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Catalyst for synthesis of aromatic phenyl car bonate and its preparing method

A technology of phenyl carbonate and catalyst, which is applied in the field of catalysts and preparations for the synthesis of aromatic phenyl carbonate, can solve problems such as low selectivity and yield, difficulty in catalyst recovery, and complicated separation process, so as to improve yield and selectivity Sexuality, simplification of the subsequent separation process, and the effect of reducing costs

Inactive Publication Date: 2004-01-28
WUHAN CHEM COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the phosgene method is serious pollution; the main problem of the transesterification method is that the reaction time is long, and the follow-up separation process is relatively complicated; while the oxidative carbonylation method uses CO, O 2 Using phenyl ester as a raw material to synthesize DPC in the next step under the action of a catalyst is not only simple in process, but also pollution-free, which is a green synthesis method
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

[0017] Weigh 15g Mn(NO 3 ) 2 , 12g La(NO 3 ) 3 , 5g Co(NO 3 ) 3 and 20g of citric acid were dissolved in an aqueous solution and stirred until dissolved, and after stirring for 12 hours, the solution was evaporated to dryness to obtain the matrix of the carrier, which was placed in an oven to dry at 100-120°C, and then placed in an oven after 4-6 hours Calcining at 500-700° C. for 5-8 hours to obtain a catalyst carrier.

[0018] Take Na 2 PdCl 4 0.1 g was dissolved in 30 ml of distilled water, and the above-mentioned carrier was added thereto, and then NaOH alkali solution was added to precipitate the active component and stirred continuously for 8-12 hours, then filtered, and the filter cake was dried in a drying oven to obtain the final catalyst.

[0019] Take 1.0g of catalyst, 50g of phenol, and 1g of tetrabutylammonium bromide into a 100ml autoclave, the reaction temperature is 40-100°C, the reaction pressure is 35MPa, the reaction time is 3 hours, and the liquid a...

Embodiment 2

[0029] Weigh 15g Mn(NO 3 ) 2 , 12g La(NO 3 ) 3 , 5g Pb(NO 3 ) 2 , 5g Ce(NO 3 ) 3 Mix evenly with the mother body and dissolve 20g of citric acid in the aqueous solution and stir until dissolved. After stirring for 12 hours, evaporate the solution to dryness to obtain the mother body of the carrier, and place it in an oven to dry at 100-120°C for 4-6 hours Then place it at 500-700° C. and bake it for 5-8 hours to obtain a catalyst carrier.

[0030] Take Na 2 PdCl 4 0.1 g was dissolved in 30 ml of distilled water, and the above-mentioned carrier was added thereto, and then NaOH alkali solution was added to precipitate the active component and stirred continuously for 8-12 hours, then filtered, and the filter cake was dried in a drying oven to obtain the final catalyst.

[0031] Take 1.0g~1.5g of catalyst, 50g of phenol, and 1g of tetrabutylammonium bromide into a 100ml autoclave respectively. The reaction temperature is 40~100°C, the reaction pressure is 3~4MPa, and th...

Embodiment 3

[0041] Weigh 15g Mn(NO 3 ) 2 , 12g La(NO 3 ) 3 , 5g Pb(NO 3 ) 2 and 20 g of citric acid were dissolved in the aqueous solution and stirred until dissolved. After stirring for 24 hours, the solution was evaporated to dryness to obtain a precursor of the carrier. Place the precursor in an oven at 100-120°C for 4-6 hours and then place it at 500-700°C for 5 hours, then add Sn salt (10-50%) and roast to obtain the catalyst carrier .

[0042] Take Na 2 PdCl 4 Dissolve 0.1 g in 30 ml of distilled water, add the above-mentioned carrier, then add NaOH alkali solution to precipitate the active component and keep stirring for 8-12 hours, then filter, and dry the filter cake in a drying oven to obtain the final catalyst.

[0043] Take 1-1.5g of catalyst, 50g of phenol, and 1g of tetrabutylammonium bromide into a 100ml autoclave respectively. The reaction temperature is 40-100°C, the reaction pressure is 3-8MPa, and the reaction time is 3-6 hours. The reacted liquid was diluted...

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Abstract

The present invention relates to a catalyst for synthesizing aromatic diphenyl carbonate by means of heterogeneous oxidative carbonylation and its preparation method. Said catalyst is made up by loading Pd or group VIII of periodic table of elements on the compound metal oxide La1-xPbxByMnO3 (B=Sn, Ce, Ti and Co) as carrier, X and Y are equal to 0-1, and the loading quantity of active component Pd is 0.01-10% (wt). Said catalyst carrier is prepared by adopting citric acid complexation process, then the active substance palladium salt is loaded on the carrier, and roasted at 200-500 deg.c so as to obtain the required solid catalyst. The maximum yield and selectivity of the diphenyl carbonate are respectively up 26% and 98%.

Description

technical field [0001] The invention relates to a catalyst for synthesizing aromatic phenyl carbonate by heterogeneous oxidative carbonylation, especially diphenyl carbonate, a preparation method thereof, and a method for preparing diphenyl carbonate with the catalyst. Background technique [0002] Polycarbonate (PC) is one of the five general-purpose engineering plastics and is widely used in many fields. Usually adopt two kinds of methods to produce PC in the prior art, promptly take dichloromethane as solvent, produce PC with bisphenol A and phosgene reaction, or carry out transesterification production under molten state bisphenol A and diphenyl carbonate (DPC) PC. The former causes environmental pollution due to the use of a large amount of highly toxic phosgene, and the use of methylene chloride also aggravates the corrosion of equipment; the latter is a green process because it does not use solvents in the preparation process and is pollution-free. [0003] At prese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C68/00C07C69/96
Inventor 吴元欣张光旭吴广文马沛生田琦峰李定或
Owner WUHAN CHEM COLLEGE
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