2,6-二叔丁基-4-氨基苯酚的合成工艺研究

Studies on synthetic process for 2,6-di-tert-butyl-4-aminophenol

以2，6-二叔丁基苯酚（DTBP）为原料通过亚硝化反应、还原反应合成2，6-二叔丁基-4-氨基苯酚（DTBAP）。通过单因素实验系统考察了反应工艺条件得出：①亚硝化反应：以95%乙醇为溶剂，以浓盐酸为酸化试剂，亚硝酸钠用量为DTBP摩尔量1.25-1.50倍，反应温度为15-20℃，反应时间2.0-2.5h，产品收率达90%以上；②还原反应：以连二亚硫酸钠为还原剂，在50-55℃下反应60min，连二亚硫酸钠用量为2，6-二叔丁基-4-亚硝基苯酚摩尔数的2.8倍及以上，产品收率可达到92%以上。制备方法操作简单，反应条件温和、易于控制，产物易于分离，产品总收率较高，反应原料廉价、容易采购，生产成本较低，适合于工业化生产。

Using the 2,6-di-tert-butyl phenol（ DTBP）as raw material,after the nitrosation reaetion and the reduetion reaetion,we could get the di-tert-butyl-4-aminophenol（ DTBAP）. Through single faetors test effeets of reaetion eonditions,we eonsider the eondition of reaetion teehnology,and get the eonelusion：①the nitrosation reaetion：we ean get the produets at the rate up to 90% above,if we make 95% ethanol as the solvent,eoneentrated hydroehlorie aeid as aeidifieation reagents;the amount of the sodium nitrite is 1. 25-1. 50 times of the moles of the DTBP,the reaetion temperature 15-20 ℃;reaetion time is 2. 0-2 . 5 h;②the reduetion reaetion：we ean get the produets at the rate up to 92%,if we make the sodium di-thionite as the reduetant,the reaetion temperature 50-55 ℃;the amount of the sodium dithionite is more than 2. 8 times of the moles of 2,6-di-tert-butyl-4-nitrosophenol. The preparation method is simple,of a mild reaetion eonditions,easy to eontrol and easy to separate the produets,of high total yield,eheap and easy to get the raw materials,low produetion costs. So it is suitable for industrial production.