公开(公告)号：US06613947B1

公开(公告)日：2003-09-02

申请号：US10168454

申请日：2002-10-21

申请人： Shantaram Narayan Naik ,  Dharma Ratnakar Ramdas Naik ,  M. Madhusudan Rao

发明人： Shantaram Narayan Naik ,  Dharma Ratnakar Ramdas Naik ,  M. Madhusudan Rao

IPC分类号： C07C3916

CPC分类号： C07C37/62 ,  C07C39/367 ,  H05K1/0373

摘要： A high purity 4,4′-isopropylidine-bis-(2,6-dibromophenol) characterised by ionic bromides less than 10 ppm, colour in alkaline solution from 60-100 HU, HPLC purity about 99.9%, APHA of 20% MeOH solution less than 10.0 HU, Fe less than 1.0 ppm, turbidity of 20% MeOH solution less than 5 NTU, pH of 10% slurry 6.0-7.0, size of the crystal particles, 250 to 280 microns with angle of repose lower than 30°. The product is produced by reacting Bisphenol-A with bromine in a “water-immiscible” polar solvent in the presence of hydrogen peroxide, aging the reaction products after the reaction, eliminating the excess bromine by reducing agents, washing the product layer with a combination of anionic surfactant, alkali, reducing agent and demineralised water under controlled pH conditions, partially distilling the organic solvent chilling the medium containing the product, filtering the crude product, boiling the crude product with alkali, reducing agent and demineralised water, filtering the TBBA, washing the product with demineralised water and drying to obtain the final high purity TBBA with high yield.

摘要翻译： 高纯度4,4'-异丙基 - 双 - （2,6-二溴苯酚），其特征在于离子型溴化物小于10ppm，碱性溶液中颜色为60-100HU，HPLC纯度约99.9％，APHA为20％MeOH溶液 小于10.0HU，Fe小于1.0ppm，浊度为20％MeOH溶液小于5NTU，pH为10％浆液6.0-7.0，晶粒尺寸为250至280微米，休止角低于30°。 该产物通过双酚A与溴在过氧化氢存在下在“与水不混溶”的极性溶剂中反应生成，使反应后的反应产物老化，通过还原剂消除过量的溴，用组合物洗涤产物层 的阴离子表面活性剂，碱，还原剂和软化水，部分蒸馏含有产物的培养基的有机溶剂，过滤粗产物，用碱，还原剂和软化水煮沸粗产物，过滤TBBA， 用软化水洗涤产物并干燥，以高产率获得最终的高纯度TBBA。