A method for preparing 4,4'-diaminodiphenylsulfone
A technology of diaminodiphenyl sulfone and dichlorodiphenyl sulfone, which is applied in 4 fields, can solve the problems of potential safety hazards, long operation time, long reaction time, etc., reduce equipment investment, increase reaction yield, and simplify equipment manufacturing Effect
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Embodiment 1
[0024] The molten 4,4'-dichlorodiphenyl sulfone is injected into the pipeline reactor through a high-pressure pump at a flow rate of 140 grams / hour, while the mass fraction is 25% ammoniacal liquor and cuprous chloride at a rate of 800 grams / hour The flow rate (wherein the flow rate of cuprous chloride is 5.6 g / h) is also jointly injected into the pipeline reactor through a high-pressure pump, and a continuous ammonolysis reaction is carried out at a pressure of 14Mpa and a temperature of 220°C. The residence time of the reaction material in the high-pressure pipeline is 20 Minutes; after the product is decompressed and discharged by a pressure reducing valve, the product is analyzed by liquid chromatography, and the ammonolysis product contains 0.1% of 4,4'-dichlorodiphenyl sulfone, and the discharge is sent to a recovery device to distill out excess ammonia and separate Crude 4,4'-diaminodiphenylsulfone; the crude product is dissolved in hydrochloric acid with a mass fraction...
Embodiment 2
[0026] The molten 4,4'-dichlorodiphenyl sulfone is injected into the pipeline reactor through a high-pressure pump at a flow rate of 140 grams / hour, while the mixture of ammoniacal liquor and cuprous chloride with a mass fraction of 20% is injected at a flow rate of 800 grams / hour Flow rate (wherein the flow rate of cuprous chloride is 4.2 grams / hour) is also squeezed into pipeline reactor jointly through high-pressure pump, carries out continuous ammonolysis reaction under 13Mpa pressure and being 235 ℃ of temperature, and the residence time of reaction material in high-pressure pipeline is 25 minutes; after the product was decompressed and discharged by the pressure reducing valve, the product was analyzed by liquid chromatography, and the ammonolysis product contained 0.08% of 4,4'-dichlorodiphenyl sulfone, and the discharge was sent to a recovery device to distill off excess ammonia and separate Obtain the crude product of 4,4'-diaminodiphenylsulfone; the crude product is d...
Embodiment 3
[0028] The molten 4,4'-dichlorodiphenyl sulfone is injected into the pipeline reactor through a high-pressure pump at a flow rate of 140 grams / hour, while the mixture of ammoniacal liquor and cuprous chloride is 30% by mass fraction at a rate of 750 grams / hour The flow rate (wherein the flow rate of cuprous chloride is 1.4 g / hour) is also injected into the pipeline reactor through a high-pressure pump, and the continuous ammonolysis reaction is carried out at a pressure of 9.5Mpa and a temperature of 250°C. The residence time of the reaction material in the high-pressure pipeline is It was 35 minutes; the product was analyzed by liquid chromatography after being decompressed and discharged by a pressure reducing valve, and the ammonolysis product contained 0.08% of 4,4'-dichlorodiphenyl sulfone, and the discharged material was sent to a recovery device, and excess ammonia was distilled out. The crude product of 4,4'-diaminodiphenylsulfone was isolated; the crude product was dis...
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