Schiff base palladium anion intercalated hydrotalcite, preparation method thereof and application thereof

An anion intercalation and Schiff base technology, applied in chemical instruments and methods, catalytic reactions, organic compounds/hydrides/coordination complex catalysts, etc., to achieve good reusability, improve dispersion and utilization, atomic Economical effect

Active Publication Date: 2017-02-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the research on Schiff base palladium int...

Method used

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  • Schiff base palladium anion intercalated hydrotalcite, preparation method thereof and application thereof
  • Schiff base palladium anion intercalated hydrotalcite, preparation method thereof and application thereof
  • Schiff base palladium anion intercalated hydrotalcite, preparation method thereof and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1. Preparation of p-aminobenzoic acid salicylaldehyde Schiff base: Weigh 3.672g (0.03mol) of salicylaldehyde and 4.128g (0.03mol) of p-aminobenzoic acid, respectively dissolve them in 60mL of water. Add the salicylaldehyde solution dropwise into the three-necked flask containing the p-aminobenzoic acid solution, stir at room temperature for 45 minutes after dropping, then gradually increase the reaction temperature to 85°C, stir and reflux for 3 hours; then cool the reaction solution to room temperature, filter 1. After the filter cake was fully washed with deionized water and dried at 65°C, 6.507 g of p-aminobenzoic acid salicylaldehyde Schiff base was obtained;

[0049] 2. Preparation of Schiff base palladium anion: Put the p-aminobenzoic acid salicylaldehyde Schiff base (6.507g, 0.027mol) obtained in step 1 into 200mL of absolute ethanol and fully disperse it to make a slurry, keep it at 35°C for 20min ; Then add NaOH ethanol solution (300mL, containing NaOH 1.08g, 0...

Embodiment 2

[0053] 1. Same as embodiment 1.

[0054] 2. Same as embodiment 1.

[0055] 3. Same as embodiment 1.

[0056] 4. Catalyzed oxidation Heck reaction: take three 25mL ball mill jars numbered A, B, C, add indole (131mg, 1mmol), SBNa-Pd / LDHs (97.5mg, containing Pd 0.08mmol), copper acetate (182mg, 1mmol), silica gel (600mg), 2 stainless steel balls with a diameter of 10mm, and then respectively add methyl acrylate (129mg, 1.5mmol) and ethyl acrylate (150mg, 1.5mmol) in three ball mill jars A, B, and C , tert-butyl acrylate (192mg, 1.5mmol), cover the ball mill jar lid, put into the ball mill and run at 30Hz to make the mixture react for 45 minutes, use GC-MS to measure the yield, the results are shown in Table 3.

Embodiment 3

[0058] 1. Same as embodiment 1.

[0059] 2. Same as embodiment 1.

[0060] 3. Same as embodiment 1.

[0061] 4. Catalyzed oxidation Heck reaction: take three 25mL ball mill jars numbered A, B, C, add indole (131mg, 1mmol), SBNa-Pd / LDHs (97.5mg, containing Pd 0.08mmol), copper acetate (182mg, 1mmol), silica gel (600mg), 2 stainless steel balls with a diameter of 10mm, and then respectively add methyl acrylate (258mg, 3mmol), ethyl acrylate (300mg, 3mmol), acrylic acid Tert-butyl ester (384mg, 3mmol), cover the ball mill jar lid, put into the ball mill and run at 30Hz to react the mixture for 60 minutes, use GC-MS to measure the yield, the results are shown in Table 3.

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Abstract

The invention provides a Schiff base palladium anion intercalated hydrotalcite. The preparation method of the Schiff base palladium anion intercalated hydrotalcite comprises the steps of firstly, complexing the metal palladium with a Schiff base to prepare a Schiff base palladium complex; secondly, synthesizing the hydrotalcite-like material of a Schiff base palladium anion intercalation through the one pot method. According to the technical scheme of the invention, the Schiff base palladium anion intercalated hydrotalcite improves the dispersiveness and the utilization rate of the noble metal palladium. When the Schiff base palladium anion intercalated hydrotalcite is applied to the solid-phase catalytic oxidation Heck reaction, the material is better in catalytic performance.

Description

[0001] (1) Technical field [0002] The invention relates to a Schiff base palladium anion intercalated hydrotalcite, a preparation method thereof, and an application in catalytic oxidation Heck reaction. [0003] (2) Background technology [0004] As a representative noble metal catalytic active component, palladium is widely used in the fields of fine chemical industry, pharmaceuticals and petrochemical industry. It is an important intermediate for the preparation of many organic and natural products. However, as a rare metal, the palladium catalyst has a small content in nature and cannot be regenerated, and its application process will also bring heavy metal pollution to the environment. At the same time, the palladium catalyst is easy to sinter to produce palladium black during use, making the product It is not easy to separate and can not be recycled, and these shortcomings greatly limit the application of palladium catalysts. Therefore, how to develop a class of pallad...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J31/22C07D209/18
CPCB01J31/2217B01J31/26B01J2231/4261B01J2231/70C07D209/18
Inventor 施炜俞静波苏为科
Owner ZHEJIANG UNIV OF TECH
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