Metal palladium nano-material catalyst and preparation and application thereof

A nanomaterial and metal technology, applied in the field of metal palladium nanomaterial catalyst and its preparation, can solve the problems of metal nanocatalysts with large influence on size and morphology, single size high-performance catalysts and the like, and achieves good morphology, single size, The effect of mild reaction conditions

Inactive Publication Date: 2011-02-16
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because metal nanocatalysts are greatly affected by their size and shape, how to prepare high-performance catalysts with good shape and single size is extremely critical.

Method used

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  • Metal palladium nano-material catalyst and preparation and application thereof
  • Metal palladium nano-material catalyst and preparation and application thereof
  • Metal palladium nano-material catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Accurately weigh a certain amount of PdCl 2 Quickly add twice the amount of PdCl in the Erlenmeyer flask 2 The concentrated hydrochloric acid (37%) of the amount of substance, fully reacts and generates brown-red chloropalladium acid hydrate (H 2 PdCl 4 .nH 2 O). Benzyl alcohol was added to the resulting colloidal solution to prepare 0.03 mol / L of H 2 PdCl 4 benzyl alcohol solution for use. Put 1.0ml 3mmol / L H 2 PdCl 4 -Benzyl alcohol solution, 1.0ml 15mmol / L PVP (in PVP monomer)-benzyl alcohol solution, join in the round bottom flask of 50ml, then add 8.0ml benzyl alcohol again, make the total volume of reaction solution be 10.0ml. Finally, the flask was connected to a microwave oven equipped with a mechanical stirrer (modified, with a structure such as Figure 4 Shown), under the fast stirring of mechanical stirrer, with 100% power (total power is 900W) rapid heating 150s, namely obtain the PVP stable (PVP as dispersant and stabilizer) snowflake palladium nan...

Embodiment 2

[0032] Accurately weigh a certain amount of PdCl 2 Quickly add twice the amount of PdCl in the Erlenmeyer flask 2 The concentrated hydrochloric acid (37%) of the amount of substance, fully reacts and generates brown-red chloropalladium acid hydrate (H 2 PdCl 4.nH 2 O) colloidal solution; Add benzyl alcohol in the colloidal solution of generation, prepare the H of 0.03mol / L 2 PdCl 4 The benzyl alcohol solution is set aside; put 1.0ml 3mmol / L H 2 PdCl 4 -Benzyl alcohol solution, 1.0ml 15mmol / L PVP (in PVP monomer)-benzyl alcohol solution, join in the round bottom flask of 50ml, then add 8.0ml benzyl alcohol again, make the total volume of reaction solution be 10.0ml. Finally, connect the flask to a microwave oven (refitted) equipped with a mechanical stirrer, and heat it with 100% power (total power is 900W) for 150s under rapid stirring of the mechanical stirrer, (following the above conditions, this operation can be reproduced ) to obtain PVP-stabilized (PVP as a disper...

Embodiment 3

[0039] Accurately weigh a certain amount of PdCl 2 Quickly add twice the amount of PdCl in the Erlenmeyer flask 2 The concentrated hydrochloric acid (37%) of the amount of substance, fully reacts and generates brown-red chloropalladium acid hydrate (H 2 PdCl 4 ·nH 2 O) colloidal solution; Add benzyl alcohol in the colloidal solution of generation, prepare the H of 0.03mol / L 2 PdCl 4 benzyl alcohol solution for use. Put 1.0ml 3mmol / L H 2 PdCl 4 -Benzyl alcohol solution, 1.0ml 15mmol / L PVP (in PVP monomer)-benzyl alcohol solution, join in the round bottom flask of 50ml, then add 8.0ml benzyl alcohol again, make the total volume of reaction solution be 10.0ml. Finally, connect the flask to a microwave oven (refitted) equipped with a mechanical stirrer, and heat it with 100% power (total power is 900W) for 150s under rapid stirring of the mechanical stirrer, (following the above conditions, this operation can be reproduced ), obtain PVP stable (PVP as dispersant and stabil...

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Abstract

The invention provides a metal palladium nano-material catalyst and preparation and application thereof. The catalyst is a self-assembly snowflake metal Pd nano-material for preparing phenylamine by catalytic hydrogenation of nitrobenzene. The preparation method of the catalyst comprises the following steps: dissolving palladium chloride into hydrochloric acid for fully reacting to generate palladium chlorate hydrate colloidal solution; adding benzyl alcohol to the obtained palladium chlorate hydrate to obtain benzyl alcohol solution of palladium chlorate; adding the H2PdC14-benzyl alcohol solution and directing agent PVP-benzyl alcohol solution to a round-bottom flask, adding benzyl alcohol as a solvent, transferring the flask into a microwave oven, rapidly heating while stirring rapidly until the solution is changed into dark brownish black from brown yellow, thus obtaining snowflake metal Pd nano-colloidal solution with stable PVP; and standing the colloidal solution to obtain sticky black precipitate, washing and drying the precipitate to obtain the self-assembly snowflake metal Pd nano-material. The snowflake metal Pd nano-material is mixed with the nitrobenzene and then transferred into a high-pressure reaction kettle, and then hydrogen is introduced into the kettle for hydrogenation of the nitrobenzene to obtain the phenylamine, wherein, the conversion rate of the nitrobenzene can reach up to 100%.

Description

technical field [0001] The invention relates to the technical field of metal nanomaterial catalysts, in particular to a metal palladium nanomaterial catalyst and its preparation method and application. The catalyst is suitable for catalyzing the hydrogenation of nitrobenzene to produce aniline. Background technique [0002] Metallic palladium (Pd) solid catalyst plays an important role in the field of catalysis. It has been widely used in low-temperature reduction of automobile exhaust, and can catalyze organic coupling reactions such as Suzuki, Heck and Stille. Studies have shown that metal Pd catalysts can exhibit high reactivity and selectivity when they exist in nanoscale form, and the morphology of nanoparticles has a significant impact on their catalytic performance. It is precisely because the microstructure such as the size and shape of metal Pd nanoparticles plays an important role in its catalytic performance, domestic and foreign researchers have long been committ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C211/51C07C209/36
Inventor 杨汉民李金林
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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