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High purity 4,4'-Isopropylidine-bis-2,6 dibromophenol and process for the preparation of such high purity 4,4'-Isopropylidine-bis-2,6 dibromophenol

机译:高纯度4,4'-异丙基吡啶-双-2,6二溴苯酚及其制备方法

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.
机译:高纯度的4,4'-异丙基吡啶-双-(2,6-二溴苯酚),其特征在于离子溴化物小于10 ppm,在碱性溶液中的颜色为60-100 HU,HPLC纯度约为99.9%,APHA为20%MeOH溶液小于10.0 HU,铁小于1.0 ppm,浊度为20%的MeOH溶液小于5 NTU,pH为10%的浆液为6.0-7.0,晶体颗粒尺寸为250至280微米,休止角小于30°。通过在过氧化氢存在下,在“水不混溶”极性溶剂中使双酚A与溴反应,在反应后使反应产物老化,通过还原剂消除过量的溴,并结合洗涤产物层来生产产物。在控制pH的条件下将阴离子表面活性剂,碱,还原剂和软化水进行部分蒸馏,将含有该产品的介质冷却,冷却粗产物,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获得高收率的最终高纯度TBBA。

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