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Catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as preparation method and application method of catalyst

A technology of diphenyl carbonate and its application method, which is applied in the field of rod-shaped nano-CeO2 supported Pd catalyst and its preparation, can solve the problems of difficult post-processing, slow reaction rate, large amount of additives, etc., and achieve difficult recycling and low cost , highly active effect

Active Publication Date: 2015-05-27
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Rod-shaped nano-CeO of the present invention 2 The preparation method of the supported Pd catalyst is simple, easy to operate and highly reproducible; the catalyst is a heterogeneous catalyst with high activity and selectivity, which is used for the oxidative carbonylation of phenol to diphenyl carbonate, and solves the problem of homogeneous Pd catalysts. and overcome the disadvantages of the existing heterogeneous catalyst system, such as slow reaction rate and long reaction time; at the same time, in the oxidative carbonylation of phenol, the use of auxiliary agents in the oxidative carbonylation of phenol is reduced, and only one It overcomes the shortcomings of the existing reaction system, such as large amount of additives, many types, difficult post-processing, and high cost.

Method used

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  • Catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as preparation method and application method of catalyst
  • Catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as preparation method and application method of catalyst
  • Catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as preparation method and application method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 0.064g PdCl 2 (containing Pd0.038g), and dissolved in 5mL of 25% ammonia water;

[0031] (2) Weigh 6.0g Ce(NO 3 ) 3 ·6H 2 O, (theory gives CeO 2 2.379g) was fully mixed with 84.2g NaOH (2.104mol) in the form of solid, and 150mL deionized water was added and stirred to obtain a suspension;

[0032] (3) Add the solution obtained in step (1) to the suspension obtained in step (2), and then transfer to a crystallization kettle lined with polytetrafluoroethylene. Put the crystallization kettle into an oven, and react for 24 hours at 110°C;

[0033] (4) After the reaction, the reaction mixture was taken out from the crystallization kettle, centrifuged, and the obtained solid was washed with deionized water, and then dried at 80°C for 20 hours;

[0034] (5) Calcining the dried solid material at 500°C for 4 hours to obtain rod-shaped nano-CeO 2 supported Pd catalyst.

[0035] The prepared catalyst was characterized by transmission electron microscopy, and the ...

Embodiment 2

[0037] With the rod-shaped nano-CeO that makes in embodiment 1 2 Supported Pd catalyst for oxidative carbonylation of phenol to prepare diphenyl carbonate.

[0038] 2.4g phenol (0.0255mol), 0.5g catalyst (calculated as Pd is 6.94×10 -5 mol) and 0.55g tetrabutylammonium bromide (0.0017mol) were added to the kettle reactor, and then 4g of dehydrating agent 4A molecular sieve and 20mL of solvent methylene chloride were added to the reactor; 0.6MPa oxygen and 6MPa carbon monoxide were charged, React at 100°C for 4 hours. The reaction solution was filtered under reduced pressure to separate the catalyst from the reaction solution, and the reaction solution was analyzed by liquid chromatography. The yield of diphenyl carbonate was 39.1%.

Embodiment 3~5

[0040] The same as the preparation method of Example 1, just change the Ce(NO 3 ) 3 ·6H 2 The amount of O was 9.0g, 4.5g and 3.0g, respectively, and different Pd loadings (Pd / CeO 2 mass ratio) rod-shaped nano-CeO 2 supported Pd catalyst.

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Abstract

The invention relates to a catalyst for synthesizing diphenyl carbonate in phenol oxidative carbonylation as well as a preparation method and an application method of the catalyst. The catalyst comprises carrier rod-shaped nanometer CeO3 and an active component Pd compound, wherein the Pd compound is based on Pd, the weight ratio of the Pd to the CeO2 is 0.1: (10:100). The catalyst is used for synthesizing the diphenyl carbonate in the phenol oxidative carbonylation, solving the separation problem of a homogeneous Pd catalyst and overcoming the shortcomings that a conventional heterogeneous catalyst system is low in reaction rate and long in reaction time, and the like; meanwhile, by using the catalyst, the using amount of additives is reduced in the phenol oxidative carbonylation, only one additive is used, and the defects such as large using amount of the additives, multiple varieties, high difficulty in aftertreatment and high cost of a conventional reaction system are overcome. In addition, according to the method, the catalyst has relatively high activity all the time in the reaction process and can be repeatedly used.

Description

technical field [0001] The invention relates to a rod-shaped nano CeO 2 Loaded Pd catalyst and preparation method thereof, specifically, relate to a kind of rod-shaped nano-CeO for phenol and carbon monoxide, oxygen reaction synthesis diphenyl carbonate 2 Supported Pd catalyst and preparation method thereof. Background technique [0002] Diphenyl carbonate is non-toxic and non-polluting. It is an important environmental chemical product that can be used to synthesize many important medicines, pesticides and other organic compounds and polymer materials; it can also be used in the plastics industry to manufacture polycarbonate and p-hydroxy Methyl benzoate, monoisocyanate, diisocyanate, etc. In recent years, since polycarbonate is widely used in electronic appliances, machinery, aviation, transportation, construction, agriculture, textile, medical and other fields, the supply exceeds demand, so the demand for its raw material diphenyl carbonate has greatly increased, making...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/63B01J32/00C07C69/96C07C68/00B82Y30/00B82Y40/00
Inventor 薛伟滕哲王志苗袁烨张东升王延吉
Owner HEBEI UNIV OF TECH
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