采用阳离子交换树脂将2,6-萘二磺酸钠转化为2,6-萘二磺酸并用于双酚S(BPS)合成,研究了转化时间、温度、树脂用量等条件对反应的影响. 较优的转化条件为:将2,6-萘二磺酸钠完全溶解后,加入用量为理论值37倍的001×7型强酸性聚苯乙烯系阳离子交换树脂,常温转化24 h,用转化产物催化合成的BPS粗品收率为93.5%,BPS质量分数为92.3%. 采用水-吸附剂体系进行精制,不添加有机试剂,BPS产品质量分数高,操作简单,易于工业化. 较优的精制条件为:7 g BPS粗品加热溶于300 g去离子水后,加入0.5 g海泡石、0.2 g活性炭,回流搅拌1 h,过滤后潮品再加热溶于180 g去离子水中,加入0.3 g海泡石,回流搅拌1 h,得白色产品,BPS质量分数可达99.7%. 精制水可循环套用且可提高BPS产品收率至82.9%.
Transformation of disodium 2,6-naphthalenedisulfonate into 2,6-naphthalenedisulfonic acid was catalyzed by cationic exchange resin and the 2,6-naphthalenedisulfonic acid was used to catalyze the synthesis of bisphenol S(BPS).The effects of the reaction time, temperature and the amount of resin were investigated.The optimized exchange process was applied as follows:After disodium 2,6-naphthalenedisulfonate was completely dissolved, 37 times of 001×7 strong acidic polystyrene type cationic exchange resin were added into the system.The converted products were used to catalyze the synthesis of BPS.The yield of crude product BPS reached 93.5% and the mass fraction of BPS was 92.3%.Crude BPS was purified by adsorbent without organic solvent.The mass fraction of the product obtained by the process is high.The improved process is easy to be operated and industrialized.The improved purification process was applied as follows:Firstly 7 g of crude BPS was dissolved in 300 g hot water.Then 0.5 g sepiolite and 0.2 g active carbon were added under stirring.The wet product was dissolved in 180 g hot water again and another 0.3 g sepiolite was added.After 1 hour of stirring, a white product was obtained and the purity of BPS reached 99.7%.The water could be recycled, resulting in increasing yield of product BPS to 82.9% at the same time.
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