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Process for the catalytic synthesis of bisphenol fluorene by using concentrated sulphuric acid

A technology of concentrated sulfuric acid and bisphenol fluorene, which is applied in the field of concentrated sulfuric acid to catalyze the synthesis of bisphenols, can solve the problems of short service life of equipment, cumbersome production operations, and high catalyst cost, and achieve the effects of less environmental pollution, low cost, and low reaction temperature

Inactive Publication Date: 2010-06-16
WUHAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the method of using concentrated sulfuric acid to catalyze the synthesis of bisphenol fluorene, using solid heteropolyacid, magnetic solid superacid and strong acid ion exchange resin to catalyze the synthesis of bisphenol fluorene has less environmental pollution, the catalyst can be recycled, and the obtained product has high purity; But the reaction time is long, the temperature is high, and the catalyst cost is high
The hydrogen chloride method (US5149886) uses hydrogen chloride gas as a catalyst to catalyze the synthesis of bisphenol fluorene, and the yield is 80% to 85%. However, due to the strong corrosion effect of hydrogen chloride gas, the service life of the equipment is short and the production operation is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Install a thermometer and a mechanical stirrer in a 250ml three-necked bottle; then add 30g of fluorenone and 125g of phenol, heat and stir to dissolve the fluorenone; then add 0.2ml of β-mercaptopropionic acid; control the temperature at about 40°C, Slowly add 4 milliliters of concentrated sulfuric acid (dropped in 1 to 2 hours), then control the temperature at 50 ° C, continue to stir for about 3 hours, and stop the reaction; add 100 milliliters of toluene and 10 milliliters of water to the solution after the reaction, at the temperature Under the condition of 45 ℃~55 ℃, stir for 5~10 minutes, stand for stratification, remove the lower layer of sulfuric acid aqueous solution, add 15 ml of 10% aqueous solution of sodium carbonate to the obtained organic phase, stir at 50 ℃ for 5 minutes, Standing for stratification, the organic layer after removing the lower aqueous solution was washed twice with demineralized water, 15 ml each time, and then the aqueous layer solution ...

Embodiment 2

[0042] Install a thermometer and a mechanical stirrer in a 500ml three-necked bottle, then add 60g of fluorenone and 250g of phenol, heat and stir to dissolve the fluorenone; then add 0.25ml of β-mercaptopropionic acid; control the temperature at about 50°C, 8.5 ml of concentrated sulfuric acid was slowly added dropwise (completed in 1 to 2 hours), then the temperature was controlled at about 50°C, and the stirring was continued for about 4 hours to stop the reaction. To the reacted solution, add 250 ml of toluene and 20 ml of water, stir at 50°C for 5 minutes, stand for stratification, remove the lower aqueous sulfuric acid solution, add 20 ml of a 10% ammonium carbonate aqueous solution to the obtained organic phase, Stir at 50°C for 5 minutes, let stand for stratification, and then wash the organic phase from which the lower aqueous solution was removed with demineralized water twice, 25 ml each time, and then remove the lower aqueous solution to obtain the organic phase. U...

Embodiment 3

[0044] Install a thermometer and mechanical stirring in a 3-liter three-necked flask, then add 360 grams of fluorenone and 1100 grams of phenol, heat and stir to dissolve the fluorenone; 50 ml of concentrated sulfuric acid was added dropwise (dropped in 1 to 2 hours). Then, the temperature was controlled at about 50° C., and the stirring was continued for about 3 hours to stop the reaction. To the reacted solution, add 1200 ml of toluene and 100 ml of water, stir at 50°C for 7 minutes, stand for stratification, remove the lower sulfuric acid solution, add 120 ml of a 10% ammonium carbonate aqueous solution to the obtained organic phase, Stir at 50° C. for 5 minutes, let stand for stratification, remove the lower aqueous solution, and wash the obtained organic phase with demineralized water twice with 100 ml each time. Then, the organic phase obtained above is steamed out toluene under reduced pressure under the conditions that the temperature is not higher than 90°C and the p...

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Abstract

The invention relates to a process for the catalytic synthesis of bisphenol fluorene by using concentrated sulphuric acid. Concentrated sulphuric acid is taken as catalyst, beta-mercapto propionic acid is taken as cocatalyst, phenol is taken as reactant and solvent, reaction with fluorenone is fully carried out under mild condition, one organic polar solvent and water are added, so as to cause unreacted phenol and product are layered with concentrated sulphuric acid; water phase is removed, the obtained organic phase is washed by alkaline solution and softened water step by step, condition is controlled and reduced pressure distillation is carried out to obtain the organic polar solvent and phenol respectively, temperature reduction is carried out, then recrystallization solvent is added for recrystallization, thus obtaining bisphenol fluorine white solid the purity of which is more than 99.0%. The process has low reaction temperature, short time, high productivity more than 90% and high purity more than 99.0%; besides, the used catalyst concentrated sulphuric acid and cocatalyst beta-mercapto propionic acid are low in cost, concentrated sulphuric acid consumption is low, phenol is easy to recycled, recovery rate reaches 80%, and environmental pollution is less, thus the method is applicable to industrialized production.

Description

technical field [0001] The invention relates to the field of preparation of bisphenol fluorene, in particular to a method for catalyzing and synthesizing bisphenol fluorene with concentrated sulfuric acid. technical background [0002] Bisphenol fluorene, scientific name 9,9-bis(4-hydroxyphenyl)fluorene, molecular formula is C 25 H 18 O 2 , molecular weight is 350.4, melting point is 222 ℃ ~ 224 ℃, white powdery substance, soluble in organic solvents such as monocyclic and bicyclic aromatic hydrocarbons, acetonitrile, toluene, methanol, isopropanol and dichloromethane. [0003] In the modern polymer processing industry, bisphenol fluorene compounds and their substituted derivatives are used as important monomers in condensation reactions, especially for the preparation of high heat resistance, good optical properties, good resistance Polycondensation products such as epoxy resin, polyurethane, polycarbonate, polyester, polyaromatic resin, polyether or polyether with flamm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/17C07C37/20
Inventor 张智勇李穿江未本美张开诚姜琦邱孟杰
Owner WUHAN POLYTECHNIC UNIVERSITY
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