO 2 After the solution was stirred in 60ml of ice bath for 30min, 50wt% H was added 3 PO 2 60ml of the solution was stirred for 1h, filtered, washed with water, and dried to obtain sulfonated reduced graphene (sulfonated graphene, SO 3 H-RGO).

[0066] Will SO...

Embodiment 3

[0068] To embodiment 1-2 obtained GO, RGO, SO 3 H-RGO and Ru(bpy) 3 ClSO 3 -RGO performed a series of characterizations, the results are shown in the attached Figures 1a-4d .

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Abstract

The invention discloses a sulfonated-graphene-based novel Ru(bpy)3<2+> nano heterogeneous catalyst and a preparation method thereof. The nano heterogeneous catalyst comprises a sulfonated graphene matrix and Ru(bpy)3<2+> groups, wherein the sulfonated graphene matrix comprises a graphene matrix and sulfonic groups distributed on the graphene matrix; the Ru(bpy)3<2+> groups are connected onto the sulfonated graphene matrix after being matched with the sulfonic groups, and the active sites of the Ru(bpy)3<2+> groups are dispersed on a two-dimensional plane of the graphene matrix. The preparation process comprises the following steps: carrying out an ion exchange reaction on sulfonated reduction graphene and Ru(bpy)3<2+> to form the nano heterogeneous catalyst. The nano heterogeneous catalyst is high in chemical and heat stability, has catalytic active sites of Ru(bpy)3<2+> with visible-light activity, is high in catalytic activity, can be well dispersed in a reaction system, is easy to recover, is suitable for repeated use, and can be widely applied to a light-induced electron transfer reaction; simultaneously, the preparation process is simple, the raw material is low in cost and easily available, the cost is low and the need of large-scale production is met.

Description

technical field [0001] The present invention relates to a kind of heterogeneous catalyst, especially a kind of sulfonated graphene-based Ru(bpy) 3 2+ Nano heterogeneous catalyst and its preparation method. Background technique [0002] Light energy is a non-toxic and non-polluting renewable energy. In recent years, the use of visible light for photocatalytic organic synthesis has become a frontier topic and research hotspot in organic chemistry. Ru(bpy) Photocatalyst Ru(bpy) 3 2+ As a typical visible light photosensitizer, it can change from the ground state to the excited state after being excited by visible light in the process of photocatalytic organic synthesis, and then interact with reducing or oxidizing reaction substrates to realize single-electron exchange between organic substrates. Transfer process (SET). At present, the catalyst has been successfully applied in various light-induced organic synthesis systems. However, the catalyst has disadvantages such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J32/00B01J21/18C07C45/65C07C49/78
Inventor 张昉李晓艳李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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