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Method for preparing 2,6-diphenyl phenol through step recrystallization in coarse dehydrogenation products

A technology of diphenylphenol and crude product, which is applied in the field of fractional recrystallization and preparation, can solve the problems of large amount of solvent, small amount of solvent and high production efficiency, and achieves the advantages of saving purification cost, simplifying operation steps and improving production efficiency. Effect

Active Publication Date: 2014-05-28
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the disadvantages of low recovery rate and large amount of solvent used for recrystallization using a single solvent, and difficult solvent recovery for recrystallization using a mixed solvent, the purpose of the present invention is to provide a method for preparing 2,6 by stepwise recrystallization from the crude dehydrogenation product -The method of diphenylphenol, described method can obtain high yield, high-purity 2,6-diphenylphenol, and solvent consumption is little, recovery rate is high, and production efficiency is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Connect a condenser tube to a 250ml three-neck flask, add 98.2g cyclohexanone and 40ml toluene, heat to 150°C, add 0.28g potassium hydroxide as a catalyst, and reflux at 150°C for 2.5 hours, after the reaction stops The reaction product was neutralized with 10% hydrochloric acid solution, the water layer was separated, dried, vacuum distilled, and fractions at different temperatures were collected to obtain a product with a mass fraction of 12.6% cyclohexanone, 35.6% dimer ketone, 50.6% trimer ketone, 1.2% high boilers.

[0023] (2) A tubular fixed-bed reactor with an aspect ratio of 10:1 is placed in a heating furnace, and the tubular fixed-bed reactor is filled with 5% Pd / Al 2 o 3 Catalyst, the reaction temperature is controlled at 290 ° C, protected by nitrogen, and after the temperature is stable, the trimerketone prepared in step (1) is input from the lower port of the tubular fixed bed reactor with a pump, and the liquid hourly space velocity is 2.9h -1 , re...

Embodiment 2

[0025] Get 100.0 g of the crude dehydrogenation product obtained in Example 1 and add it to isopropanol, wherein the mass ratio of the crude dehydrogenation product to isopropanol is 0.5:1, and heat to 40° C. to completely dissolve the crude dehydrogenation product. The temperature was lowered, and the solution was allowed to stand at 20° C. for 5 h, and filtered to obtain crystals. Add the crystals into ethanol, wherein the mass ratio of crystals to ethanol is 0.5:1, heat to 50°C and the crystals are completely dissolved, cool down, let the solution stand at 20°C for 5 hours, filter and vacuum dry to obtain white needles The crystal is 2,6-diphenylphenol. Adopt external standard method, HPLC carries out analysis, and analysis condition is: column temperature 30 ℃, mobile phase is the methanol aqueous solution of 80%, mobile phase flow rate is 0.5ml / min, records recrystallization recovery rate to be 77.08%, crystal purity is 92 %.

Embodiment 3

[0027] Get 100.0 g of the crude dehydrogenation product obtained in Example 1 and add it to isopropanol, wherein the mass ratio of the crude dehydrogenation product to isopropanol is 2:1, and heat to 50° C. to completely dissolve the crude dehydrogenation product. The temperature was lowered, and the solution was allowed to stand at 20° C. for 5 h, and filtered to obtain crystals. Add the crystals into ethanol, wherein the mass ratio of crystals to ethanol is 2:1, heat to 60°C and the crystals are completely dissolved, cool down, and let the solution stand at 20°C for 5 hours, filter and vacuum dry to obtain white needles The crystal is 2,6-diphenylphenol. Adopt external standard method, analyze with HPLC, analysis condition is: 30 ℃ of column temperature, mobile phase is the methanol aqueous solution of 80%, and mobile phase flow velocity is 0.5ml / min, records recrystallization recovery rate 63.9%, crystal purity is 99%.

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Abstract

The invention discloses a method for preparing 2,6-diphenyl phenol through step recrystallization in coarse dehydrogenation products and belongs to the field of chemical engineering materials. The method comprises the following steps that: (1) coarse dehydrogenation products are added into isopropanol, the materials are heated until the complete dissolution is realized, the temperature is lowered, the solution is subjected to still standing for 10 to 15 hours at 20 DEG C, and crystals are obtained through filtering; (2) the crystals obtained in the step (1) are added into ethanol and are heated to realize the complete dissolution, the temperature is lowered, the solution is subjected to still standing for 10 to 15 hours at 20 DEG C, filtering and vacuum drying are carried out, crystals are obtained, namely 2,6-diphenyl phenol is obtained. The method has the advantages that high-yield and high-purity 2,6-diphenyl phenol can be obtained, in addition, the solvent consumption is low, the recovery rate is high, and the production efficiency is high.

Description

technical field [0001] The invention relates to a method for preparing 2,6-diphenylphenol by fractional recrystallization from crude dehydrogenation products, belonging to the field of chemical materials. Background technique [0002] 2,6-Diphenylphenol is an important chemical raw material, which is widely used in many fields, such as adsorption materials, engineering plastics, insulating materials, antioxidants, etc. 2,6-Diphenylphenol's good rigidity and special hydrogen bonding make it more and more widely used in the fields of medicine and functional materials. Poly 2,6-diphenyl-p-phenylene ether synthesized from 2,6-diphenylphenol, because of its good moisture resistance, not easy to oxidize, high temperature resistance, not easy to lose, low background value, easy to heat desorption and With the advantages of high desorption efficiency, it has been widely used in gas detection and environmental protection. [0003] Chinese patent application 201010523427.1 "A Prepar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/84
CPCY02P20/52
Inventor 陈欢张洪彬许东海
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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