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Catalyst of composite oxides of molybdenum, cupper bimetal in use for synthesizing diphenyl carbonate through ester exchange

A technology of composite oxides and diphenyl carbonate, applied in the preparation of organic carbonates, etc., can solve the problems of product and catalyst separation and recovery difficulties, and achieve the effects of easy separation, good stability, and no pollution to the environment

Inactive Publication Date: 2007-02-21
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In DE 344552 and JP 63-92662, it is shown that most of the catalyst used by the author in the transesterification reaction is an organic compound of Ti and Sn, such as n-butyl carbonate [Ti(OC 4 h 9 ) 4 ], dibutyl tin oxide [(C 4 h 9 )SnO], butyl tin trichloride [C 4 h 9 SnCl 3 ], aluminum phenoxide [Al(OPh) 3 ] etc., this type of homogeneous catalyst shows better catalytic performance, and the yield of diphenyl carbonate is higher, but there are problems in the homogeneous catalytic system that the product is separated from the catalyst and difficult to recycle, and the prices of organotin and titanium more expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 2g (NH 4 ) 6 Mo 7 o 24 4H 2 O and 0.135g basic copper carbonate, so that Mo / Cu (molar ratio) = 1 / 0.1, mix; add absolute ethanol to the above mixed powder, mechanically grind for 0.5 ~ 1h; put the solid mixed sample in an oven at 110°C Dry for 4 hours in a muffle furnace at 550°C for 10 hours, take out and grind to obtain a bimetallic composite oxide catalyst. In a three-necked beaker connected with a nitrogen inlet tube, a constant pressure dropping funnel, a thermometer and a rectification column, add 0.72 g of the prepared catalyst and 15 g of phenol. When the temperature rises to 175°C, start to add dimethyl carbonate dropwise. The total amount of dimethyl carbonate added is 13.5ml. The reaction time is calculated from the beginning of dropwise addition of dimethyl carbonate, and the reaction is 9 hours; Azeotrope of Methanol and Dimethyl Carbonate. The mixed fraction and the reaction liquid containing the products methyl phenyl carbonate and diphenyl carb...

Embodiment 2

[0033]The preparation method of the catalyst is the same as in Example 1, and the molar ratio of molybdenum and copper is adjusted to make Mo / Cu=1 / 0.25. The analysis method of reaction condition and product is the same as embodiment 1, and the activity result of catalyst is as follows: the conversion rate of phenol is 40.63%, and the productive rate of methylphenyl carbonate and diphenyl carbonate is respectively 15.3% and 23.31%.

Embodiment 3

[0035] The preparation method of the catalyst is the same as in Example 1, and the molar ratio of molybdenum and copper is adjusted to make Mo / Cu=1 / 0.35. The analysis method of reaction condition and product is the same as embodiment 1, and the activity result of catalyst is as follows: the conversion ratio of phenol is 40.29%, and the productive rate of methylphenyl carbonate and diphenyl carbonate is respectively 10.94% and 26.33%.

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Abstract

A catalyst with high activity and selectivity and able to be recovered easily for preparing diphenyl carbonate from dimethyl carbonate and phenol ester by ester exchange is basically and proportionally prepared from the oxide of Mo and the oxide of Cu through co-deposition or grinding, and calcining at 300-900 deg.C.

Description

technical field [0001] The invention belongs to a bimetallic composite oxide heterogeneous catalyst, in particular to a molybdenum-copper composite metal oxide catalyst for synthesizing diphenyl carbonate by transesterification of dimethyl carbonate and phenol. Background technique [0002] Diphenyl carbonate is an important intermediate material with low toxicity and no pollution. It can be used to synthesize many important organic compounds and polymer materials, especially it can replace the highly toxic substance phosgene and bisphenol A. The production performance is excellent of polycarbonate. At present, the synthesis methods of diphenyl carbonate mainly include phosgene method, phenol oxidative carbonylation method, and transesterification method. Due to the use of highly toxic and highly corrosive substance phosgene, the phosgene method has seriously polluted the environment and has been gradually eliminated; although the oxidative carbonylation method has a high a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/885C07C68/06C07C69/96
Inventor 王公应童东绅胡续腾曾毅王越陈彤姚洁雷永诚石大川李正张德胜
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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