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Porous organic composites, synthesis methods and applications of in-situ supported palladium nanoparticles

A palladium nanoparticle and synthesis method technology, which is applied in the field of catalyst preparation, can solve problems such as difficult functional modification, low stability of PdNP, and difficulty in obtaining it, and achieve the effects of short reaction time, less catalyst consumption, and easy recovery

Active Publication Date: 2022-04-15
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 composites, synthesis methods and applications of in-situ supported palladium nanoparticles
  • Porous organic composites, synthesis methods and applications of in-situ supported palladium nanoparticles
  • Porous organic composites, synthesis methods and applications of in-situ supported palladium nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Example 1: Preparation of imidazole salt ligand A.

[0083] The specific preparation steps are as follows:

[0084] (1) 4,7-dibromo-2,1,3-benzothothiadia (5.86 g, 20 mmol) and hexahydride (48 mg, 0.2 mmol, 1 mol%) were in ethanol / tetrahydrofuran (110 mL / 50ml of the mixed solution of mixed solution, then add NABH 4 (2.27g, 60mmol) (Due to the reaction, NABH 4 The temperature should be reduced and slowly added to multiple times, continue to return to the reaction for 6 h, and monitor it through TLC. After the reaction was completed, 80 ml of water was added to the system, stirred for a mixture for several minutes, and then filtered, and the organic solvent was filtered. Dichloromethane (3 × 80 mL) extract, the combined organic phase was washed with brine, dried over anhydrous sulfate. Column chromatography (petroleum ether: ethyl acetate = 5: 1) Purified the crude product to obtain intermediate 1 (3,6-dibromide), which is a yellow solid.

[0085] Intermediate 1 (4.79 g, 1...

Embodiment 2

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

[0092] The specific preparation steps are as follows:

[0093] (1) in N 2 Under 0 ° C, SiCl was added to the 250ml round bottom flask of 4-bromoacetophenone (5.98 g, 30 mmol) absolute ethanol (60 mL) solution. 4 (7.1 mL, 60 mmol) was maintained at 0 ° C for 1 h, then stirred at room temperature for 24 h. After the end of the reaction, 100 ml of water was added to the system, and the combined organic phase was dried over anhydrous magnesium sulfate, and the organic solvent was stirred down, and the crystal crystal compound 4 was refined in ethanol. 4 ( 4.38g, 81%), for white solid.

[0094] (2) Intermediate compound 4 (2.17 g, 4 mmol), dual-frequency which alcohol (4.57 g, 18 mmol), potassium acetate (5.89 g, 60 mmol), PDCl 2 (DPPF) (0.59g, 0.8mmol) Add to 250ml round bottom flask, N 2 DMF (60 mL) was added under protected, heated to 80 ° C for 16 h, and was monitored by TLC. After the reaction, cooled to room temperature, filtere...

Embodiment 3

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

[0098] Imidazole-ligand A (664 mg, 1.2 mmol) and borate ligand b (550 mg, 0.8 mmol), and catalyst Pd (PPH) were added to 250 ml round bottom flask. 3 ) 4 (0.14g, 0.12mmol), after n 2 Protection Under the addition of DMF (120ml) and K 2 CO 3 The aqueous solution (10 mL, 2M) was heated to 110 ° C for 72 h, and the reaction was completed to room temperature, filtered and used for DMF, H 2 O and MeOH were washed with a crude product, and the resulting solid crude product was repeatedly extracted with dichloromethane with dichloromethane by a Sodo extract. After the end of the extraction, dried at 110 ° C, and the product PD @ PTC-POP was densely gray solid. 0.32g, 45%, the weight average molecular weight is 3911).

[0099] The PD @ PTC-POP material includes infrared spectroscopy (IR), powder X-ray diffraction (PXRD), scanning electron microscope (SEM), XPS spectrum, high resolution transmission electron microscope (HRTEM), scanning electr...

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PUM

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Abstract

The present disclosure provides porous organic composites, synthesis methods and applications of in-situ loaded palladium nanoparticles. The porous organic composites include porous organic polymers and palladium nanoparticles, and the palladium nanoparticles are loaded on the porous organic polymers in situ. The repeating unit of the porous organic polymer has the following chemical structural formula: wherein, R is n-dodecyl. The porous organic composites provided by this disclosure perfectly combine the catalytic function of Pd NPs, the performance of imidazole-based ionic liquids, and the heterogeneous catalytic properties based on porous organic polymers to form a multifunctional catalytic system, which can finally meet the requirements of sustainable chemistry. and green synthesis requirements.

Description

Technical field [0001] The present disclosure belongs to the technical field of catalyst preparation, which relates to a porous organic complex, synthesis method and application of the former load palladium nanoparticles. Background technique [0002] The statements here only provide background information related to the present disclosure, and do not necessarily constitute prior art. [0003] Phase-Transfer Catalyst, PTC) can accelerate the rate of reacting between the two-phase (water phase-organic phase) in the middle of the two-phase (water phase - organic phase), is a class of interfaces that can be transmitted between two phases. Catalysts of one or more reactants. In recent years, the environment has been seriously damaged, and people have more and more attention to the protection of the environment, while phase transfer catalysts have received more and more due to their environmental protection and low-cost solvent systems, mild reaction conditions and relatively simple o...

Claims

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Application Information

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Patent Type & Authority Patents(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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