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Macromolecular gel network-based ultrafine nano-palladium catalyst and preparation method thereof

A polymer gel, ultra-fine nano technology, applied in the field of ultra-fine nano-palladium catalyst and its preparation, can solve the problems of high requirements on carrier microstructure, complicated synthesis steps and high cost, achieve good catalytic activity and simple preparation method , mild conditions

Inactive Publication Date: 2019-05-21
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of this type of catalyst generally has high requirements on the microstructure of the carrier, and the synthesis steps are relatively cumbersome, with low yield and high cost.

Method used

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  • Macromolecular gel network-based ultrafine nano-palladium catalyst and preparation method thereof
  • Macromolecular gel network-based ultrafine nano-palladium catalyst and preparation method thereof
  • Macromolecular gel network-based ultrafine nano-palladium catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 400mg of polyvinyl alcohol into the reaction flask, add 10mL of DMF, heat and stir to dissolve; after the reaction solution is cooled to room temperature, add 1.22g of N,N-carbonyldiimidazole in batches, stir at room temperature for 3h, then add 413mg of propargylamine, and continue stirring for 16h Then add 4mL ammonia water to quench the reaction; figure 2 As shown, the resulting mixed solution was concentrated and then dropped into absolute ethanol to precipitate an alkyne-functionalized polyvinyl alcohol (Alkyne-PVA) with a grafting rate of 40%. After vacuum drying, a light yellow product was obtained. The light yellow product was detected as figure 1 Infrared spectra of alkyne-functionalized polyvinyl alcohols shown.

[0031] Take 5 mg of sodium tetrachloropalladate, dissolve it in 50 μL of deionized water and 100 μL of DMF to obtain a mixed solution, quickly drop 1 mL of the Alkyne-PVA solution (solution concentration: 50 mg / mL) prepared above into it, mix...

Embodiment 2

[0034] Weigh 400mg of polyvinyl alcohol into the reaction flask, add 10mL of DMF, heat and stir to dissolve; after the reaction solution is cooled to room temperature, add 1.22g of N,N-carbonyldiimidazole in batches, stir at room temperature for 3h, then add 413mg of propargylamine, and continue stirring for 16h Then add 4mL ammonia water to quench the reaction; figure 2 As shown, the resulting mixed solution was concentrated and then dropped into absolute ethanol to precipitate an alkyne-functionalized polyvinyl alcohol (Alkyne-PVA) with a grafting rate of 40%. After vacuum drying, a light yellow product was obtained. The light yellow product was detected as figure 1 Infrared spectra of alkyne-functionalized polyvinyl alcohols shown.

[0035] Take 10 mg of sodium tetrachloropalladate, dissolve it in 50 μL of deionized water and 100 μL of DMF mixed solution, quickly drop 1 mL of the Alkyne-PVA solution (solution concentration: 50 mg / mL) prepared above into it, mix well, and ...

Embodiment 3

[0038] Weigh 800mg of polyvinyl alcohol into the reaction bottle, add 20mL of DMF, heat and stir to dissolve; after the reaction solution is cooled to room temperature, add 486mg of N,N-carbonyldiimidazole in batches, stir at room temperature for 3h, add 83mg of propargylamine, and continue stirring for 16h The reaction was quenched by adding 4 mL of ammonia water; the resulting mixture was concentrated and dropped into absolute ethanol to precipitate to obtain alkyne-functionalized polyvinyl alcohol (Alkyne-PVA) with a grafting rate of 19%, and to obtain a light yellow product after vacuum drying.

[0039]Take 8.86 mg of palladium chloride, dissolve it in 100 μL of deionized water and 200 μL of DMF mixed solution, and quickly drop it into 2 mL of the Alkyne-PVA solution prepared by the above method, the solution concentration is 50 mg / mL. Mix evenly and let stand to prepare Pd(II) gel. After washing with deionized water for several times, add 7mL of aqueous solution containin...

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Abstract

The invention discloses a macromolecular gel network-based ultrafine nano-palladium catalyst and a preparation method thereof. The catalyst is an acetylene-rich macromolecule-supported catalyst; the palladium is uniformly fixed to cross-linking points of a gel network which is formed by acetylene-rich macromolecules; the preparation method for the macromolecular gel network-based ultrafine nano-palladium catalyst comprises the following steps: adding a palladium precursor into an acetylene-rich macromolecular solution; standing for 15 to 20 hours at 10 to 40 DEG C to obtain a stable gel material; reducing through a reducing agent, washing and drying to obtain the palladium catalyst. According to the palladium catalyst, Pd is uniformly dispersed in the gel network effectively by the cross-linking network, so that palladium catalyst has higher the catalytic activity and the selectivity, and is stable to air and water vapour. The preparation method of the macromolecular gel network-basedultrafine nano-palladium catalyst is simple and mild in conditions, and facilitates scale synthesis.

Description

technical field [0001] The invention relates to a palladium catalyst, in particular to an ultrafine nano-palladium catalyst based on a polymer gel network and a preparation method thereof. Background technique [0002] Precious metal catalysts are of great significance in modern industry, and metal catalysts are required in many chemical production processes. However, with the development of modern industry, the demand for precious metals is increasing day by day. The reserves of precious metal resources on the earth are limited due to the scarcity and high price of precious metal resources. Although traditional homogeneous catalysts have good catalytic activity and selectivity, they are difficult to separate and recover. Taking Pd-based catalysts as an example, in the fields of medicinal chemistry and fine chemical industry, Pd(PPh 3 ) 4 Catalysts containing phosphorous ligands enable the production of chemicals. The recovery and purification process of the catalyst is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/00
Inventor 帅茂兵杨晓娇赵鹏翔常凤雯岳国宗朱婧黄德顺魏建宇
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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