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A kind of preparation method of diphenyl ether

A technology of diphenyl ether and phenol, which is applied in the field of preparation of diphenyl ether, can solve problems such as complex procedures and long reaction time, and achieve the effect of filling the gap in China, low cost and few reaction steps

Active Publication Date: 2021-09-07
SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN102146024A discloses a preparation method of diphenyl ether, which generates a salt solution of phenol through phenol and alkali, then refluxes chlorinated benzene to remove water in the system, and then in the presence of a catalyst, drips chlorinated benzene to perform U11mann reaction to generate the target compound; in this method, phenol is the raw material and also the solvent. The catalyst is copper sulfate pentahydrate or copper chloride wet material or a mixture of the two. The whole process needs at least 12.5 hours, and the reaction time is long and the process complex defect

Method used

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  • A kind of preparation method of diphenyl ether
  • A kind of preparation method of diphenyl ether
  • A kind of preparation method of diphenyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019]

[0020] Open the nitrogen purging pipeline and the fixed-bed reactor to replace the air therein. The raw material phenol is preheated to 100° C., and then pumped into the fixed-bed reactor. Magnesium oxide (68% by mass) is housed in the fixed-bed reactor. %) / 4A zeolite (mass percentage 32%) catalyst, heat the fixed bed reactor to 400°C, the pressure inside the reactor is 0.1MPa, adjust the nitrogen flow rate so that the residence time of the material in the fixed bed reactor is 15 seconds, The diphenyl ether, water and unreacted raw material phenol produced by the reaction leave the fixed-bed reactor in a gaseous state, enter the multi-stage condenser to cool into liquid, and then enter the rectification tank for rectification separation, and the collected water is used as circulating water supplement , Phenol re-enters the reaction system for recycling, the finished product enters the finished product tank, and the finished product is analyzed by gas chromatography ...

Embodiment 2

[0022]

[0023] Open the nitrogen purging pipeline and the fixed-bed reactor to replace the air therein. The raw material phenol is preheated to 120° C., and then pumped into the fixed-bed reactor. Magnesium oxide (60% by mass) is housed in the fixed-bed reactor. %) / 4A zeolite (40% by mass) catalyst, the fixed bed reactor was heated to 500°C, the pressure inside the reactor was 0.2MPa, and the nitrogen flow rate was adjusted so that the residence time of the material in the fixed bed reactor was 5 seconds. The diphenyl ether, water and unreacted raw material phenol produced by the reaction leave the fixed-bed reactor in a gaseous state, enter the multi-stage condenser to cool into liquid, and then enter the rectification tank for rectification separation, and the collected water is used as circulating water supplement , Phenol re-enters the reaction system for recycling, the finished product enters the finished product tank, and the finished product is analyzed by gas chroma...

Embodiment 3

[0025]

[0026] Open the nitrogen purging pipeline and the fixed-bed reactor to replace the air therein. The raw material phenol is preheated to 80° C., and then pumped into the fixed-bed reactor. Magnesium oxide (77% by mass) is housed in the fixed-bed reactor. %) / 4A zeolite (mass percentage 23%) catalyst, heat the fixed bed reactor to 300 °C, the pressure inside the reactor is 0.05MPa, adjust the nitrogen flow rate so that the residence time of the material in the fixed bed reactor is 30 seconds, The diphenyl ether, water and unreacted raw material phenol produced by the reaction leave the fixed-bed reactor in a gaseous state, enter the multi-stage condenser to cool into liquid, and then enter the rectification tank for rectification separation, and the collected water is used as circulating water supplement , Phenol re-enters the reaction system for recycling, the finished product enters the finished product tank, and the finished product is analyzed by gas chromatography...

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Abstract

The invention relates to a preparation method of diphenyl ether, which adopts a continuous flow fixed-bed reactor, and phenol is contacted with a magnesium oxide / zeolite catalyst packed in the reactor in a nitrogen atmosphere environment and reacted to form diphenyl ether. Phenol is used as a raw material, and diphenyl ether is obtained through high-temperature catalytic reaction in a fixed-bed reactor, followed by rectification and separation. The patent of the invention has the advantages of fewer reaction steps, low cost, and less pollution, and realizes green catalysis for industrial production of diphenyl ether.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of biphenyl ether. Background technique [0002] Diphenyl ether, also known as diphenyl ether, is an important chemical intermediate, which can be used in the production of flame retardants, flavors and fragrances, dyes, etc., and can also be used as a high-temperature heat carrier, with a wide range of uses. The traditional synthesis method of diphenyl ether is formed by condensation of chlorobenzene and phenol in caustic soda solution in the presence of copper oxide catalyst, and the finished product is obtained through alkali washing and distillation. Protection brings great pressure. [0003] CN102146024A discloses a preparation method of diphenyl ether, which generates a salt solution of phenol through phenol and alkali, then refluxes chlorinated benzene to remove water in the system, and then in the presence of a catalyst, drips c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/09C07C43/263
CPCC07C41/09C07C43/263
Inventor 詹石玉刘东东高双庆南彦冬
Owner SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD