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Method for preparation of diphenyl carbonate by ester interchange

A technology of diphenyl carbonate and dimethyl carbonate, applied in the field of transesterification to prepare diphenyl carbonate, can solve the problems of easy deactivation, heterogeneous catalyst activity, low selectivity, etc.

Active Publication Date: 2015-11-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the prior art has the problems of heterogeneous catalyst activity, low selectivity, and easy deactivation, and a new method for preparing diphenyl carbonate by transesterification is provided

Method used

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  • Method for preparation of diphenyl carbonate by ester interchange

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 9.0gSnCl 2 2H 2 O and 38.1gGa(NO 3 ) 3 Dissolve in 500mL water, add 300mL aqueous solution containing 29.3g anhydrous sodium carbonate to it, collect the obtained precipitate, wash with deionized water 3 times, each time 1000mL, and dry the obtained precipitate in an oven at 120°C for 24 hours , fired at 600°C for 5 hours to obtain SnO 2 / Ga 2 o 3 Mixed oxide catalyst MO-1, in which SnO and Ga 2 o 3 The parts by weight are respectively 30 parts and 70 parts.

Embodiment 2～15

[0022] The mixed metal oxide catalyst obtained is shown in Table 1 by changing the type and amount of mixed metal salts and precipitants used, and keeping the rest of the conditions unchanged.

[0023] Table 1

[0024]

Embodiment 16

[0026] Take by weighing 10g of the MO-1 catalyst prepared by the above [Example 1] and place it in a 300mL stainless steel reactor, add N 2 Replace the air in the reactor, then fill with 50.0g phenyl acetate and 14.1g dimethyl carbonate, heat up to 175°C, react for 5 hours and then cool down, the reaction product is chromatographically analyzed to obtain the conversion of dimethyl carbonate (DMC) The yield was 87.9%, the selectivity of diphenyl carbonate (DPC) was 46.5%, and the selectivity of methylphenyl carbonate (MPC) was 52.9%.

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Abstract

The invention relates to a method for preparation of diphenyl carbonate by ester interchange, and mainly solves the problems that a heterogeneous phase catalyst has low activity and selectivity, and proneness to inactivation. In the invention, dimethyl carbonate and phenyl acetate, whose mol ratio ranges from 0.1 to 5, serve as materials, react in the presence of a catalyst for 1-20 hours at a temperature of 120-190 DEG C to prepare diphenyl carbonate, wherein the weight ratio of the catalyst to the phenyl acetate ranges from 0.01 to 0.5, the catalyst is a mixture of two metal oxides AaOb / BcOd; A is selected from Sn, Mn or Bi, and B is selected from Al, Ga, Fe, In, Zr or Cr. The method for preparation of diphenyl carbonate by ester interchange solves problems well and can be used in ester interchange of dimethyl carbonate and phenyl acetate for preparing diphenyl carbonate.

Description

technical field [0001] The invention relates to a method for preparing diphenyl carbonate by transesterification. Background technique [0002] Diphenyl carbonate is a raw material for the preparation of polycarbonate by non-phosgene method. The traditional preparation method is phosgene method, which is subject to policy restrictions due to the potential harm of highly toxic phosgene to the environment and safe production. Synthesis of diphenyl carbonate (DPC) by transesterification of phenol (PhOH) and dimethyl carbonate (DMC) under the action of a catalyst is currently the only industrialized non-phosgene synthesis route of diphenyl carbonate. However, this route has the problems of low equilibrium conversion and high energy consumption for the separation of DMC and methanol azeotrope. The route of transesterification between dimethyl carbonate and phenyl acetate (PA) to generate diphenyl carbonate has the advantages of high equilibrium conversion rate, no azeotropic com...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
Inventor 陈梁锋何文军
Owner CHINA PETROLEUM & CHEM CORP
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