Palladium-nickel-titanium ethylene glycol coordination polymer heterogeneous catalyst as well as preparation method and application thereof

A technology of heterogeneous catalysts and coordination polymers, applied in the direction of organic compound/hydride/coordination complex catalysts, carbon-based compound preparation, organic compound preparation, etc., can solve the problem of poor stability of heterogeneous palladium catalysts, Low recycling rate and other issues, to achieve huge industrial application value, low cost, and the effect of stabilizing palladium nanoparticles

Active Publication Date: 2021-08-13
NANJING UNIV OF POSTS & TELECOMM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of poor stability and low recycling rate of heterogeneous palladium catalysts formed by existing porous coordination polymers, the present invention provides a micron-scale rod-shaped palladium-nickel-titanium glycol coordination polymer heterogeneous catalyst Materials and preparation methods, prepared coordination polymer palladium heterogeneous catalyst with high stability and good recycling performance

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  • Palladium-nickel-titanium ethylene glycol coordination polymer heterogeneous catalyst as well as preparation method and application thereof
  • Palladium-nickel-titanium ethylene glycol coordination polymer heterogeneous catalyst as well as preparation method and application thereof
  • Palladium-nickel-titanium ethylene glycol coordination polymer heterogeneous catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) the palladium acetate of weighing 0.01mol and nickel acetate tetrahydrate of 0.01mol are dissolved in the ethylene glycol (EG) solution of 60ml;

[0033] (2) Slowly add 0.02 mol of tetrabutyl titanate to the above solution (1) dropwise, and stir for 10 h at a speed of 600 r / min, the color of the solution is yellow;

[0034] (3) After the reaction, the reactants were taken out and washed with ethanol to obtain a yellow object, which was dried in a blast drying oven at 60° C., and the color changed from yellow to gray, and a micron-sized rod-shaped palladium-nickel-titanium glycol compound was obtained. bit polymer heterogeneous catalyst;

[0035] The micro-morphology of the palladium-nickel-titanium glycol coordination polymer is as attached figure 1 , whose XRD characterization is as figure 2 , it can be seen that the synthesized palladium-nickel-titanium glycol coordination polymer structure has a length of 0.8-1.1 μm and a diameter of 100-120 nm. The material h...

Embodiment 2

[0040] (1) Weighing 0.005mol of palladium acetate and 0.01mol of nickel acetate tetrahydrate are dissolved in the ethylene glycol (EG) solution of 60ml;

[0041] (2) Slowly add 0.015 mol of tetrabutyl titanate to the above solution (1) dropwise, and stir for 10 h at a speed of 600 r / min, the color of the solution is yellow;

[0042] (3) After the reaction, the reactants were taken out and washed with ethanol to obtain a yellow object, which was dried in a blast drying oven at 60° C., and the color changed from yellow to gray, and a micron-sized rod-shaped palladium-nickel-titanium glycol compound was obtained. bit polymer heterogeneous catalyst;

[0043] The microscopic appearance of this example is the same as that of Example 1, but the length of the synthesized palladium-nickel-titanium glycol coordination polymer is between 1.8-2 μm, and the diameter is between 100-120 nm. The material has a rod-like structure and is solid. Cylindrical.

Embodiment 3

[0045] (1) Weighing 0.002mol of palladium acetate and 0.01mol of nickel acetate tetrahydrate are dissolved in 60ml of ethylene glycol (EG) solution;

[0046] (2) Slowly add 0.012 mol of tetrabutyl titanate to the above solution (1) dropwise, and stir for 10 h at a speed of 600 r / min, the color of the solution is yellow;

[0047] (3) After the reaction, the reactants were taken out and washed with ethanol to obtain a yellow object, which was dried in a blast drying oven at 60° C., and the color changed from yellow to gray, and a micron-sized rod-shaped palladium-nickel-titanium glycol compound was obtained. bit polymer heterogeneous catalyst;

[0048] The microscopic appearance of this example is the same as that of Example 1, but the synthesized palladium-nickel-titanium glycol coordination polymer is between 3 and 5 μm, and its diameter is between 100 and 120 nm. The material is rod-shaped, solid, and cylindrical shape.

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Abstract

The invention provides a palladium-nickel-titanium ethylene glycol coordination polymer heterogeneous catalyst as well as a preparation method and an application thereof. The invention provides a synthesis method of a micron-sized rod-like heterogeneous catalyst of a palladium-nickel-titanium ethylene glycol coordination polymer, which is simple and easy to obtain and can be massively prepared at one time. The preparation method comprises the following specific preparation steps: firstly, dissolving palladium salt and nickel salt in ethylene glycol to form a 0.1-0.4 mol.L <-1 > solution, then dissolving a titanium source in the ethylene glycol solution, and continuously stirring at room temperature to prepare the micron-sized rod-like heterogeneous catalyst material. The length of the rod-like structure is 0.8-5 microns, and the diameter of the rod-like structure is 100-120 nm. The prepared material can effectively catalyze the Suzuki coupling reaction, and the heterogeneous catalyst is high in catalytic efficiency, convenient to recycle and reusable, and has important significance in industrial production.

Description

technical field [0001] The invention belongs to the technical field related to the development of catalytic materials, in particular to a micron-sized rod-shaped palladium-nickel-titanium glycol coordination polymer heterogeneous catalyst and its preparation method and application. Background technique [0002] The Suzuki coupling reaction is one of the most versatile and widely utilized reactions in industry, because this reaction is the most direct and efficient method for carbon-carbon bond formation in the synthesis of biaryl compounds. Palladium catalyst is the most widely used metal catalyst with the best catalytic effect in Suzuki coupling reaction. However, the rare natural reserves of noble metal palladium lead to the high cost of palladium catalysts, and the difficulty of recyclability of homogeneous catalysts and the potential contamination of residual metal catalysts in the reaction products make the highly active palladium catalysts that can be easily recovered ...

Claims

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Application Information

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IPC IPC(8): B01J31/28B01J31/22C07C45/68C07C49/782
CPCB01J31/28B01J31/1691C07C45/68B01J2531/847B01J2531/46B01J2531/0213B01J2231/4211B01J35/23C07C49/782Y02P20/584
Inventor 宋娟范宇轩李翠杨召张航
Owner NANJING UNIV OF POSTS & TELECOMM
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