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Porous organic composite loaded with palladium nanoparticles in situ, synthesis method and application

The technology of a palladium nanoparticle and a synthesis method, which is applied in the field of catalyst preparation, can solve the problems of difficult functional modification, difficulty in obtaining, and low stability of PdNP, and achieves the effects of short reaction time, easy recovery, and no need for inert gas protection.

Active Publication Date: 2019-08-23
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, after research by the inventors of the present disclosure, it has been found that these porous carriers loaded with Pd NPs have problems such as low stability, difficulty in functional modification, and difficulty in obtaining

Method used

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  • Porous organic composite loaded with palladium nanoparticles in situ, synthesis method and application
  • Porous organic composite loaded with palladium nanoparticles in situ, synthesis method and application
  • Porous organic composite loaded with palladium nanoparticles in situ, synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Example 1: Preparation of Imidazolium Ligand A.

[0083] Concrete preparation steps are as follows:

[0084] (1) Mix 4,7-dibromo-2,1,3-benzothiadiazole (5.86g, 20mmol) and cobalt chloride hexahydrate (48mg, 0.2mmol, 1mol%) in ethanol / tetrahydrofuran (110mL / 50mL) of the mixed solution was heated to reflux, followed by the addition of NaBH 4 (2.27g, 60mmol) (due to the exothermic reaction, NaBH 4 The temperature should be lowered and added carefully and slowly several times), and the reflux reaction was continued for 6h, which was monitored by TLC. Cool to room temperature after the reaction, add 80 mL of water to the system, stir for several minutes, then filter the precipitate, and remove the organic solvent by rotary evaporation. Dichloromethane (3 x 80 mL) was extracted and the combined organic phases were washed with brine and dried over anhydrous magnesium sulfate. The crude product was purified by column chromatography (petroleum ether: ethyl acetate = 5:1) to...

Embodiment 2

[0091] Example 2: Preparation of boronate ligand B.

[0092] Concrete preparation steps are as follows:

[0093] (1) in N 2 Under protection, SiCl was added dropwise to a 250 mL round bottom flask containing 4-bromoacetophenone (5.98 g, 30 mmol) in absolute ethanol (60 mL) at 0 °C 4 (7.1 mL, 60 mmol), kept stirring at 0°C for 1 h, then stirred at room temperature for 24 h. After the reaction was completed, 100 mL of water was added to the system, dichloromethane (3 × 100 mL) was extracted, the combined organic phase was dried with anhydrous magnesium sulfate, the organic solvent was removed by rotary evaporation, and then recrystallized in ethanol to obtain intermediate compound 4 ( 4.38 g, 81%) as a white solid.

[0094] (2) Intermediate compound 4 (2.17g, 4mmol), double pinacol borate (4.57g, 18mmol), potassium acetate (5.89g, 60mmol), PdCl 2 (dppf) (0.59g, 0.8mmol) was added to a 250mL round bottom flask, N 2 DMF (60 mL) was added under protection, heated to 80° C. for...

Embodiment 3

[0097] Example 3: Synthesis of Pd@PTC-POP.

[0098] Add imidazolate ligand A (664mg, 1.2mmol) and boronate ligand B (550mg, 0.8mmol) and catalyst Pd (PPh 3 ) 4 (0.14g, 0.12mmol), after N 2 Add DMF (120mL) and K by injection under protection 2 CO 3 Aqueous solution (10mL, 2M), heated to 110°C for 72h, cooled to room temperature after the reaction, filtered and washed with DMF, H 2 O and MeOH were washed to obtain a crude product, and the resulting solid crude product was repeatedly extracted with dichloromethane for 48 h through a Soxhlet extractor. After the extraction was completed, it was dried in vacuum at 110 ° C to obtain the final product Pd@PTC-POP, which was a dark gray solid ( 0.32g, 45%, weight average molecular weight is 3911).

[0099] The Pd@PTC-POP materials were carried out including infrared spectroscopy (IR), powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), XPS spectroscopy, high-resolution transmission electron microscopy (HRTEM), sca...

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Abstract

The disclosure provides a porous organic composite loaded with palladium nanoparticles in situ, a synthesis method and an application. The porous organic composite comprises a porous organic polymer and palladium nanoparticles, and the palladium nanoparticles are loaded in situ on the porous organic polymer. The repeating unit of the porous organic polymer is represented by the following chemicalformula in the specification, wherein R is n-dodecyl. The porous organic composite perfectly combines a catalytic function of Pd NPs, ionic liquid properties of imidazolyl, and heterogeneous catalyticproperties based on a porous organic polymer, a multifunctional catalytic system is formed, and finally requirements of sustainable chemistry and green synthesis can be satisfied.

Description

technical field [0001] The disclosure belongs to the technical field of catalyst preparation, and relates to a porous organic compound loaded with palladium nanoparticles in situ, a synthesis method and an application. Background technique [0002] The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art. [0003] Phase-transfer catalyst (Phase-transfer catalyst, PTC) can accelerate the rate of mutual reaction between substrates in two incompatible phases (aqueous phase-organic phase), and is a type of catalyst that can be transported at the interface between the two phases. A catalyst for one or more reactants. In recent years, the environment has been severely damaged, and people have paid more and more attention to the protection of the environment. Due to its environmental protection and low-cost solvent system, mild reaction conditions and relatively simple operating procedures, phase tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C15/54C07C2/86C08G61/12
CPCB01J31/28C07C2/861C08G61/123C07C2531/28B01J2231/4266C08G2261/312C08G2261/3241C08G2261/411C07C15/54
Inventor 陈雲奇董育斌董英
Owner SHANDONG NORMAL UNIV
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