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Preparation method of polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalytic material

A polyvinylpyrrolidone, montmorillonite technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of solvent resistance and mechanical strength stability. , Polyvinylpyrrolidone has problems such as low thermal stability and low recycling times, and achieves the effects of good complexing ability, excellent catalytic activity and stability, and excellent solvent resistance.

Active Publication Date: 2018-10-16
SHAOXING UNIVERSITY
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  • Claims
  • Application Information

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Problems solved by technology

It can be used not only as a stabilizer for transition metal nanoparticles, but also as a carrier for transition metal catalysts directly. However, polyvinylpyrrolidone has the disadvantages of low thermal stability, insufficient solvent resistance, and insufficient mechanical strength stability. It is easy to age and degrade in high-temperature organic solvents, and the loss of transition metals is serious, resulting in the application of heterogeneous catalytic materials made of polyvinylpyrrolidone directly loaded with transition metals, and the number of cycles is not high (only 3 times) (Guo, L. P. ; Li, C.P.; Meng, Q. R.; Liang, H. O.; Sun, W. Y.; Li, H.Q., Liu H. Appl. Surf. Sci. 2013, 283, 107-114)

Method used

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  • Preparation method of polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalytic material
  • Preparation method of polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalytic material

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Weigh 1g of polyvinylpyrrolidone (K30, molecular weight 40,000), add it to 200g of 2wt% dilute acetic acid to prepare a dilute acetic acid solution with a weight content of 0.5% of polyvinylpyrrolidone, and set aside;

[0031] (2) Weigh 0.15g of solid palladium chloride, dissolve it in 50g of 2% sodium chloride solution, and make it into a sodium chloropalladate solution for later use;

[0032] (3) Weigh 4g of sodium cationic montmorillonite, add 200mL of distilled water, heat in a water bath at 50°C, stir evenly to form a 2% montmorillonite suspension, and then add the polyvinylpyrrolidone dilute acetic acid solution obtained in step (1) Slowly add to the montmorillonite suspension, and continue to stir for 12 hours, so that the PVP molecules are fully intercalated into the MMT layer, and the MMT / PVP mixed suspension is obtained;

[0033] (4) Under continuous stirring, add 4 grams of sodium chloropalladate solution obtained in step (2) dropwise to the MMT / PVP mixed...

Embodiment 2

[0040] (1) Weigh 1.8g of polyvinylpyrrolidone (K30, molecular weight 40,000), add it to 200g of 2wt% dilute acetic acid, and make a dilute acetic acid solution with a weight content of 0.9% of polyvinylpyrrolidone, and set aside;

[0041] (2) Weigh 0.3 g of solid palladium chloride, dissolve it in 50 g of 2% sodium chloride solution, and make it into a sodium chloropalladate solution for later use;

[0042] (3) Weigh 4.2g of sodium cationic montmorillonite, add 200mL of distilled water, heat in a water bath at 50°C, stir evenly to form a 2.1% montmorillonite suspension, and then add the polyvinylpyrrolidone dilute acetic acid obtained in step (1) Slowly add the solution into the montmorillonite suspension, and continue to stir for 12 hours, so that the PVP molecules are fully intercalated into the MMT layer, and the MMT / PVP mixed suspension is obtained;

[0043] (4) Under continuous stirring, add 4 grams of sodium chloropalladate solution obtained in step (2) dropwise to the M...

Embodiment 3

[0050] (1) Weigh 1.2 g of polyvinylpyrrolidone (K30, molecular weight 40,000), add it to 100 g of 2wt% dilute acetic acid, and make a dilute acetic acid solution with a weight content of 1.2% of polyvinylpyrrolidone, and set aside;

[0051] (2) Weigh 0.15g of solid palladium chloride, dissolve it in 50g of 2% sodium chloride solution, and make it into a sodium chloropalladate solution for later use;

[0052] (3) Weigh 1.8g of sodium-type cationic montmorillonite, add 100mL of distilled water, heat in a water bath at 50°C, stir evenly to form a 1.8% montmorillonite suspension, and then add the polyvinylpyrrolidone dilute acetic acid obtained in step (1) Slowly add the solution into the montmorillonite suspension, and continue to stir for 12 hours, so that the PVP molecules are fully intercalated into the MMT layer, and the MMT / PVP mixed suspension is obtained;

[0053] (4) Under continuous stirring, add 2 grams of sodium chloropalladate solution obtained in step (2) dropwise to...

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Abstract

The invention relates to a preparation method of a polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalytic material, and belongs to the technical field of the preparation process of the chemical catalyst. The preparation method comprises the following steps: (1) preparing an acetic acid of the polyvinylpyrrolidone; (2) preparing a sodium tetrachloropalladate solution; (3) preparing a montmorillonite / polyvinylpyrrolidone intercalation composite mixing system through solution intercalation; and (4) preparing the polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalyst. The preparation method of the polyvinylpyrrolidone intercalation modified montmorillonite loaded palladium catalytic material keeps the excellent solvent resistance,the higher thermal stability and the stronger molecular adsorption property of a montmorillonite matrix, and also has the excellent complexing power and the size stabilizing effect of a polyvinylpyrrolidone macromolecule on the active component of a palladium nano-particle, and the catalytic material shows excellent comprehensive performances in the organic catalytic reaction.

Description

technical field [0001] The invention relates to a preparation method of a polyvinylpyrrolidone intercalated modified montmorillonite-loaded palladium catalytic material used for heterogeneous catalysis of organic reactions, and belongs to the technical field of catalyst material preparation technology. Background technique [0002] Transition metal palladium catalyzed organic coupling reactions are widely used in the field of organic synthesis, and its catalytic processes mainly include homogeneous catalysis and heterogeneous catalysis. Heterogeneous catalysis has benefited from the advantages of easy product separation of catalysts, less transition metal residues in products, and reusable catalysts, which have attracted more and more attention from the industry. The general process of the preparation method of the heterogeneous catalytic material is realized by loading the transition metal active component on a suitable inert solid material. Montmorillonite is one of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J31/26
CPCB01J31/06B01J31/26
Inventor 曾敏峰左树锋杨震舒贵青徐蒙蝶赵静王玉东刘奇
Owner SHAOXING UNIVERSITY
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