Method for synthesizing diaryl carbonic acid ester and dimethyl ether by one-step method and catalyst

A diaryl carbonate and synthesis method technology, applied in the direction of organic carbonate preparation, organic chemistry, etc., can solve the problems of incomplete DMC reaction, shortening the reaction process, etc., to shorten production time, reduce production cost, and improve conversion The effect of rate sum

Inactive Publication Date: 2010-03-24
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of a pressurized reactor makes the reaction process more demanding on the reactor, and does not shorten the reaction process flow. In addition, this process cannot completely react DMC, so another rectification tower is still needed to separate DMC in the subsequent process. and methanol

Method used

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  • Method for synthesizing diaryl carbonic acid ester and dimethyl ether by one-step method and catalyst
  • Method for synthesizing diaryl carbonic acid ester and dimethyl ether by one-step method and catalyst

Examples

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example 1

[0024] Example 1. Add the catalyst V of the good transesterification reaction of physical mixing in the reactor 2 o 5 And dehydration catalyst HZSM-5 1.4g, its ratio is: V 2 o 5 :HZSM-5=2:1 (mass ratio), then add 94.0g of phenol and 45.0g of DMC respectively. Stirring was started, and the temperature was gradually increased to 190°C. After 5.0 hours of reaction, 10.2 g of DME was obtained, and the yield of DME was 90.5%. The mixture in the reactor was filtered while it was hot, and the catalyst was recovered. The filtrate was distilled under reduced pressure at 4 mmHg and 150° C., and unreacted phenol was recovered when the fraction temperature was around 60° C. The conversion rate of phenol reached 49.0%. The crude product of DPC was obtained at a distillate temperature of about 130°C. The crude product was dissolved in hot absolute ethanol, then cooled to 10°C for crystallization, and filtered to obtain 49.2g of pure DPC, with a DPC yield of 46.0%.

example 2

[0025] Example 2. Add the catalyst V of the good transesterification reaction of physical mixing in the reactor 2 o 5 And dehydration catalyst HZSM-5 1.0g, the ratio is: V 2 o 5 : HZSM-5=2:1 (mass ratio), then add p-nitrophenol 70.0g, DMC 22.5g respectively. Stirring was started, and the temperature was gradually increased to 190°C. After 5.0 hours of reaction, 4.7 g of DME was obtained, and the yield of DME was 90.4%. Filter the mixture in the reaction kettle while it is hot to recover the catalyst. The filtrate is subjected to vacuum distillation at 3mmHg and 160°C. When the distillate temperature is around 80°C, the unreacted p-nitrophenol is recovered, and the conversion of p-nitrophenol The rate reached 44.8%. The distillate temperature is about 140°C to obtain the crude product of di-p-nitrocarbonate. Dissolve the crude product in hot absolute ethanol, then cool the temperature to 10°C for crystallization, and filter to obtain 30.0g of pure p-nitrocarbonate , The yi...

example 3

[0026] Example 3. Add the catalyst V of the good transesterification reaction of physical mixing in the reactor 2 o 5 And dehydration catalyst HZSM-5 0.9g, its ratio is: V 2 o 5: HZSM-5=2:1 (mass ratio), then add p-ethylphenol 61.0g, DMC 22.5g respectively. Stirring was started, and the temperature was gradually increased to 190° C. After 6.0 hours of reaction, 4.8 g of DME was obtained, and the yield of DME was 92%. Filter the mixture in the reaction kettle while it is hot to recover the catalyst. The filtrate is distilled under reduced pressure at 3mmHg and 160°C. When the distillate temperature is around 80°C, the unreacted p-ethylphenol is recovered, and the conversion of p-ethylphenol The rate reached 45.4%. The distillate temperature is about 135°C to obtain the crude product of di-p-ethyl carbonate. Dissolve the crude product in hot absolute ethanol, then cool the temperature to 10°C for crystallization, and filter to obtain 27.6g of pure p-nitrocarbonate , The yie...

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Abstract

Provided is a synthesis method and a catalyst for catalyzing, coupling and synthesizing diaryl carbonate and dimethyl ether by a single step. A coupling catalyst is compounded by an ester changing catalyst and a dehydration catalyst, the reaction of diaryl carbonate and the reaction of dimethyl ether are simultaneously performed in a same reaction device and under same reaction conditions. The method of the invention avoides the separation process of dimethyl-carbonate and methanol azeotrope, saves the expense for separation of dimethyl-carbonate and methanol azeotrope, reduces production cost, shortens the production time and reduces energy consumption.

Description

technical field [0001] The invention relates to a synthesis method and a catalyst for synthesizing diaryl carbonate and dimethyl ether by one-step catalytic coupling, specifically refers to the phase of transesterification reaction and dehydration reaction using phenol, substituted phenol or aromatic alcohols and dimethyl carbonate as raw materials Synthetic method and used catalyst for synthesizing diaryl carbonate and dimethyl ether by coupled one-step method. technical background [0002] Diaryl carbonates, especially diphenyl carbonate (DPC), have received extensive attention because of their broad application prospects. At present, the domestic demand for DPC is almost entirely dependent on imports, so it is of great theoretical and practical significance to carry out research on more effective synthetic DPC processes and catalysts. [0003] The methods for synthesizing diaryl carbonates include phosgene method, transesterification method and oxidative carbonylation me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/06
Inventor 白荣献李光兴王庶梅付名
Owner HUAZHONG UNIV OF SCI & TECH
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