Preparation method of PtPd/Fe3O4 (platinum-palladium/ferroferric oxide) nanocatalyst and application thereof in HECK reaction

A nano-catalyst and nano-technology, applied in the direction of physical/chemical process catalysts, catalysts, carbon compound catalysts, etc., can solve the problems of poor economy, low recycling rate, and low practical value, and achieve simple preparation process and recycling. The effect of convenience and excellent catalytic performance

Inactive Publication Date: 2016-08-24
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, nano-palladium is easy to form palladium black and lose its activity during use, resulting in low recycling rate and low practical value.
In order to solve the above problems, researchers have turned their attention to

Method used

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  • Preparation method of PtPd/Fe3O4 (platinum-palladium/ferroferric oxide) nanocatalyst and application thereof in HECK reaction
  • Preparation method of PtPd/Fe3O4 (platinum-palladium/ferroferric oxide) nanocatalyst and application thereof in HECK reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: PtPd / Fe 3 o 4 Preparation of nanocatalysts

[0040] (1) Preparation of carrier and its pretreatment

[0041] In a 50ml beaker, accurately weigh 0.2125g of FeCl 3 ·6H 2The urea of ​​0,0.1432g, the polyvinylpyrrolidone of 0.1663g, then add the 1 of 8.5ml, the 2-propanediol, the mixture is stirred on the magnetic stirrer until the solution is mixed and transferred in the reaction kettle after obtaining the yellow transparent solution, after sealing React at 190°C for 16h. After the reaction, cool to room temperature, transfer the product to a wide-mouth glass bottle, wash with deionized water and ethanol several times, and use magnetic separation to pour out the supernatant in the wide-mouth bottle. Disperse the washed black precipitated particles in 10 mL of ethanol to obtain Fe 3 o 4 Nanomagnetic materials.

[0042] (2) Preparation of Pt-Pd sol

[0043] In a 50ml beaker, accurately weigh 0.0789g of polyvinylpyrrolidone, measure 3.86×10 -3 mol / L aqueo...

Embodiment 2

[0046] Example 2: PtPd / Fe 3 o 4 Applications of nanocatalysts

[0047] Application of Pt-Pd Magnetic Nano-Supported Catalysts in Heck Reaction

[0048] Add 0.16mL of iodobenzene, 3mL of DMF, 0.20mL of styrene, the Pt-Pd magnetic nano-loaded catalyst prepared above into a 100ml three-necked flask, stir well and then add 0.2764g of K 2 CO 3 , with electric stirring at 90 °C for 9 h. After the reaction, the catalyst was separated from the product, and the catalyst was left for recycling. The results are shown in Table 1. As can be seen from Table 1, PtPd / Fe 3 o 4 The conversion rate of nanometer catalyst to iodobenzene is about 100%, and the conversion rate drops significantly after the catalyst is recycled for 4 times.

[0049] Wherein the conversion rate is calculated by reactant iodobenzene gas phase peak area: iodobenzene initial peak area S 1 , the iodobenzene peak area S after the reaction 2 , then the conversion rate is: (S 1 -S 2 ) / S 1 .

[0050] Table 1 PtPd...

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Abstract

The invention discloses a preparation method of a PtPd/Fe3O4 (platinum-palladium/ferroferric oxide) nanocatalyst and an application thereof in HECK reaction, and belongs to the technical field of nanocatalysts. The preparation method is characterized in that a catalyst carrier is magnetic Fe3O4 nanoparticles, and the average particle size is 18nm; the active components are Pt and Pd nanoparticles, and the average particle sizes are respectively 12nm and 10nm; the average mass percentages of Pt and Pd in the catalyst are respectively about 0.39% and 0.75%; the balance is Fe3O4 nanoparticles. The preparation method comprises the following steps of oxidizing and reducing FeCl3 6H2O into the Fe3O4 nanoparticles by a hydrothermal method; cleaning, and metering volume for use; using polymers of polyvinylpyrrolidone and the like as stabilizers, and reducing a certain ratio of chloroplatinic acid and chloropalladic acid by a reducing agent, so as to prepare a Pt-Pd sol; adding the treated Fe3O4 nanoparticles into the Pt-Pd sol, stirring, filtering, and drying, so as to finally prepare the Pt-Pd magnetic nanometer-supported catalyst. The catalyst prepared by the preparation method has higher catalytic activity in the Heck reaction.

Description

technical field [0001] The present invention relates to PtPd / Fe 3 o 4 The preparation of nano catalyst and its application in HECK reaction belong to the technical field of nano catalyst. Background technique [0002] The Heck reaction is a coupling reaction of organic halides and olefins to generate substituted olefins under the catalysis of strong base and palladium. It is one of the most important and promising carbon-carbon bond formation reactions catalyzed by transition metals. In organic intermediates, organic It is widely used in the synthesis of functional materials, drugs, and natural products. Therefore, the preparation of noble metal palladium catalysts has attracted more attention. [0003] Some scientists prepare palladium catalysts by using complexes, among which phenylphosphine complexes have the best effect, which not only greatly improves the catalytic performance but also greatly reduces the reaction time, but this ligand brings harm to the environment ...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C2/86C07C15/52
CPCB01J23/8906B01J35/0033C07C2/861C07C2523/89C07C15/52
Inventor 戴兢陶陈晓孙元旭袁风雨
Owner YANCHENG TEACHERS UNIV
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