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Catalyst for synthesizing diphenyl carbonate used in non-homogeneuos oxidation carbonylation and method for preparing the same

A heterogeneous oxidation, diphenyl carbonate technology, applied in the preparation of carbon dioxide or inorganic carbonate, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the difficulty of catalyst recovery, problems such as low selectivity and yield, to achieve the effect of simple and convenient preparation process, simple preparation and lower production cost

Inactive Publication Date: 2008-03-26
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the catalysts used in the synthesis of DPC by oxidative carbonylation at home and abroad are liquid-phase catalysts. The disadvantages are that the recovery of the catalyst is difficult, and the selectivity and yield are relatively low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of Mn-Cu double metal oxides by co-precipitation method: take 4.1g MnSO 4 ·H 2 O, add 15ml of deionized water to dissolve and prepare a solution; another 0.9g CuSO 4 , add 15ml of deionized water to make a solution; mix the two solutions, add 4ml of 20% sodium carbonate aqueous solution for precipitation, and keep stirring, filter after aging for 24 hours, and then dry the precipitate in vacuum Drying in an oven at 100°C for 12 hours; then roasting the dried material in a muffle furnace at 600°C for 7 hours to obtain a manganese-based composite oxide carrier;

[0027] Take PdCl 2 Dissolve 40mg in 40ml of deionized water, adjust the pH value of the solution to about 1 with concentrated hydrochloric acid, and heat to dissolve; add the manganese composite oxide carrier prepared above into the solution, and adjust the pH value to 8 with NaOH solution to precipitate The active component was stirred continuously for 2 hours, then filtered, dried, and finally c...

Embodiment 2

[0030] Mn-Ce bimetallic oxides were prepared by indirect mechanical grinding method, taking 4.2 g MnSO 4 ·H 2 0, add 15ml deionized water to dissolve, be mixed with solution; Add 4ml concentration and be 20% sodium carbonate aqueous solution and carry out precipitation, and aging 10 hours, filter, obtain manganese carbonate precursor; Then manganese carbonate precursor is in vacuum oven Dry for 12 hours; then bake the dried product in a muffle furnace at 600°C for 7 hours to obtain manganese oxide; take another 0.8g CeO 2 , mix and stir the two oxides on a grinder evenly, dry the mixture in a vacuum oven at 100°C for 12 hours; then bake the dried product in a muffle furnace at 500°C for 8 hours to obtain a manganese-based oxide catalyst support;

[0031] Take PdCl 2 Dissolve 40 mg in 40 ml of deionized water, adjust the pH value of the solution to about 1 with concentrated hydrochloric acid, then heat to dissolve, add the above-mentioned manganese composite oxide catalyst c...

Embodiment 3

[0034] Mn-Pb double metal oxides were prepared by direct mechanical milling method, taking 3.2 g MnCO 3 , another 1.8g PbCO 3 , mix and stir the two salts on a grinder evenly, dry the mixture in a vacuum oven at 100°C for 12 hours; Catalyst carrier;

[0035] Take PdCl 2 Dissolve 40 mg in 40 ml of deionized water, drop the pH value of the solution to about 1 with concentrated hydrochloric acid, then heat and dissolve, add the manganese composite oxide catalyst carrier prepared above into the solution, and then add NaOH alkali solution to adjust the pH value to 9, to precipitate active components, and kept stirring for 3 hours, then filtered, dried, and finally roasted at 200°C for 3 hours to obtain the final catalyst, with a palladium loading of 0.5%;

[0036] Get 1.0g above-mentioned prepared catalyst, 47g phenol, 1g tetrabutylammonium bromide, 74mg benzoquinone respectively and join in the autoclave of 250ml, pass into O 2 The pressure of CO is 0.3MPa, the pressure of CO...

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Abstract

The present invention relates to a catalyst for synthesizing diphenyl carbonate by utilizing heterogeneous oxidation carbonylation and preparation method of said catalyst. Said preparation method includes the following steps: making palladium salt be loaded on the manganese series composite metal oxide carrier, said manganese series composite metal oxide carrier is formed from manganese oxygen compound and metal oxide of any one kind or more than one kind of La, Ce, Ti, Zr, V, Cr, Mo, W, Fe, Co, Ni, Cu, Ag, Zn, Bi, Pb and Sn, the loaded quantity of active component Pd is 0.01wt%-10wt%, utilizing impregnating process, precipitation process or mixed fuel burning process to make the active component palladium salt be loaded on the manganese series composite metal oxide carrier, drying and calcining for 1-8h at 200-600deg.C so as to obtain the invented solid catalyst. Said catalyst can be used for preparing diphenyl carbonate, its productivity is up to 22.0% and its selectivity is up to 98.3%.

Description

technical field [0001] The invention relates to a catalyst for synthesizing diphenyl carbonate by heterogeneous oxidative carbonylation and a preparation method of the catalyst. Background technique [0002] Polycarbonate (PC) is the only product with transparency among the five general-purpose engineering plastics, and it is also the fastest-growing general-purpose engineering plastic in recent years. It has a wide range of applications in machinery manufacturing, electronics, military, security, and optical fiber communication application. The production methods of PC mainly include phosgene interfacial polycondensation method and non-phosgene melt transesterification method. The former causes environmental pollution due to the use of a large amount of highly toxic phosgene; the latter has attracted much attention because it is good for the environment. [0003] Diphenyl carbonate (DPC) is one of the raw materials for the synthesis of PC by melt transesterification. The s...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/656C07C69/96C07C68/04
CPCY02P20/141
Inventor 吴元欣杜治平刘敏袁华杨小俊戈军伟邬茂
Owner WUHAN INSTITUTE OF TECHNOLOGY
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