A kind of loaded palladium multilayer composite film and preparation method thereof

A multi-layer composite and thin-film technology, which is used in the preparation of organic compounds, chemical instruments and methods, and condensation between hydrocarbons and non-hydrocarbons to produce hydrocarbons, etc., can solve the problems of low catalyst service life, difficult recycling, and high reaction temperature. Achieve stable performance, high catalytic activity, and strong electron delocalization.

Active Publication Date: 2018-03-06
滨州市科创孵化器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, both homogeneous palladium catalysts and heterogeneous palladium catalysis have been greatly developed. Homogeneous palladium catalysts have been widely used due to the advantages of mild reaction conditions, good catalytic effect, high selectivity and less by-products in the reaction. application, but because it is difficult to separate from the product, the disadvantages such as the low service life of the catalyst limit its application, such as a kind of spirofluorene pyridine palladium nanoparticles disclosed by Zhao Xiuhua et al. and its preparation method (CN103951611A), the catalytic efficiency is high, but not easy to recycle
Heterogeneous catalysts are easy to separate from the product and can be recycled multiple times, but the catalytic efficiency is not as good as that of homogeneous palladium catalysts, and the required reaction temperature is high, thus limiting its industrial application

Method used

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  • A kind of loaded palladium multilayer composite film and preparation method thereof
  • A kind of loaded palladium multilayer composite film and preparation method thereof
  • A kind of loaded palladium multilayer composite film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Spray a layer of polyimide organic polymer film coating on the surface of a clean single crystal silicon wafer with a high-pressure vacuum gun, and then dry it with nitrogen flow; (2) apply polyimide organic polymer film The coated monocrystalline silicon chip is soaked in palladium acetate aqueous solution (concentration of palladium ion is 0.05mmol / L), takes out after 25min, cleans the free palladium ion on the surface with distilled water, blows dry with nitrogen flow afterwards, and then this monocrystalline Soak the crystalline silicon wafer in an acetone solution of fluorenonepyridine (0.05mmol / L) for 25min, take it out, rinse it with distilled water and blow it dry with nitrogen flow, and form a composite film of palladium fluorenonepyridine loaded on the surface of the single crystal silicon wafer; (3) in step (2), on the monocrystalline silicon chip that one deck palladium fluorenone pyridine composite film is formed on the surface, spray one deck polyimide ...

Embodiment 2

[0028] (1) spray one layer of polystyrene organic polymer film coating on the clean mica sheet surface with a high-pressure vacuum gun, then blow dry with nitrogen flow; (2) will be coated with polystyrene organic polymer film coating Soak the mica sheet in an aqueous solution of palladium nitrate (the concentration of palladium ions is 0.1mmol / L), take it out after 45 minutes, wash the free palladium ions on the surface with distilled water, and then dry it with a nitrogen stream, and then place the mica sheet in the fluorenone pyridine Soak in the acetone solution (concentration of fluorenone pyridine is 0.1mmol / L) for 45min, take out and rinse with distilled water and blow dry with nitrogen flow, promptly form the composite thin film of one deck loading palladium fluorenone pyridine on the mica sheet surface; (3) In step (2), on the mica sheet that one deck palladium fluorenone pyridine composite film is formed on the surface, spray one deck polystyrene organic polymer film ...

Embodiment 3

[0030] (1) Spray a layer of polyimide organic polymer film coating on the surface of a clean quartz sheet with a high-pressure vacuum gun, and then dry it with nitrogen flow; (2) coat the polyimide organic polymer film The quartz sheet of layer is soaked in palladium nitrate aqueous solution (concentration of palladium ion is 0.08mmol / L), takes out after 30min, cleans the free palladium ion on the surface with distilled water, blows dry with nitrogen flow afterwards, and then this quartz sheet is placed in fluorene Soak in the acetone solution of ketopyridine (the concentration of fluorenone pyridine is 0.07mmol / L), take out and rinse with distilled water and blow dry with nitrogen flow, promptly form the composite thin film of one deck loading palladium fluorenone pyridine on the quartz plate surface; 3) In the step (2), the surface forms a layer of loaded palladium fluorenone pyridine composite film on the quartz sheet, and then sprays a layer of polyimide organic polymer fil...

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Abstract

The invention discloses a palladium-supporting multilayer composite film and a preparation method thereof. According to the invention, a layer of organic high-molecular film is sprayed onto the surface of a substrate; the substrate is repeatedly soaked in a palladium salt water solution and a fluorenone pyridine solution; and the multilayer composite film is formed with a self-assembly manner. The preparation process of the film substrate is simple, and the performance of the film is stable. The film assists in highly effectively catalyzing a carbon-carbon coupling reaction, and can be repeatedly used, such that catalyst consumption is reduced, and environment pollution is reduced. The film can be widely applied in the field of catalysis.

Description

technical field [0001] The invention belongs to the field of thin-film catalysis, and in particular relates to a palladium-loaded multilayer composite thin-film substrate for catalytic coupling reaction and a preparation method thereof. Background technique [0002] Biphenyl compounds constructed by carbon-carbon coupling reactions are widely found in people's daily life, such as agrochemicals, medicinal chemistry, natural products, commercial dyes, liquid crystal materials, and functional materials. Therefore, carbon-carbon coupling reactions are organic One of the most important methods in synthetic reactions has always been a research hotspot in the fields of catalytic chemistry, organic chemistry, and material chemistry. The cross-coupling reaction catalyzed by transition metals or their complexes is one of the most important means to construct the structure of biphenyl. Complete under milder conditions. Metal Pd or its complexes are one of the most widely used and eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C43/205C07C41/30C07C15/52C07C15/54C07C2/86
CPCB01J31/1815B01J35/065B01J2231/4205B01J2231/4211B01J2231/4261B01J2231/4266B01J2531/0213B01J2531/824C07C2/861C07C41/30C07C43/205C07C15/52C07C15/54
Inventor 孙尧刚李星赵亚云
Owner 滨州市科创孵化器有限公司
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