Complex metal oxide catalyst for synthesis of diphenyl carbonate by ester exchange reaction and preparation method thereof

A technology of diphenyl carbonate and composite metal, applied in metal/metal oxide/metal hydroxide catalyst, organic carbonate preparation, catalyst activation/preparation, etc., can solve unstable performance, difficulty in separation and recovery of catalyst, cost Expensive and other problems, to achieve the effect of good stability, good economic and social benefits, and no corrosion of equipment

Inactive Publication Date: 2010-12-08
CHANGZHOU INST OF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problems existing in the prior art such as difficult catalyst separation and recovery, high price, and unstable performance, the present invention provides a composite metal oxide catalyst for the heterogeneous catalytic synthesis of diphenyl carbonate by transesterification reaction and its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1, take by weighing 20.0 grams of ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 ? h 2O) (containing about 11 grams of molybdenum) was dissolved in distilled water to make a 30% (mass percent) solution; then it was mixed with the prepared 20% (volume percent) acetic acid solution by a parallel flow method, and 50ml was added dropwise n-Butyl titanate (containing about 7.0 grams of titanium), stirred, precipitated, and vacuum filtered; the resulting precipitate or gel was dried in an oven at 90-120°C for 12 hours; the dried precipitate was placed in a muffle furnace Calcined at 400°C for 3 hours and taken out to obtain a molybdenum-titanium composite metal oxide catalyst.

[0039] 2. Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 12.0 grams of dimethyl carbonate (about 0.13 mol) and 5.0 grams of the prepared molybdenum-titanium composite oxide catalyst and add them to a 250ml high-pressure reactor with an intelligent constant temperature controller , sealed with fa...

Embodiment 2

[0042] 1. Weigh sodium molybdate (Na 2 MoO 4 ? h 2 (0) 20.0 grams (containing about 7.9 grams of molybdenum) are dissolved in distilled water to be made into a 40% (mass percent) solution; then it is mixed with the prepared 20% (volume percent) nitric acid solution in parallel flow, and simultaneously, Add 45ml of isopropyl titanate (containing about 6.8 grams of titanium) dropwise, stir, precipitate, and vacuum filter; dry the resulting precipitate or gel in an oven at 90-120°C for 12 hours; dry the dried precipitate in a horse Calcined in a Furnace at 500°C for 5 hours and taken out to obtain a molybdenum-titanium composite metal oxide catalyst.

[0043] 2. Weigh 80.0 grams of phenyl acetate (about 0.60 mol), 25.0 grams of dimethyl carbonate (about 0.28 mol) and 3.0 grams of the prepared molybdenum-titanium composite oxide catalyst and add them to a 250ml high-pressure reactor with an intelligent constant temperature controller , sealed with fasteners, and then confirmed...

Embodiment 3

[0046] 1. Weigh ammonium dimolybdate ((NH 4 ) 2 Mo 2 o 7 ) 20.0 grams (containing about 11.0 grams of molybdenum), dissolved in distilled water, and made into a 50% (mass percent) solution; Titanium (TiOSO 4 ? h 2 O) The solution (containing about 1.1 grams of titanium) is mixed, stirred, precipitated, and vacuum filtered by a parallel flow method; the resulting precipitate is dried in an oven at 90-120° C. for 12 hours; the dried precipitate or gel is Baking in a muffle furnace at a temperature of 500° C. for 3 hours, taking out the molybdenum-titanium composite metal oxide catalyst.

[0047] 2. Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 36.0 grams of dimethyl carbonate (about 0.40 mol) and 8.0 grams of the prepared molybdenum-titanium composite oxide catalyst and add them to a 250ml high-pressure reactor with an intelligent constant temperature controller , sealed with fasteners, and then confirmed the airtightness of the high-pressure airtight reaction ket...

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PUM

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Abstract

The invention discloses a complex metal oxide catalyst for synthesis of diphenyl carbonate by ester exchange reaction and a preparation method thereof. The catalyst basically consists of a molybdenum-titanium complex oxide, wherein the weight ratio of the molybdenum to the titanium is 100:10-100; the roasting temperature is between 300 and 600 DEG C; base raw materials for preparing the catalyst are a molybdenum compound and a titanium compound; and the preparation method adopts a coprecipitation method or mechanical grinding method. The catalyst has high catalytic activity and good selectivity for the reaction of synthesizing the diphenyl carbonate by ester exchange, and particularly has the advantages of simple preparation method, easy separation and recycling, no environmental pollution, no corrosion to equipment and the like, so the catalyst can be widely applied to production of the diphenyl carbonate.

Description

technical field [0001] The invention belongs to a composite metal oxide catalyst and a preparation method thereof, in particular to a molybdenum-titanium composite metal oxide catalyst for synthesizing diphenyl carbonate by transesterification and a preparation method thereof. Background technique [0002] Diphenyl carbonate [DPC] is non-toxic and non-polluting. It is an important "green" chemical product that can be used to synthesize many important organic compounds and polymer materials, especially to replace highly toxic phosgene and bisphenol A. Produces polycarbonate with excellent properties. [0003] The synthesis methods of diphenyl carbonate mainly include phosgene method, phenol oxidative carbonylation method and transesterification method. Because phosgene is highly toxic and will cause serious environmental pollution, the traditional phosgene method is being phased out. Although the oxidative carbonylation of phenol has simple and easy-to-obtain raw materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/28B01J37/03B01J37/00C07C69/96C07C68/06
Inventor 王公应曹平杨先贵唐聪明王越姚洁雷永诚康涛
Owner CHANGZHOU INST OF CHEM
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