首页> 外国专利> HIGH PURITY 4,4-ISOPROPYLIDENE-BIS-(2,6 DIBROMOPHENOL) AND PROCESS FOR THE PREPARATION OF SUCH HIGH PURITY 4,4-ISOPROPYLIDENE-BIS-(2,6 DIBROMOPHENOL)

HIGH PURITY 4,4-ISOPROPYLIDENE-BIS-(2,6 DIBROMOPHENOL) AND PROCESS FOR THE PREPARATION OF SUCH HIGH PURITY 4,4-ISOPROPYLIDENE-BIS-(2,6 DIBROMOPHENOL)

机译:高纯度4,4-异丙烯-双-(2,6二溴酚)和制备这种高纯度4,4-异丙烯-双-(2,6二溴酚)的方法

摘要

A high purity 4-4'-isopropylidine-(2,6-di-bromophenol) characterized by ionic impurities less than 10 ppm, colour in alkaline solution from 60-100 HU, HPLC purity about 99.9 %, APHA of 20 % MeOH solution less than 10.00 HU, Fe less than 1.0 ppm, turbidity of 20 % MeOH solution less than 5.0 HU, pH of 10 % slurry 6.0-7.0, average particle size of 250-280 nm and angle of repose equal to or less than 35°. 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4-4'-异丙基-(2,6-二溴苯酚),特征在于离子杂质小于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10.00 HU,铁小于1.0 ppm,浊度为20%的MeOH溶液小于5.0 HU,pH为10%的浆液为6.0-7.0,平均粒径为250-280 nm和休止角等于或小于35° 。通过在过氧化氢的存在下,在“水不混溶”极性溶剂中使双酚A与溴反应,反应后反应产物老化,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产率的最终高纯度TBBA。

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