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 an application method is applied in the field of rod-shaped nano-CeO2-supported Pd catalyst and its preparation, which can solve the problems of difficult post-processing, slow reaction rate, large amount of auxiliary agents, etc., and achieves difficult recycling and low cost. , the effect of high activity

Active Publication Date: 2014-03-05
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 out 0.064g PdCl 2 (Containing Pd0.038g), and dissolve it in 5mL 25% ammonia water;

[0031] (2) Weigh 6.0g Ce(NO 3 ) 3 ·6H 2 O, (theoretically get CeO 2 2.379g) Mix it with 84.2g NaOH (2.104mol) in solid form, add 150mL deionized water, stir to obtain a suspension;

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

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

[0034] (5) The solid material obtained after drying is calcined at 500°C for 4 hours to obtain rod-shaped nano CeO 2 Support Pd catalyst.

[0035] The prepared catalyst was characterized by transmission electron microscope, the results are as follows ...

Embodiment 2

[0037] The rod-shaped nano CeO prepared in Example 1 2 The supported Pd catalyst is used for the 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 of tetrabutylammonium bromide (0.0017mol) were added to the tank reactor, and then 4g of dehydrating agent 4A molecular sieve and 20mL of solvent dichloromethane were added to the reactor; filled with 0.6MPa oxygen and 6MPa carbon monoxide, React at 100°C for 4 hours. The reaction liquid was filtered under reduced pressure to separate the catalyst and the reaction liquid, and the reaction liquid was analyzed by liquid chromatography. The yield of diphenyl carbonate was 39.1%.

Embodiment 3～5

[0040] The preparation method is the same as in Example 1, except that the Ce(NO 3 ) 3 ·6H 2 The amount of O was 9.0g, 4.5g and 3.0g respectively, and the prepared Pd loading amount (Pd / CeO 2 Mass ratio) of rod-shaped nano CeO 2 Support 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 Supported Pd catalyst and preparation method thereof, specifically, relates to a rod-shaped nano CeO used for the reaction of phenol, carbon monoxide and oxygen to synthesize diphenyl carbonate 2 Supported Pd catalyst and its preparation method. Background technique [0002] Diphenyl carbonate is non-toxic and pollution-free. It is an important environmentally friendly chemical product. It 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 produce polycarbonate and p-hydroxyl Methyl benzoate, monoisocyanate, diisocyanate, etc. In recent years, because polycarbonate has been widely used in electronic appliances, machinery, aviation, transportation, construction, agriculture, textiles, medical and other fields, and the supply exceeds demand, the demand for its raw material diphenyl carbonate has increa...

Claims

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Application Information

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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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