Magnetic oxidized graphene loaded phosphine Schiff base palladium catalyst and preparing method and application thereof

A technology of oxidized rock and catalyst, which is applied in the field of catalysis, can solve the problems of poor practicability and low cycle efficiency, and achieve the effects of low cost, simple preparation process and strong practicability

Active Publication Date: 2016-05-11
南京申基医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Graphene oxide has been reported as a carrier of pyridine Schiff base palladium catalyst (CN103447092). Although this new immobilized Schiff base catalyst can efficiently catalyze the Suzuki reaction, the catalyst can only be recycled by centrifugation, which has poor practicability and recycling. low efficiency

Method used

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  • Magnetic oxidized graphene loaded phosphine Schiff base palladium catalyst and preparing method and application thereof
  • Magnetic oxidized graphene loaded phosphine Schiff base palladium catalyst and preparing method and application thereof
  • Magnetic oxidized graphene loaded phosphine Schiff base palladium catalyst and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of graphene oxide:

[0024] Take graphite powder and sodium nitrate, add concentrated sulfuric acid and stir evenly, then put it into an ice bath, add potassium permanganate while stirring, keep the temperature below 20°C, then raise the temperature to 35°C and keep it warm for 1~2h, then slowly add to remove Deionized water, the volume ratio of deionized water and concentrated sulfuric acid added is 2:1, and the temperature is raised to 85~95°C, kept for 15 minutes, and then 10mL of 30% hydrogen peroxide and deionized water are added, and the deionized water added at this time The volume ratio of water to concentrated sulfuric acid is 6:1, and the obtained product is centrifuged, washed with dilute hydrochloric acid, dried, and ground to obtain graphene oxide; the mass ratio of graphite powder to sodium nitrate is 2:1, concentrated sulfuric acid and graphite The ratio of powder is 23mL / mg, and the mass ratio of potassium permanganate to graphite powder ...

Embodiment 2

[0033] (1) The preparation of graphene oxide is the same as in Example 1;

[0034] (2) Magnetic Fe 3 o 4 The preparation is with embodiment 1;

[0035] (3) Preparation of magnetic graphene oxide supported phosphine Schiff base palladium:

[0036] Weigh 200 mg of graphene oxide prepared in the above step (1) and add it to a beaker, add 40 g of arginine-containing DMF solution, wherein the mass fraction of arginine is 10%, ultrasonically disperse for 80 min, and the resulting solution is heated at 85 ° C The mixture was stirred and reacted for 150 min, cooled to room temperature, centrifuged, washed with deionized water and ethanol in sequence, and dried at room temperature in vacuum for 11 h to obtain aminated graphene oxide (GO-NH 2 );

[0037] 100mgGO-NH 2 Add 60g of 2-diphenylphosphinebenzaldehyde in ethanol solution, wherein the mass fraction of 2-diphenylphosphinebenzaldehyde is 5%, ultrasonic treatment for 150min, the resulting solution was stirred and reacted at 80°...

Embodiment 3

[0041] (1) The preparation of graphene oxide is the same as in Example 1;

[0042] (2) Magnetic Fe 3 o 4 The preparation is with embodiment 1;

[0043] (3) Preparation of magnetic graphene oxide supported phosphine Schiff base palladium:

[0044] Weigh 200 mg of the graphene oxide prepared in the above step (1) into a beaker, add 53 g of DMF solution containing dopamine, wherein the mass fraction of dopamine is 15%, ultrasonically disperse for 90 min, and the resulting solution is stirred and reacted at 90 ° C for 180 min , cooled to room temperature, centrifuged, washed with deionized water and ethanol in sequence, dried in vacuum at room temperature for 12 hours, and aminated graphene oxide (GO-NH 2 );

[0045] 100mgGO-NH 2 Add 50g of 2-diphenylphosphinebenzaldehyde in ethanol solution, wherein the mass fraction of 2-diphenylphosphinebenzaldehyde is 8%, ultrasonic treatment for 160min, the resulting solution was stirred and reacted at 85°C for 360min, cooled to room tem...

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Abstract

The invention discloses a magnetic oxidized graphene loaded phosphine Schiff base palladium catalyst and a preparing method and application thereof. Oxidized graphene prepared through an improved Hummers method serves as a catalyst carrier, phosphine Schiff base serves as ligand, palladium salt serves as an active component, the loading capacity of palladium particles accounts for 5.0-10.0% of the total mass of the catalyst, and the particle size is 5-15 nm. The prepared catalyst is high in stability and capable of preventing precious metal palladium from aggregating or losing; the catalyst has high catalytic activity and can efficiently promote the Heck coupled reaction; more importantly, due to good magnetic response, the catalyst can be fast recovered and reused through simple magnetic separation under the action of an external magnetic field, and practicability is high.

Description

technical field [0001] The invention relates to a catalyst, in particular to a preparation method and application of a magnetic graphene oxide-supported phosphine Schiff base palladium catalyst, and belongs to the technical field of catalysis. Background technique [0002] Schiff base, also known as imine (-RC=N-), is an important class of nitrogen-containing organic compounds. Its synthesis is relatively easy. Various Schiff bases. N on the Schiff base structure has a lone pair of electrons, which can form complexes with various metal ions, so Schiff base compounds play an important role in coordination chemistry. Although the complexes formed by mononuclear, dinuclear and polynuclear Schiff bases and metal ions are widely used in the fields of medicine, materials and catalysis. However, traditional small molecule Schiff bases have disadvantages such as difficult recovery and difficult reuse. In order to solve these limitations, supported Schiff base metal complexes have...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C2/88C07C15/52
CPCB01J31/28B01J2531/0213B01J2531/824C07C2/88C07C2531/28C07C15/52
Inventor 刘想赵晓华朱建军石秋忠杨晔徐吉成陆道明
Owner 南京申基医疗科技有限公司
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