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Schiff base complex catalyst for synthesizing diphenyl carbonate through oxidative carbonylation of phenol

A technology of diphenyl carbonate and catalyst, applied in the field of preparation of diphenyl carbonate, can solve the problems of low DPC yield, complex catalyst preparation process and the like, and achieve the effects of short preparation time and simple preparation process

Inactive Publication Date: 2012-07-18
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] Aiming at problems such as complex catalyst preparation process and low DPC yield in the existing reaction of phenol liquid-phase oxidative carbonylation to prepare diphenyl carbonate, the present invention provides a Schiff base for preparing phenol liquid-phase oxidative carbonylation to diphenyl carbonate Palladium complex catalyst and preparation method thereof, which can obviously simplify the catalyst preparation process and improve the selectivity of DPC

Method used

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  • Schiff base complex catalyst for synthesizing diphenyl carbonate through oxidative carbonylation of phenol
  • Schiff base complex catalyst for synthesizing diphenyl carbonate through oxidative carbonylation of phenol
  • Schiff base complex catalyst for synthesizing diphenyl carbonate through oxidative carbonylation of phenol

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preparation example Construction

[0032] The general reaction formula of the preparation Schiff base ligand involved in the present invention is:

[0033]

Embodiment 1

[0035] 1.0814g of o-phenylenediamine and 2.4424g of salicylaldehyde were respectively dissolved in 30mL of 90% absolute ethanol, and the ethanol solution of o-phenylenediamine was added dropwise to the ethanol solution of salicylaldehyde, and stirred at 60°C Reflux for 1 hour, and after cooling, columnar bright yellow crystals are precipitated, filtered, washed several times with absolute ethanol, and dried in a vacuum oven at 60°C to obtain o-phenylenediamine glycalaldehyde ligand L 1 .

[0036]Take 1mmol of ligand L 1 Dissolve in 30mL ethanol and tetrahydrofuran (volume ratio 2:1) mixed solvent, take 1mmol PdCl 2 Dissolve 2mmol KCl in 20mL double-distilled water, add the ligand solution drop by drop to the palladium solution, finish dripping for 10 minutes, stir thoroughly for 20 minutes, transfer to a microwave digestion tank, irradiate with microwaves at low fire for 3 minutes, and then follow the furnace Cool to room temperature, wash the precipitate with distilled wate...

Embodiment 2

[0043] 1.2020g of ethylenediamine and 4.8848g of salicylaldehyde were respectively dissolved in 30mL of 95% absolute ethanol, and the ethanol solution of ethylenediamine was added dropwise to the ethanol solution of salicylaldehyde, and stirred and refluxed at 80°C for 1h , yellow crystals were precipitated after cooling, filtered, washed with absolute ethanol several times, and dried in a vacuum oven at 80°C to obtain the desired ligand ethylenediamine salicylaldehyde L 2 .

[0044] Take 1mmol of ligand L 2 Dissolve in 20mL ethanol and DMF (volume ratio 1:1) mixed solvent, take PdCl 2 : KCl=1:2 (molar ratio, PdCl 2 content of 1 mmol) was dissolved in 20 mL of double-distilled water, and the ligand solution was added dropwise to the palladium solution. After fully stirring for 20 min, it was transferred to a microwave digestion tank, microwaved at low heat for 3 min, and then cooled to room temperature with the furnace. , washed with distilled water and ethanol, and dried i...

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Abstract

The invention discloses a catalyst for synthesizing diphenyl carbonate through liquid-phase oxidative carbonylation of phenol. The catalyst is of a homogeneous system taking a Schiff base palladium complex as a major catalyst and further comprises an inorganic redox assistant, an organic redox assistant and a surfactant, wherein the molar ratio of materials is as follows: the palladium: the inorganic redox assistant:the organic redox assistant: the surfactant=1:(5-20):(20-60):(80-120). Compared with the traditional catalyst for the liquid-phase oxidative carbonylation of the phenol, the catalyst disclosed by the invention is simple in preparation process and short in preparation time; the activity of the catalyst can be adjusted by altering the structure of the palladium complex; moreover, the catalyst has very high catalytic activity and selectivity; and the yield and selectivity of diphenyl carbonate can reach 60.0% and 95.9% at most.

Description

technical field [0001] The invention relates to the preparation of diphenyl carbonate, in particular to a catalyst for synthesizing diphenyl carbonate by liquid-phase oxidative carbonylation of phenol and its application. Background technique [0002] As a green, environmentally friendly, non-toxic, non-polluting, non-corrosive organic intermediate, diphenyl carbonate (DPC) is widely used in the synthesis of polycarbonate, methyl p-hydroxybenzoate, and monoisocyanate. At present, the production process of diphenyl carbonate mainly focuses on phosgene method, transesterification method and oxidative carbonylation method. The phosgene method uses highly toxic phosgene, which is very harmful to the environment and the human body, and the generated by-product HCl is corrosive to the equipment, so it is gradually being eliminated; while the transesterification method is limited by its own thermodynamic properties, The reaction is slow and the yield is low; while the oxidative ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C249/02C07C251/24C07D213/74C07F15/00C07C69/96C07C68/00
Inventor 程庆彦李超毅刘玉扑王延吉赵新强
Owner HEBEI UNIV OF TECH
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