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Process for preparing multiphase catalysts for ester exchange synthesizing diphenyl carbonate

A technology of diphenyl carbonate and heterogeneous catalysts, which is applied in the direction of organic carbonate preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of separation, recovery and environmental pollution, and achieve low cost and low raw material price The effect of being cheap and easy to obtain and the preparation method is simple

Active Publication Date: 2008-09-03
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the yield of diphenyl carbonate on homogeneous catalysis is high, there are problems such as separation, recovery and environmental pollution.

Method used

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  • Process for preparing multiphase catalysts for ester exchange synthesizing diphenyl carbonate
  • Process for preparing multiphase catalysts for ester exchange synthesizing diphenyl carbonate
  • Process for preparing multiphase catalysts for ester exchange synthesizing diphenyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First, 100-250 mesh SiO 2 Activation at 600°C for 6 hours, vacuum treatment for 8 hours, vacuum degree -0.095~-0.08MPa, weigh 2.4g of it in 80ml of anhydrous ethanol solution containing titanocene dichloride, TiO 2 with SiO 2 The molar ratio is 1:20, triethylamine is added under the protection of nitrogen, the molar ratio of triethylamine to titanocene dichloride is 1, reflux dipping for 8h, filtering, washing, drying overnight at 100-120°C, and then Calcined at 600°C for 6h to obtain the catalyst.

[0023] Embodiment 2 carries out the transesterification reaction of dimethyl carbonate and phenol with the catalyst prepared in embodiment 1

[0024] (1) in the there-necked flask that is connected with air guide tube and thermometer, constant pressure dropping funnel and rectifying column, add the catalyst 1.0 gram of embodiment 1;

[0025] (2) under feeding nitrogen, add 15 grams of phenol;

[0026] (3) When heated to 178° C., start to add dimethyl carbonate (DMC) dro...

Embodiment 3

[0028] The preparation step of embodiment 3 catalyst is the same as embodiment 1, but changes TiO 2 Precursors, as shown in Table 1. Carry out the transesterification reaction of dimethyl carbonate and phenol with the prepared catalyst, the reaction conditions are the same as in Example 2, and the activity results are shown in Table 1.

[0029] Table 1 Different TiO 2 Effect of Precursors on Catalyst Activity

[0030]

[0031] * MPC-methylphenyl carbonate, DPC-diphenyl carbonate

Embodiment 4

[0033] The preparation step of catalyst is the same as embodiment 1, but changes TiO 2 with SiO 2 The molar ratio is shown in Table 2. The prepared catalyst was used to carry out the transesterification reaction of dimethyl carbonate and phenol, the reaction conditions were the same as in Example 2, and the activity results were shown in Table 2.

[0034] Table 2 Different TiO 2 / SiO 2 The effect of molar ratio on catalyst activity

[0035]

[0036] * MPC-methylphenyl carbonate, DPC-diphenyl carbonate

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Abstract

The invention relates to a method for preparing a multiphase catalyst used for ester exchange synthesis of diphenyl carbonate from methyl carbonate and phenol. The catalyst is obtained by immersion-graft reaction of SiO2 as carrier, TiO2 as active component and triethylamine in the presence of organic solvents, followed by calcination. The invention solves the problem of low ester exchange efficiency in the prior art. The TiO2 / SiO2 catalyst prepared by the inventive method has higher catalytic activity and ester exchange selectivity in the ester exchange synthesis of diphenyl carbonate from methyl carbonate and phenol, wherein the phenol conversion rate reaches 48.1% and the overall selectivity of ester exchange products (methoxyphenyl carbonate and diphenyl carbonate) is more than 99.5%. Additionally, the inventive method has the advantages of easily-available raw materials, low cost and simple process.

Description

technical field [0001] The invention discloses a preparation method of a heterogeneous catalyst for transesterifying dimethyl carbonate and phenol to synthesize diphenyl carbonate. Background of the invention [0002] Diphenyl carbonate is an important chemical intermediate, which can synthesize many organic compounds and polymer materials through halogenation, nitration, hydrolysis, ammonolysis and other reactions, especially it can replace highly toxic phosgene and bisphenol A through melting ester Polycarbonate with excellent performance was synthesized by exchange reaction. At present, the synthesis of diphenyl carbonate mainly adopts phosgene method, transesterification method and oxidative carbonylation method. Due to the high toxicity and strong corrosiveness of phosgene, the traditional phosgene method has great safety and environmental problems, and is being gradually eliminated; the oxidative carbonylation method has not yet been reported on industrialization due ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06C07C68/06C07C69/96
Inventor 陈彤罗淑文王公应雷永诚曾毅姚洁
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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