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A kind of synthetic method and application of the palladium nanoparticle of polymer microsphere immobilization

A polymer and palladium nanotechnology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, hydrocarbons, etc., can solve the problem of low activity

Inactive Publication Date: 2015-12-09
PEKING UNIV SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

That is to say, after each catalytic cycle, the activity of these immobilized catalysts will be lower than before due to falling off from the carrier. Therefore, in the face of recovery and repeated utilization, these immobilized catalysts have great limitations in practical applications.

Method used

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  • A kind of synthetic method and application of the palladium nanoparticle of polymer microsphere immobilization
  • A kind of synthetic method and application of the palladium nanoparticle of polymer microsphere immobilization
  • A kind of synthetic method and application of the palladium nanoparticle of polymer microsphere immobilization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of 5 μm matrix material microspheres, that is, the polymer core of the composite microspheres:

[0044] Take 32.8g of 26.0% polystyrene seed suspension aqueous solution with a particle size of 1.9 μm, 450g of deionized water, and 0.23g of 10% sodium dodecylbenzenesulfonate aqueous solution into a 2000mL four-necked round-bottomed flask, blow in nitrogen, and stir Then heated to 60°C. Take 15.0g of divinylbenzene, 135.0g of styrene, 10.7g of 10% sodium dodecylbenzenesulfonate aqueous solution, and 165g of deionized water, mix them with a homogeneous mixer, and add them to a four-necked round-bottomed flask. After stirring for 2 hours, the temperature was lowered to 40°C, and 0.2g of 30% hydrogen peroxide was added. Take 1.1g of tert-butyl hydroperoxide, 0.3g of 10% sodium dodecylbenzenesulfonate aqueous solution, 65g of deionized water, mix them with a homogeneous mixer, add them to a four-neck round bottom flask, and then add 56.3g of 20% polyethylene Pyrr...

Embodiment 2

[0046] Chloromethylation of microspheres in Example 1 generates chloromethyl groups on the outside of the microspheres, that is, chloromethylation of polystyrene-divinylbenzene microspheres:

[0047] 10.0 g of the microspheres in Example 1 and 100 mL of anhydrous chloroform were added into a 250 mL three-necked flask, and mechanical stirring was used to disperse the microspheres in the chloroform. The dispersed microspheres were stirred (120 rpm) at 0 °C for 1 hour, 1.7 mL of anhydrous tin tetrachloride was added, and after stirring for 5 minutes, 8.0 mL of chloromethyl ether was added dropwise. After the dropwise addition was completed, the reaction system was maintained at 0° C. and stirred for 30 minutes, then heated to 30° C. and continued to stir for 3 hours. After the reaction, the microspheres were filtered with a sand core funnel to remove the solution, and then the microspheres were washed with 200 mL of the following solvents in sequence: deionized water, 5% hydrochl...

Embodiment 3

[0049] Amination Example 2 microspheres form the first generation of microspheres with a dendritic structure on the outside, that is, the first step, amination of the chloromethylated polystyrene-divinylbenzene microspheres as the carrier:

[0050] Add 10.0g of microspheres and 140mL of N,N-dimethylformamide in Example 2 into a 250mL three-necked flask, stir mechanically to disperse the microspheres, add 25.0mL of ethylenediamine, and stir the system at 80°C for 16 hours . After the reaction, the microspheres were filtered with a sand core funnel to remove the solution, and then the microspheres were washed with ethanol and acetone in turn, and the washed microspheres were dried in an oven at 60°C for 12 hours to obtain the first-generation aminated microspheres.

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Abstract

The invention provides a synthesizing method of polymer microsphere immobilized palladium nanometer particles. The synthesizing method comprises the following steps of: step one, performing amination on methylated polystyrene-divinylbenzene microsphere as a carrier; step two, synthetizing beta-alanine methyl propionate microspheres; step three, synthetizing a polyamide polymer microsphere with a dendritic structure; step four, acidifying the polymer microsphere with an arborization polyamide structure, performing borane treatment to form the arborization polyamide polymer microsphere containing hydroboron; and step five, finally synthetizing microsphere immobilized palladium nanometer particles. The invention provides an application of the polymer microsphere immobilized palladium nanometer particles. The polymer microsphere immobilized palladium nanometer particles synthetized by the method provided by the invention can be used as catalysts in Suzuki-Miyaura reaction and have catalytic activity and repeatability superior to those of the immobilized palladium catalyst synthetized by the traditional method.

Description

technical field [0001] The invention relates to the field of nano synthesis and application, in particular to the synthesis and application of palladium nanoparticles. Background technique [0002] Suzuki-Miyaura reaction (also known as Suzuki coupling reaction) is currently one of the most effective ways to synthesize biphenyl compounds, and biphenyl compounds are the main raw materials for optoelectronic display materials. In addition, cross-coupling reactions are also used in biomedicine , Natural product synthesis, engineering materials and other fields have a wide range of applications, and a large number of experiments have been used to study catalysts for this type of reaction. Since the precious metals contained in the catalyst are uniformly distributed in the liquid phase in the traditional catalytic reaction, the recovery and utilization of the extremely fine particle catalyst after the reaction has always been a very important issue. Traditional homogeneous catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J35/08C07C205/37C07C205/06C07C201/12C07C43/205C07C41/30C07C15/14C07C1/32C07C49/782C07C49/84C07C45/68
Inventor 江必旺潘峥婴郑洁林生跃吴俊成陈荣姬
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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