ChemicalBook CAS DataBase List Biphenyl-4,4'-dicarboxylic acid

Biphenyl-4,4'-dicarboxylic acid synthesis

13synthesis methods

Product Name:Biphenyl-4,4'-dicarboxylic acid
CAS Number:787-70-2
Molecular formula:C14H10O4
Molecular Weight:242.23

613-33-2 Synthesis

613-33-2
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$9.00/10g

787-70-2
386 suppliers
$8.00/5g

Yield:787-70-2 98.6%

Reaction Conditions:

with oxygen;acetic anhydride for 17 h;Reflux;Large scale;Green chemistry;

Steps:

S1. Ingredients: Put 1500kg of anhydrous glacial acetic acid, 133kg of 4,4'-dimethylbiphenyl, 2kg of cobalt acetate, and 2kg of acetic acid into a 2000L titanium reactor equipped with a titanium condenser, oxygen pipe and thermometer. Manganese, 2kg potassium bromide, 1kg cerium acetate and 6kg acetic anhydride;Preparation of crude S2, 4,4'-biphthalic acid: Then turn on oxygen 5m³/h, heat to reflux for reaction, add 120kg of acetic anhydride after 5h, and sample 4,4'-dimethylbiphenyl after 12h After the reaction is completed, the crude product of 4,4'-diphthalic acid is obtained by cooling, crystallization and filtration, which is 195-205kg after washing on the centrifuge;S3. Treatment of reaction mother liquor: transfer the mother liquor to the decolorization kettle, add 10kg activated carbon, heat to 80, stir and decolorize at 80-90 for 40min, then filter into the reactor, measure the water content, make up the acetic anhydride, and then add them separately 0.2kg of cobalt acetate, 0.2kg of manganese acetate, 0.2kg of potassium bromide and 0.1kg of cerium acetate, put in 133kg of 4,4'-dimethylbiphenyl, pass oxygen and react with the normal batch operation, and then apply the mother liquor according to this method;Pretreatment of S4,4,4'-diphthalic acid purification: respectively add 2000L water, 300kg liquid caustic soda and the crude product of step S3 into the 3000L glass-lined reactor, and then heat to 70-80 to dissolve the material and adjust the pH 7, then add 5kg of activated carbon, stir and decolorize for 30min, and then hot filter;Refining of S5, 4,4'-diphthalic acid: the mother liquor is put into another 3000L glass-lined reactor, 30% dilute sulfuric acid is added dropwise to make PH=1, spin dry, rinse on the centrifuge, spin dry, and dry. 174kg of 4,4'-biphthalic acid, with a content of 99.6%.

References:

CN111138268,2020,A Location in patent:Paragraph 0023-0034