Process for producing 4, 4'-bisphenol sulfone

A manufacturing method, phenol sulfone technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult to handle solid block, no post-processing operation advantage, difficulty, etc., to achieve simple reflux operation, Easy to recycle and reuse, and the effect of promoting the removal of water

Inactive Publication Date: 2005-06-01
NIPPON SODA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is a problem that the reaction product obtained after the solvent is distilled off becomes a solid block that is industrially difficult to handle, and it is necessary to control the reaction conditions for adjusting the removal rate of the solvent and the isomerization rate
In addition, in this invention, two types of solvents are used: a suspending agent (for example, Aisopa-(registered trademark of Exxon Chemical Co., Ltd.) H, initial boiling point 176°C) and an entrainer (for example, Aisopa-E, initial boiling point 115°C) It is indispensable, but when using solvents with different physical properties as described above, the problem is that when the solvent is reused, it will be difficult to manage the boiling point, etc., and it will also lead to an increase in production costs.
[0010] Therefore, in above-mentioned prior art, also do not have the method that the aftertreatment operation after reaction is favorable

Method used

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  • Process for producing 4, 4'-bisphenol sulfone
  • Process for producing 4, 4'-bisphenol sulfone
  • Process for producing 4, 4'-bisphenol sulfone

Examples

Experimental program
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Effect test

Embodiment 1

[0101] Put 98.7g (1.05mol) of phenol, 75ml of Aisopa-H, and 50ml of mesitylene into a 500ml four-neck flask equipped with a stirrer, a thermometer, and a water separation tube. 51.6 g (0.50 mol) of 95% sulfuric acid was added dropwise thereto, and then the temperature was raised.

[0102] Distillation of the reaction liquid started from around 148° C., the distillate was condensed in a water separation tube and separated into two layers, and the upper organic layer was continuously returned to the reaction system. The temperature of the reaction system reached 170° C. after about 4 hours from the start of the temperature rise, the generation of water stopped, and the amount of water separated in the water separation tube was 20.5 g. Thereafter, 50 ml of Asopa-H was added, and it took 3 hours for the temperature of the reaction system to reach 175° C. to distill off mesitylene. The composition of the reactant was analyzed by high-performance liquid chromatography (HPLC), and t...

Embodiment 2

[0106] 98.7 g (1.05 moles) of phenol and 100 ml of Aisopa-G were charged into a 500 ml four-necked flask equipped with a stirrer, a thermometer, and a water separation tube, and 95% sulfuric acid 51.6 g was added dropwise to the mixture at 50°C under stirring conditions. g (0.50 mol), the temperature was raised.

[0107] Distillation of the reaction liquid started at around 144°C, and the distillate was condensed and separated into three layers in a water separation tube. The upper layer was a solvent layer, the middle layer was a water layer, and the bottom layer was a phenol layer. The upper solvent layer was continuously returned to the reaction system, and the bottom phenol layer was extracted every 15 minutes and returned to the reaction system. The temperature of the reaction system reached 167° C. in about 7 hours from the start of the temperature rise, the generation of water stopped, and the amount of water separated in the water separation tube was 21.2 g. The total...

Embodiment 3

[0111] Put 117.5 g (1.25 moles) of phenol and 100 ml of Aisopa-G into a 500 ml four-necked flask equipped with a stirrer, a thermometer, a water separation tube, and a Wedman-type rectification column, and add phenol to it at 50 ° C under stirring conditions. After 51.6 g (0.50 mol) of 95% sulfuric acid was added dropwise to the mixture, the temperature was raised.

[0112] Distillation of the reaction liquid started around 144°C, and the distillate was condensed and separated into three layers in the water separation tube, the upper layer being a solvent layer, the middle layer being a water layer, and the bottom layer being a phenol layer. The upper solvent layer was continuously returned to the reaction system, and the bottom phenol layer was reacted without returning to the reaction system. The temperature of the reaction system reached 167° C. in about 10 hours from the start of the temperature rise, and the generation of water stopped. The amount of water separated in th...

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Abstract

A process for producing 4,4'-bisphenol sulfone by reacting phenol with sulfuric acid, which comprises conducting the dehydration reaction in a mixed solvent comprising mesitylene and an aliphatic saturated hydrocarbon having a boiling point of 175 DEG C or higher and finally distilling off the mesitylene from the reaction system, or comprises conducting the reaction in a solvent comprising an aliphatic saturated hydrocarbon in a reaction vessel equipped with a fractionating device. Thus, 4,4'-bisphenol sulfone can be produced in high yield with a higher operating efficiency. Also provided is a process for easily producing 4,4'-bisphenol sulfone having a high purity which comprises conducting the reaction in a solvent containing an aliphatic saturated hydrocarbon, subsequently adding a C1-3 alcohol to the reaction mixture, separating the alcohol layer from the resultant mixture, and recrystallizing the 4,4'-bisphenol sulfone from the alcohol layer.

Description

technical field [0001] The present invention relates to a method for producing 4,4'-bisphenol sulfone (or 4,4'-dihydroxydiphenylsulfone, hereinafter referred to as 4,4'-BPS) by reacting phenol and sulfuric acid. Background technique [0002] 4,4'-BPS is a useful compound generally used as a raw material for engineering plastics such as polysulfone (PSF) and polyethersulfone (PES). In order to produce this 4,4'-BPS, although the method of reacting phenol and sulfuric acid has been frequently studied, the main problems of this technology are how to efficiently remove water and how to reduce the by-product isomer 2,4 '-BPS to increase the yield of 4,4'-BPS in both ways. [0003] A kind of 4, the manufacture method of 4 '-BPS is disclosed in the Japanese Patent Application Publication No. 3-101656, and the feature of this method is, use mesitylene as reaction solvent, make phenol and while removing water under reflux condition The sulfonating agent and the like react to cause ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/00C07C317/22
CPCC07C315/00
Inventor 肥高友也
Owner NIPPON SODA CO LTD
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