Preparation method of 1,1'-sulfonyl bis(4-(2-propylene)oxy benzene)

A technology of oxybenzene and propylene, applied in the field of preparation of 1,1'-sulfone bis[4-(2-propene)oxybenzene], which can solve the problems of increasing production cost, affecting production efficiency, high reaction temperature, etc. , to achieve the effects of increasing the cost, improving the safety of the reaction, and reducing the reaction temperature

Active Publication Date: 2013-05-01
LIANYUNGANG NIUTAIKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the boiling point of chloropropene is only 44.6°C, when the reaction temperature is 70-90°C, a large-capacity condenser must be used to prevent the chloropropene from vaporizing and escaping. At the same time, the high reaction temperature also increases energy consumption; The use of organic alcohol solvents to dissolve the raw material 4,4'-dihydroxydiphenyl sulfone also requires solvent recovery, which increases production costs; moreover, the reaction time for this preparation is relatively long, reaching 5 to 8 hours, which affects production efficiency

Method used

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Examples

Experimental program
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Embodiment

[0017] Embodiment: According to the ratio and reaction conditions of the embodiment, in a four-necked flask equipped with stirring, reflux condenser, thermometer and dripping device, add 4,4'-dihydroxydiphenyl sulfone, alkali, phase transfer catalyst , water, potassium iodide, stirring to completely dissolve 4,4'-dihydroxydiphenyl sulfone, warming up to the reaction temperature, adding allyl chloride dropwise with a dropping funnel, and keeping warm until the detection of 4,4'-dihydroxydiphenyl sulfone is basically no exist, after the reaction is finished, cool down to room temperature and discharge, filter with suction, wash the filter cake with water until neutral, and dry to obtain 1,1'-sulfone-bis[4-(2-propene)oxybenzene] product. The content (purity) was analyzed by liquid chromatography, and the yield was calculated as 4,4'-dihydroxydiphenyl sulfone.

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PUM

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Abstract

The invention relates to improvement of a preparation method for synthesizing 1,1'-sulfonyl bis(4-(2-propylene)oxy benzene) by taking 4,4'-dihydroxydiphenylsulfone and chloropropene as raw materials. The invention is characterized in that a reaction is carried out in an alkali aqueous solution, a phase transfer catalyst and a potassium iodide catalyst are added in the reaction, the mol ratio of reaction raw materials is that the ratio of 4,4'-dihydroxydiphenylsulfone: chloropropene: alkali is equal to 1: (2.0-2.4): (2.0-4.0), the weight ratio of the phase transfer catalyst to 4,4'-dihydroxydiphenysulfone is (0.003-0.03): 1, the mol ratio of potassium iodide to chloroproene is (0.006-0.03)-1. The invention has the advantages that: the reaction temperature is low, required to be 30-65 DEG Conly; the reaction time is reduced, required to be 3-4.5 hours only; the yield is higher than 93%; the product purity is higher than 99%; the reaction requires no condenser for condensation to prevent chloropropene from escaping by gasification; the reaction safety is high; and the equipment investment is low.

Description

technical field [0001] The present invention is an improvement to the preparation method for synthesizing 1,1'-sulfone-based bis[4-(2-propene)oxybenzene] with 4,4'-dihydroxydiphenyl sulfone and allyl chloride as raw materials, and particularly relates to a The preparation method has low reaction temperature, short reaction time and high product purity and yield. Background technique [0002] 1,1'-sulfone-based bis[4-(2-propenyl)oxybenzene] has many uses, such as the color developer of thermosensitive recording materials, the raw material of polymer flame retardants and the polymer heat-resistant materials raw material. [0003] U.S. Patent No. 4,596,997 discloses that 4,4'-dihydroxydiphenyl sulfone reacts with allyl halides in a solvent to prepare 1,1'-sulfone-based bis[4-(2-propene)oxybenzene], which can also be Speed ​​up the reaction by adding a phase transfer catalyst. The disadvantage of this method is that the used solvent may contain organic solvents, which will le...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/22C07C315/04
Inventor 陈律毛锋尹益
Owner LIANYUNGANG NIUTAIKE CHEM
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