Method for catalyzing synthesis of 4,4'-dichlorodiphenylsulfone by solid acid
A technology of dichlorodiphenyl sulfone and solid acid catalysis, applied in the field of phenyl sulfone, can solve the problems of difficult separation and recovery, corrosion of equipment by strong acid, affecting product quality, etc., and achieves the effects of low cost, high utilization rate and high product yield
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[0042] The invention provides a method for synthesizing a solid acid catalyst, which is a method known to those skilled in the art, and specifically includes the following steps:
[0043] The first step, the preparation of monoester compound:
[0044] Weigh 28.01g of 3-hydroxypropanesulfonic acid and 23.20g of fumaric acid, dissolve them in 400.00g of ethyl acetate, stir at 50°C for 6 hours, and remove the ethyl acetate by distillation to obtain a monoester containing olefin, carboxylic acid group and sulfonic acid group compound. The reaction equation is as follows:
[0045] .
[0046] The second step, synthesizing solid acid catalyst:
[0047] Dissolve 23.80g monoester compound in 300.00g ethanol, add 0.15g benzoyl peroxide, heat up to 70°C and stir for 2 hours to form oligomer, add 13.02g divinylbenzene, 56.00g 1-octene, 0.35g Benzoyl peroxide, 20.00g toluene (porogen), 2.00g sodium dodecyl sulfate (dispersant), heat up at 80°C, stir for 5 hours, filter, vacuum dry at...
Embodiment 1
[0050]135.58g (0.5mol) of 4,4´-dichlorodiphenyl sulfoxide, 271.50g of chlorobenzene, and 1.00g of the prepared catalyst were put into the reaction kettle, stirred and heated to 50 °C to make 4,4´-dichlorobenzene. The diphenyl sulfoxide was completely dissolved in the solvent, and 65.00 g of 30% hydrogen peroxide was added dropwise to the mixture containing 4,4´-dichlorodiphenyl sulfoxide; the reaction progress was monitored by TLC thin layer chromatography, and the reaction was completed. Then, filter out the catalyst while hot, immerse the catalyst in an aqueous ethanol solution for washing, and vacuum dry for use; add 0.5 g of activated carbon to the filtrate to remove impurities and decolorize, filter out the activated carbon while hot, and cool the obtained filtrate to 5 ° C for 2 hours of cooling and crystallization , filtered again to obtain a wet product and a water-oil two-phase mixed solution, and the wet product was vacuum-dried at 100 °C for 12 hours to obtain 4,4´-d...
Embodiment 2
[0052] 135.58g (0.5mol) of 4,4´-dichlorodiphenyl sulfoxide, 401.50g of chlorobenzene, and 2.50g of the prepared catalyst were put into the reaction kettle, stirred and heated to 50°C to make 4,4´-dichlorobenzene. The diphenyl sulfoxide was completely dissolved in the solvent, and 78.00 g of 30% hydrogen peroxide was added dropwise to the mixture containing 4,4´-dichlorodiphenyl sulfoxide; the reaction progress was monitored by TLC thin layer chromatography, and the reaction was completed. Then, filter out the catalyst while hot, immerse the catalyst in an aqueous ethanol solution for washing, and vacuum dry for use; add 0.80 g of activated carbon to the filtrate to remove impurities and decolorize, filter out the activated carbon while hot, and cool the obtained filtrate to 5° C. and crystallize by cooling for 2 hours. , filtered again to obtain a wet product and a water-oil two-phase mixed solution, and the wet product was vacuum-dried at 100 °C for 12 hours to obtain 4,4´-dic...
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