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Preparation of nickel (II) supported mixed phase cadmium sulfide material and application of photocatalytic activation saturated hydrocarbon bonds

A cadmium sulfide, mixed-phase technology, used in the preparation of organic compounds, carbon-based compounds, catalysts for physical/chemical processes, etc., can solve the problems of low toluene conversion, low efficiency, and low speed

Inactive Publication Date: 2018-11-13
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The rate of these two catalysts to oxidize toluene into benzaldehyde is low, the reaction time is long, the efficiency is low, and the conversion rate of toluene is low

Method used

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  • Preparation of nickel (II) supported mixed phase cadmium sulfide material and application of photocatalytic activation saturated hydrocarbon bonds
  • Preparation of nickel (II) supported mixed phase cadmium sulfide material and application of photocatalytic activation saturated hydrocarbon bonds
  • Preparation of nickel (II) supported mixed phase cadmium sulfide material and application of photocatalytic activation saturated hydrocarbon bonds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of CdS: Add cadmium nitrate into deionized water at a ratio of 0.5~5.0mmol: 2.0~20.0mL, stir and dissolve completely at 18~25°C to obtain cadmium nitrate aqueous solution; add 0.04ml oleic acid to it, that is Obtain A solution; then add sodium borohydride into deionized water at a ratio of 2.0~15.0mmol:0.4~3.0mL, stir and dissolve completely at 18~25°C to obtain sodium borohydride aqueous solution; then add it to the A solution , mixed evenly and treated by microwave, the mixed solution changed from colorless solution to black solution, cooled to room temperature; adding 1 to 3 times the volume of absolute ethanol to the black solution to wash, centrifuged 3 to 5 times to obtain black Solid; ultrasonically disperse the black solid in absolute ethanol at a ratio of 0.5~5.0mol:2~20mL, add ammonium sulfide solution after magnetic stirring for 10~15min, and stir at 18~25°C for 0.5~3h to obtain yellow or Yellow-green solution; centrifuge with absolute ethanol...

Embodiment 2

[0029] (1) Preparation of CdS: Same as Example 1;

[0030] (2) Preparation of Ni(II) / CdS: Take 200mg of CdS prepared in step (1) and evenly disperse in 10ml of deionized water; take 8.10mg of nickel chloride and disperse it in 10ml of deionized water to dissolve; then mix the above two solutions In a 25 mL flask, stirred at 70°C for 1.5h, the reaction solution was washed three times with deionized water, and the resulting product was dried in an oven at 60°C for 4h to obtain Ni(II) with a Ni(II) loading of 1.0wt%. ) / CdS samples. The sample was used to catalyze the oxidation of toluene to benzaldehyde at a rate of 189.08 μmolh -1 g -1 ), the conversion rate of toluene was 8.3%; the selectivity for the activation of saturated C-H (sp3) bond in toluene was up to 72.9%.

Embodiment 3

[0032] (1) Preparation of CdS: Same as Example 1;

[0033] (2) Preparation of Ni(II) / CdS: take 200mg of CdS prepared in step (1) and evenly disperse in 10ml of deionized water; take 24.30mg of nickel chloride and disperse it in 10ml of deionized water to dissolve; then mix the above two solutions In a 25 mL flask, and stirred at 80°C for 2h, the reaction solution was washed three times with deionized water, and the resulting product was dried in an oven at 60°C for 4h to obtain Ni(II) with a Ni(II) loading of 3.0wt%. / CdS sample. The sample was used to catalyze the oxidation of toluene to benzaldehyde at a rate of 216.70 μmolh -1 g -1 ), the conversion rate of toluene was 8.8%; the selectivity for the activation of saturated C-H (sp3) bond in toluene was up to 78.8%.

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Abstract

The invention discloses a nickel (II) supported mixed phase cadmium sulfide composite material Ni(II) / CdS. The preparation method comprises the following steps: respectively and uniformly dispersing cadmium sulfide and nickel chloride into deionized water, mixing the two solutions after dissolving, namely respectively and uniformly dispersing cadmium sulfide (CdS) and nickel chloride (NiCl2.6H2O)into deionized water, mixing the two solutions after dissolving, stirring and reacting at a temperature of 40-80 DEG C for 0.5-3 hours, washing with deionized water after the reaction is completed, and drying, so as to obtain the target product Ni(II) / CdS. The product Ni(II) / CdS obtained after modifying the mixed crystal CdS by Ni(II) in the invention has excellent photocatalytic performance, is used for a reaction for catalytically oxidizing the toluene into benzaldehyde, has a high catalytic rate (can reach 216.70umolh<-1>g<-1> and high toluene conversion rate (can reach 8.8%), and has highactivation selectivity (can reach 78.8%) on saturated C-H (sp3) in the toluene.

Description

technical field [0001] The invention relates to a preparation method of nickel (II) loaded mixed-phase cadmium sulfide composite material Ni (II) / CdS, which is mainly used in the reaction of photocatalyst activation of saturated carbon-hydrogen bonds. Background technique [0002] Selective activation of saturated C–H(sp3) bonds in hydrocarbons to generate high value-added chemicals has important practical significance for chemical synthesis and transformation. However, choosing environmentally friendly oxygen as the oxygen source is usually very difficult to control for the selective oxidation of C–H bonds. In thermodynamic heterogeneous catalysis, the use of transition metal particles and harsh reaction conditions (such as high temperature and pressure) are often involved. Selective oxidation of saturated carbon–hydrogen bonds (sp3) under mild conditions is a major industrial challenge in chemical synthesis. In the industrial carbon-hydrogen bond (sp3) oxidation process,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043C07C45/36C07C47/54
CPCC07C45/36B01J27/043B01J35/39C07C47/54
Inventor 佘厚德李良善孙毅东苏碧桃王其召王磊黄静伟
Owner NORTHWEST NORMAL UNIVERSITY
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