The preparation method of diphenyl carbonate compound

A technology of diphenyl carbonate and diester carbonate, which is applied in the field of preparation of diphenyl carbonate compounds, and can solve the problems of low selectivity, low utilization rate of raw materials, and non-environmental protection

Active Publication Date: 2021-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The object of the present invention is to provide a kind of preparation method of diphenyl carbonate compound in order to overcome the low selectivity of the method for preparing diphenyl carbonate compound of the prior art, low raw material utilization rate and environmental protection, by the present invention The method for preparing diphenyl carbonate compounds can improve the selectivity of diphenyl carbonate compounds; and, the catalyst is easy to separate, recycle and reuse from the reaction solution, without negative impact on the environment, and is suitable for large-scale industry Production

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  • The preparation method of diphenyl carbonate compound
  • The preparation method of diphenyl carbonate compound
  • The preparation method of diphenyl carbonate compound

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preparation example Construction

[0018] The present invention provides a method for preparing diphenyl carbonate compounds represented by formula (I), wherein the preparation method comprises: in the presence of a catalyst, making phenyl acetate compounds represented by formula (II) and The carbonic acid diester compound shown in (Ⅲ) is transesterified, and the catalyst contains 1,4-diazabicyclo[2.2.2]octane;

[0019]

[0020] where R is hydrogen or C 1 -C 4 the alkyl group, R 1 and R 2 are each independently methyl or ethyl.

[0021] Preferably, the catalyst is 1,4-diazabicyclo[2.2.2]octane.

[0022] In the present invention, preferably, R is hydrogen, methyl or ethyl, more preferably hydrogen or methyl, even more preferably hydrogen.

[0023] In the present invention, preferably, R in formula (II) is at the para-position of the ester group.

[0024] Specific examples of the phenyl acetate compounds represented by the above formula (II) include: phenyl acetate, p-cresol acetate, p-ethylphenol acetat...

Embodiment approach

[0041] According to a preferred embodiment of the present invention, the preparation method comprises: first mixing the phenyl acetate compound shown in formula (II) with the catalyst, and heating the obtained mixture to the temperature required for the transesterification reaction , and then the carbonic acid diester compound represented by formula (III) is mixed with the mixture.

[0042] According to another preferred embodiment of the present invention, the preparation method comprises: mixing the catalyst, the phenyl acetate compound shown in formula (II) and the carbonic acid diester compound shown in formula (III), to obtain The mixture is heated to the temperature required for the transesterification reaction, and after 2-5 hours of reaction, an entrainer is added to the reaction solution.

[0043] In the present invention, in order to improve the conversion rate of reactants and product selectivity, preferably, the entrainer is added to the reaction solution in 2-3 ti...

Embodiment 1

[0070] Under the protection of nitrogen, mix 20.42g of phenyl acetate and 3.36g of 1,4-diazabicyclo[2.2.2]octane in a three-necked round bottom flask equipped with a separator, and the temperature of the oil bath reaches 80°C After that, add 6.76g dimethyl carbonate (the molar ratio of phenyl acetate, 1,4-diazabicyclo[2.2.2]octane and dimethyl carbonate is 1:0.2:0.5), under normal pressure (0.1 MPa) conditions, the methyl acetate and its azeotrope generated by the simple distillation method are steamed to the liquid separator and removed while reacting. After reacting for 2 hours, cool for about 6 minutes, add entrainer toluene to the round bottom flask, add 2 times in total, the time interval between two adjacent additions is 3 hours, and add 5mL toluene each time. The reaction ended after a total of 9 hours, and the catalyst was recovered by rectification. The reaction liquid is carried out to gas chromatographic analysis, phenyl acetate conversion rate 77.1%, the selectivi...

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Abstract

The present invention relates to the field of diphenyl carbonate compounds, and discloses a preparation method of a diphenyl carbonate compound represented by formula (I), wherein the preparation method comprises: in the presence of a catalyst, making the formula (II) The shown phenyl acetate compound and the carbonic acid diester compound shown in formula (Ⅲ) carry out transesterification reaction, and described catalyst contains 1,4-diazabicyclo[2.2.2]octane; Wherein, R is hydrogen or C 1 -C 4 the alkyl group, R 1 and R 2 are each independently methyl or ethyl. The method can improve the selectivity of diphenyl carbonate compounds; the adopted catalyst has stable chemical properties, is safe, is cheap and does not corrode equipment; meanwhile, the catalyst is easy to separate, recover and reuse from the reaction liquid.

Description

technical field [0001] The invention relates to the field of diphenyl carbonate compounds, in particular to a preparation method of diphenyl carbonate compounds. Background technique [0002] As an important fine chemical intermediate, diphenyl carbonate (DPC) is mainly used to replace phosgene for polycondensation reaction with bisphenol A to synthesize polycarbonate (PC). , Optical and electronic properties, widely used in automobile manufacturing, construction, medical, aerospace and other fields. In addition, DPC can be used to synthesize some other chemical products, such as polyaryl carbonate, monoisocyanate, etc., and can also be used as a plasticizer for polyamide and polyester. In recent years, with the promotion and application of polycarbonate clean production technology in the world, the market demand for DPC has grown rapidly. Therefore, the research and development of DPC green and efficient production technology has become the focus of university laboratorie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/06C07C69/96
CPCC07C68/06C07C69/96
Inventor 谢伦嘉王大韡刘青曾佳
Owner CHINA PETROLEUM & CHEM CORP
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