Preparation method for 4,4'-dichlorodiphenyl sulfone

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, which is applied in the field of preparation of 4,4'-dichlorodiphenyl sulfone, which can solve the problem of unsatisfactory oxidation strength and oxidation effect of oxidants, increase solvent recovery, etc. question

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, which is applied in the field of preparation of 4,4'-dichlorodiphenyl sulfone, which can solve the problem of unsatisfactory oxidation strength and oxidation effect of oxidants, increase solvent recovery, etc. question

CN107540581AInactive Publication Date: 2018-01-05CHENGDU HUIEN FINE CHEM
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  • Preparation method for 4,4'-dichlorodiphenyl sulfone
  • Preparation method for 4,4'-dichlorodiphenyl sulfone
  • Preparation method for 4,4'-dichlorodiphenyl sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] At 25°C, add 5.3g of glacial acetic acid, 5g of hydrogen peroxide (mass fraction 30%), and 0.5g of concentrated sulfuric acid into a 250mL four-neck flask equipped with a stirrer, thermometer and condenser, and stir the reaction at ≤25°C After 12 hours, it is used as an oxidizing agent and transferred to a balance feeder for use. At 80°C, add 10g of 4,4'-dichlorodiphenyl sulfoxide and 17g of glacial acetic acid to a 250mL four-neck flask equipped with a balance feeder, agitator, thermometer and condenser, and then gradually Add the above-mentioned oxidant dropwise (the dropwise addition is completed within 0.5h), and then continue to react for 1h. After the reaction is completed, cool down to below 5°C, filter, wash, and dry to obtain 10.37g of crude product of 4,4'-dichlorodiphenylsulfone. The weight is 3.7%, the crude product yield is 97.95%, and the melting range is 146-148°C. White crystals are obtained by ethanol recrystallization. ).

[0020] Structural characte...

Embodiment 2

[0028] At 25°C, add 24g of glacial acetic acid to a 250mL four-necked flask equipped with a balance feeder, stirrer, thermometer and condenser, and drop 2.5g (0.022mol) of hydrogen peroxide at ≤25°C in 0.25g of concentrated sulfuric acid to catalyze After generating peracetic acid under the action, add 5g (0.018 mol) raw material 4,4'-dichlorodiphenyl sulfoxide at 60°C, cool down to below 5°C after the reaction, filter, wash and dry to obtain 4,4' - The crude product of dichlorodiphenyl sulfone was 5.09g, the weight gain was 1.8%, the yield of the crude product was 96.40%, and the melting range was 146.5~148.5°C.

Embodiment 3

[0030] At 25°C, add 30g of glacial acetic acid to a 250mL four-necked flask equipped with a balance feeder, stirrer, thermometer and condenser, and add 2.5g of hydrogen peroxide dropwise at ≤25°C. Catalyze with (0.25g) concentrated sulfuric acid After generating peracetic acid at low temperature, add 5g of raw material 4,4'-dichlorodiphenyl sulfoxide at 40°C, cool down to below 5°C after the reaction, filter, wash, and dry to obtain 4,4'-dichlorodiphenyl The crude product of sulfone is 5.06g, the weight gain is 1.2%, the yield of the crude product is 95.83%, and the melting range is 146.5~148°C.

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Abstract

The invention provides a preparation method for 4,4'-dichlorodiphenyl sulfone. According to the invention, 4,4'-dichlorodiphenyl sulfoxide is used as a raw material; formic acid or glacial acetic acidis used as a reaction medium; and an acid peroxide oxidizing agent corresponding to the composition of the reaction medium is used for an oxidation reaction so as to prepare 4,4'-dichlorodiphenyl sulfone. The preparation method has better effect than traditional methods using hydrogen peroxide as an oxidizing agent, and is simple and easily practicable.

Description

technical field [0001] The invention relates to an improved preparation method of 4,4'-dichlorodiphenyl sulfone. Background technique [0002] 4,4'-dichlorodiphenyl sulfone is an important organic synthesis intermediate, which can be widely used in the fields of medicine, dyes and pesticides, and can be used as a monomer for the modification of polyphenylene sulfide, a polymer material. [0003] There are many synthetic methods of 4,4'-dichlorodiphenyl sulfone, such as phosphorus oxychloride method, sulfuric acid method, pyrosulfate method, chlorosulfonic acid method, sulfur trioxide method, etc., but these methods have their own advantages and disadvantages. Obvious deficiency. For this reason, the CN 102351756A Chinese patent literature proposes the process of using chlorobenzene, thionyl chloride, and hydrogen peroxide as raw materials to synthesize 4,4'-dichlorodiphenyl sulfone: using AlCl 3 As a catalyst, chlorobenzene and thionyl chloride are used as raw materials fo...

Claims

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Application Information

Patent Timeline
05 Jan 2018
Publication
CN107540581A
IPC
C07C315/00; C07C317/14
Inventors
李晶晶; 李露娅