Dehydration control method for synthesis of bisphenol S

A control method and technology of synthesis reaction, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of poor control of dehydration process, low yield of bisphenol S, poor product quality, etc. Decolorization, purification and purification, the effect of improving purity

Active Publication Date: 2015-04-29
KEMAI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In order to solve the problems of poor control of the dehydration process, low yield of bisphenol S and poor product quality when bisphenol S is obtained through sulfonation reaction of phenol and concentrated sulfuric acid, a controlled dehydration method is proposed. process method

Method used

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  • Dehydration control method for synthesis of bisphenol S

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add naphthalene disulfonic acid catalyst 20g, mesitylene 600g, phenol 493g in the four-necked reaction flask that reflux water divider is housed, stir and be warming up to 80 ℃, dropwise concentration 96% vitriol oil 256g (2.5 mole), and in The dropwise addition was completed in 2 hours. Then the temperature is raised rapidly to the reflux of mesitylene, and at the same time, the azeotropic dehydration is carried out by mesitylene. Theoretically, the total amount of water that needs to be removed is the sum of the water brought in by the concentrated sulfuric acid and the water generated by the reaction. Theoretically, the reaction to generate bisphenol S should produce 90mL of water, and the concentrated sulfuric acid will bring 10.2mL of water, the total is 100.2mL.

[0026] During the first 3 hours of the dehydration process, 75% of the total water, ie 75.2 mL, was removed. In the remaining 6 hours of the dehydration process, continue to remove 25% of the remaining...

Embodiment 2

[0029] Add naphthalene disulfonic acid catalyst 20g, mesitylene 600g, phenol 493g in the four-necked reaction flask that reflux water divider is housed, stir and be warming up to 80 ℃, dropwise concentration 96% vitriol oil 256g (2.5 moles), and in The dropwise addition was completed in about 2 hours. Then the temperature is raised rapidly to the reflux of mesitylene, and at the same time, the azeotropic dehydration is carried out by mesitylene. Theoretically, the total amount of water that needs to be removed is the sum of the water brought in by the concentrated sulfuric acid and the water generated by the reaction. Theoretically, the reaction to generate bisphenol S should produce 90mL of water, and the concentrated sulfuric acid will bring 10.2mL of water, the total is 100.2mL.

[0030] During the first 3 hours of the dehydration process, 85% of the total water volume, ie 85.2 mL, was removed. In the remaining 6 hours of the dehydration process, continue to remove 15% of...

Embodiment 3

[0033]Add naphthalene disulfonic acid catalyst 20g, mesitylene 600g, phenol 493g in the four-necked reaction flask that reflux water divider is housed, stir and be warming up to 80 ℃, dropwise concentration 96% vitriol oil 256g (2.5 mole), and in The dropwise addition was completed in 2 hours. Then the temperature is raised rapidly to the reflux of mesitylene, and at the same time, the azeotropic dehydration is carried out by mesitylene. Theoretically, the total amount of water that needs to be removed is the sum of the water brought in by the concentrated sulfuric acid and the water generated by the reaction. Theoretically, the reaction to generate bisphenol S should produce 90mL of water, and the concentrated sulfuric acid will bring 10.2mL of water, the total is 100.2mL.

[0034] During the first 3 hours of the dehydration process, 80% of the total water volume, ie 80.2 mL, was removed. In the remaining 6 hours of the dehydration process, continue to remove 20% of the rem...

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Abstract

The invention discloses a dehydration control method for synthesis of bisphenol S, which is implemented by calculating a theoretical amount of dehydrated water according to a synthetic reaction equation of the bisphenol S and the feeding molar ratio of phenols and sulfuric acid; and controlling the early stage of the reaction to be in a rapid dehydration state and the late stage of the reaction to be in a slow dehydration state, wherein preferably, in one third of the dehydration process, 75-85% of water is dehydrated, and in the rest two thirds of the dehydration process, 25-15% of water is further dehydrated. The purity of the bisphenol S after being refined is 99.5% or over, and the chromaticity is less than 20 (platinum-cobalt colorimetric method). By controlling the dehydration speed in the process of bisphenol S synthesis, the excessive oxidation of phenols and phenolsulfonic acid can be avoided, and the purity of bisphenol S in a crude product can be improved. A synthetic bisphenol S crude-product is shallow in appearance color and low in chromaticity; and the purity of the bisphenol S crude-product is relatively high, so that the bisphenol S crude-product is easily further decolored, refined and purified.

Description

technical field [0001] The technology of the invention belongs to the field of organic intermediate preparation, and relates to a dehydration control method for synthesizing bisphenol S; in particular, it proposes a method for controlling dehydration when sulfuric acid and phenol are used to synthesize bisphenol S. Background technique [0002] Bisphenol S, namely 4,4'-dihydroxydiphenyl sulfone, has excellent heat resistance, light resistance and oxidation resistance. Polymer polyethersulfone, polysulfone ether ketone, etc. can be synthesized from bisphenol S as a monomer. Bisphenol S can also undergo bromination or allylation reactions, such as the preparation of tetrabromobisphenol S, or octabromo-S ether, which is an excellent flame retardant. Bisphenol S is also mainly used as an intermediate of developer for thermal pressure-sensitive recording paper. [0003] The methods for preparing bisphenol S mainly include the following. [0004] Hydrolysis. 4,4'-dichlorodiphe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/22C07C315/00
Inventor 张天永李彬陈松张国玲王树华
Owner KEMAI CHEM
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