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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

Active Publication Date: 2016-06-29
JIANGSU AOLUNDA HIGH TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] This kind of ammonolysis reaction is generally carried out in a high-pressure reactor. The kettle-type ammonolysis process is relatively mature, but there are defects: first, intermittent reaction, long operation time and small output; second, the reaction time of kettle-type ammonolysis Long, high temperature and high pressure, the by-product ammonium chloride is extremely corrosive to the equipment, and there are potential safety hazards; third, the investment is large, and the autoclave is made of special steel, which is difficult to manufacture

Method used

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  • A method for preparing 4,4'-diaminodiphenylsulfone

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Experimental program
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Effect test

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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Abstract

The invention discloses a method for preparing 4,4'-diaminodiphenyl sulfone. The method comprises the following steps: 1) 4,4'-Dichlorodiphenyl sulfone, an aminating agent and a cuprous chloride catalyst are fed into a pipeline reactor in a mixed manner or a separate manner, continuous ammonolysis reaction is carried out under a reaction pressure of 9.5-14 MPa and at a temperature of 220-250 DEG C, and the retention time ranges from 20 minutes to 35 minutes; 2) continuous discharge is performed at a reduced pressure, excessive ammonium hydroxide is recycled, and materials are separated and dehydrated to obtain a crude 4,4'-diaminodiphenyl sulfone product; 3) the crude 4,4'-diaminodiphenyl sulfone product is dissolved in hydrochloric acid, the solution is decolorized, filtered and cooled to below 10 DEG C, the pH value is adjusted between 2 and 2.5, and the solution is filtered centrifugally, neutralized through washing, and dried to obtain a pure 4,4'-diaminodiphenyl sulfone product. According to the method, the reaction can be continuous, the reaction time is short, the productivity is improved, energy consumption is greatly reduced, reaction yield and product purity are high, the manufacturing of equipment is simple and the investment is reduced.

Description

Technical field: [0001] The invention relates to a method for preparing 4,4'-diaminodiphenylsulfone, in particular to a pipelined preparation method of 4,4'-diaminodiphenylsulfone. technical background: [0002] 4,4'-Diaminodiphenylsulfone, also known as dapsone, is a widely used chemical substance, which can be used as a curing agent in epoxy resin curing, and can also be used to treat human or animal bacterial infections Therapeutic agent for , has been approved as an antibiotic by the Food and Drug Administration since 1963. With regard to its use in human medicine, 4,4'-diaminodiphenylsulfone is in fact an effective antibiotic used initially in the treatment of leprosy and later also as an inhibitor of dermatitis herpetiformis. Dapsone has recently been used as an effective antibiotic for the prophylaxis of Pneumocystis carinii pneumonia (PCP), an opportunistic disease in HIV infection usually diagnosed when the disease is severe and often occurs in, and appears to be, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 陈律吴红民毛锋吴俊钮强
Owner JIANGSU AOLUNDA HIGH TECH IND