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Pd/crystallized carbon nitride heterojunction photocatalyst, preparation method thereof and application of photocatalytic Ullmann coupling reaction

A photocatalyst and coupling reaction technology, which is applied in the direction of physical/chemical process catalysts, photochemical reaction preparation of amino compounds, organic chemical methods, etc., can solve problems such as limiting the application of nitrogen-carbon polymers, low surface area active site charge recombination rate, etc. , to achieve the effect of green reaction system, short reaction time, good repeatability and stability

Active Publication Date: 2018-08-28
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Bulk nitrogen-carbon polymers obtained from the polymerization of nitrogen-rich precursors such as melamine, dicyandiamide, and cyanamide exhibit relatively low surface areas due to dense π-π stacking between C-N layers by van der Waals forces , limited active sites and fast charge recombination rate, all of which limit the application of nitrogen-carbon polymers in fields such as photocatalysis

Method used

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  • Pd/crystallized carbon nitride heterojunction photocatalyst, preparation method thereof and application of photocatalytic Ullmann coupling reaction
  • Pd/crystallized carbon nitride heterojunction photocatalyst, preparation method thereof and application of photocatalytic Ullmann coupling reaction
  • Pd/crystallized carbon nitride heterojunction photocatalyst, preparation method thereof and application of photocatalytic Ullmann coupling reaction

Examples

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Effect test

Embodiment 1

[0035] 1. Preparation of g-C 3 N 4 Nanosheets

[0036] Place 3g of melamine in a crucible with a cover, place it in a muffle furnace, raise the temperature to 550°C at a rate of 5°C / min, and keep it warm for 4 hours to obtain 600mg g-C 3 N 4 Nanosheets.

[0037] 2. Preparation of crystalline carbon nitride nanoribbons

[0038] 600mg g-C 3 N 4Nanosheets, 3.3g of potassium chloride and 2.7g of anhydrous lithium chloride were ground and mixed evenly and put into a porcelain boat, calcined at 450°C for 4 hours in an argon atmosphere, cooled naturally to room temperature, and cleaned with deionized water and ethanol. Vacuum drying at 60°C for 12 hours to obtain crystalline carbon nitride nanobelts.

[0039] 3. Preparation of Pd / Crystalline Carbon Nitride Heterojunction Photocatalyst

[0040] Taking the mass of the catalyst as 100%, and according to the loading capacity of Pd as 6%, 300 mg of crystalline carbon nitride nanobelts were uniformly dispersed in 40 mL of methanol,...

Embodiment 2

[0045] In this example, based on the mass of the catalyst as 100%, and according to the loading of Pd as 1%, 300 mg of crystalline carbon nitride nanobelts were uniformly dispersed in 40 mL of methanol, and 40 mL of 0.0007 mol / L palladium acetate in methanol was added, Other steps are identical with embodiment 1, obtain Pd / crystalline carbon nitride heterojunction photocatalyst (recorded as Pd 1 / CN-C).

Embodiment 3

[0047] In this example, based on the mass of the catalyst as 100%, and according to the loading of Pd as 3%, 300 mg of crystalline carbon nitride nanobelts were uniformly dispersed in 40 mL of methanol, and 40 mL of 0.0021 mol / L palladium acetate methanol solution was added, Other steps are identical with embodiment 1, obtain Pd / crystalline carbon nitride heterojunction photocatalyst (recorded as Pd 3 / CN-C).

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Abstract

The invention discloses a Pd / crystallized carbon nitride heterojunction photocatalyst, a preparation method thereof and application of photocatalytic Ullmann coupling reaction. The catalyst is prepared in the manner that as a supporter, crystalline carbon nitride uniformly carries Pd nanoparticles with particle diameter of 3-7nm, wherein the loading capacity of Pd is 1%-10% based on 100% of the mass of the catalyst. The preparation method comprises the following steps: firstly, preparing g-C3N4 nanosheet through thermal polycondensation of melamine, then calcining with potassium chloride and anhydrous lithium chloride to obtain crystalline carbon nitride nanobelt, and reacting with palladium acetate and methanol in a closed system to obtain the Pd / crystallizationcarbon nitride heterojunction photocatalyst. The Pd / crystalline carbon nitride heterojunction photocatalyst disclosed by the invention is used for catalyzingUllmann C-C coupling reaction of halogenated aromatics to synthesize biphenyl compounds, and has the advantages of high catalytic activity and stability, mild reaction conditions, short reaction time and high product yield rate.

Description

technical field [0001] The invention belongs to the technical field of Ullmann (Ullmann C-C) coupling reaction, and in particular relates to a Pd / crystalline carbon nitride heterojunction photocatalyst, a preparation method of the catalyst and the catalytic Ullmann C-C coupling reaction of the catalyst Applications. Background technique [0002] The formation and breaking of C-C and C-X (X is N, O, S heteroatoms) bonds is a very important organic synthesis process. Since Ullmann (Ullmann) et al. discovered in 1901 that two molecules of halogenated aromatics can be coupled to form biphenyl compounds through carbon-carbon coupling, and thus named this type of reaction as Ullmann coupling reaction, the related C-C Coupling, C-N coupling and C-O coupling reactions are regarded as one of the classic organic synthesis pathways, and are widely used in the synthesis of compounds such as fuels, drugs, liquid crystals, semiconductors and organic conductors. At the same time, in term...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07B37/00C07C1/26C07C15/14C07C17/269C07C25/18C07C41/30C07C43/205C07C209/80C07C211/50C07C253/30C07C255/51
CPCC07B37/00C07C1/26C07C17/269C07C41/30C07C209/80C07C253/30B01J27/24B01J35/393B01J35/396B01J35/39C07C15/14C07C25/18C07C43/2055C07C211/50C07C255/51
Inventor 顾泉贾巧慧张素芬雷鹏飞
Owner SHAANXI NORMAL UNIV
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