对2,4-二硝基苯酚合成方法的改进

Modification on a Synthetic Method of 2,4 Dinitrophenol

明显改进了由２，４－二硝基氯苯合成２，４－二硝基苯酚的生产工艺。在１０００ｍＬ四颈瓶中进行的试验表明：水解及酸化反应的原料２，４－二硝基氯苯、氢氧化钠、盐酸的适宜摩尔比为１∶（２．０８～２．２３）∶（１．１１～１．２３），适宜的水解温度及酸化温度分别为９１～１０２℃、７０℃，适宜的搅拌速度为４００～５００ｒ／ｍｉｎ，适宜的水解反应时间为１５０ｍｉｎ。６０ｔ／ａ的生产装置在十分相似的工艺条件下运行获得成功，工业生产装置上搅拌器转速改变为１３６ｒ／ｍｉｎ。新的工艺流程水解步骤完成后直接进行酸化，过滤可在室温至３５℃下进行，操作过程大为简化，废水显著减少，产率达到９８％。

A two—step method for synthesizing 2,4 dinitrophenol from 2,4 dinitrochlorobenzene (Ⅰ) has been significantly modified.Experiments in a 1000mL flask show that the optimum hydrolytic temperature and reaction time are 91～102℃ and 2 5h respectively,acidizing temperature is 70℃,the optimum molar ratio of the three reactants (2,4 dinitrochlorobenzene Ⅰ,sodium hydroxide Ⅱ,hydrochloric acid Ⅲ)is Ⅰ∶Ⅱ∶Ⅲ=1∶(2 08～2 23)∶(1 11～1 23),and the optimum stirring speed is 400～500r/min. According to the conditions above,a 60t/a industrial plant ran successtully by changing stirring speed to 136r/min. By acidizing directly after complete hydrolysis,the new process is much simpler,produces less waste water,and the yield is 98%.