CN111661968A - 头孢西丁酸废液中回收溶剂工艺 - Google Patents
头孢西丁酸废液中回收溶剂工艺 Download PDFInfo
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Abstract
近年来,随着制药行业的快速发展,我国原料药和药品的制剂生产一万多种,废水废排放量达0.25GT/年。年平均处理率还不到30%。在制药产品的生产工艺中产生大量的高污染的有机废水,成分复杂,毒性大,色度高,水质水量变化大而难生物降解,是工业废水中较难处理的一种,被列入《国家危险废物名录》2016版中,编号HW02类。在生产头孢西丁酸原料药过程中,产生的残余排污水中含有两种有机溶剂,即乙酸乙酯和丙酮混合液,难以用常规的工艺将其单一的回收利用。头孢西丁酸废液中回收溶剂工艺采用的方法为:先从废水中回收两混合溶剂,再进行盐析,将乙酸乙酯与丙酮分离、脱水、分馏等工序,处理后即达到工业级的乙酸乙酯与丙酮产品回收利用。
Description
一、技术领域
21世纪,制药行业进入了快速发展的阶段,2016年统计数据表明,我国已成为名副其实的医药制品生产大国,是世界第二大原料药生产国。
制药过程非常复杂,产生的中间体和代谢产物,大量的高浓度、高毒性、难降解的残留物。随着制药行业的持续发展,废水排放量越来越大,占到总工业废水量的3%左右。该类废水被列入《国家危险废物名录》2016版中,编号HW02类。
本发明对头孢西丁酸废液中回收溶剂工艺,属于环境技术领域,研究的学科是环境科学技术,环境工程学及有毒污染物防治工程。自2010年7月1日起,强制推行《制药工业水污染物排放标准》,已成为国家环境保护重点治理的行业之一。
二、背景技术
目前制药废水治理技术有:
1.混凝沉淀法:
这是最常用的预处理方法,通过投加化学药剂,使其产生吸附,中和微粒间电荷,压缩扩散双电子层产生的混聚作用。在重力作用下沉淀。其优点为不仅有效降低污染物浓度还可以改善废水的生物降解性能,缺点是会产生大量的化学污泥,造成二次污染,出水的PH值较低,含盐量高,对氨氮的除去率较低。
2.吸附法:
指利用多孔性固体吸附废水中一种或几种污染物,以回收或去除污染物,从而使废水得到净化的方法,优点是处理效果好,缺点是成本高。
有关资料介绍,膜分离、铁碳法、光催化氧化法、生化法、上流式厌氧污泥床(UASB)、HVSB、UBF、ABR等生化处理技术。
根据制药废水的特点,仅靠单一的处理工艺很难使出水达标排放,必须用多种工艺联合处理的方法,才能有效即达到处理的最终要求。同时必须对废水中回收部分有回收价值的有机溶剂,才能实现资源处理费用与成本平衡,回收与利用的社会经济价值。
参考文献
1.制药厂废水处理技术及研究进展.陈美花.科学与财富.2018,(20).
2.制药厂废水处理技术研究进展.张岩.工业水处理.2018.5.38.(5.)
3.中华人民共和国工业和信息化部.医药工业发展规划指南.(EBOL).208-11-07.
4.Karelidv.LarssonG.Berade B.Pilod Scale removal Pnafcuaceuti-Calsofgranular and Poudered activrated Carbon Tracrment at tnce WastewaterTreatment Plants[J].Journal of Environmental Management.2017.193,491-502.
三、发明内容
本发明在工业化生产线上实施的方法为:针对乙酸乙酯与丙酮为低沸点、易挥发的特点,对两混合溶剂的废水量置于蒸馏釜内进行蒸馏,将两溶剂与废水分离。蒸馏液通过盐析手段,将乙酸乙酯与丙酮分离,乙酸乙酯加无水硫酸钠除杂,丙酮经过分馏后,加无水氯化钙干燥。
有机残余液经氧化——混凝方式处理,可达标排放。
四、具体工艺步骤如下:
1.乙酸乙酯物化参数
无色具有芳香气味的液体,微溶于水,沸点77℃,在空气中可燃极限2.2-9%。
2.丙酮物化参数
无色易挥发、易燃液体,能与水、醇、醚等有机溶剂混溶,沸点56.5℃,爆炸极限2.05-19.0(体积)。
3.将两溶剂的废水置于密封蒸馏釜进行蒸馏,收集两溶剂混合液,在有搅拌容器中,加入20%的氯化钠溶剂盐析。有机相为乙酸乙酯,用无水硫酸钠脱水,水相中丙酮经过分馏、脱水剂用无水氯化钙干燥。
Claims (3)
1.一种头孢西丁酸废液中回收溶剂工艺,将有毒残留液置于蒸馏容器中,加热对乙酸乙酯、丙酮等混合液进行常规蒸馏,得到无色的混合溶剂。
2.根据权利要求1的概述:蒸馏液经过化验,准确测得乙酸乙酯、丙酮的含量。混合溶剂在1:17转的搅拌釜内,加入10%的含盐(氯化钠溶液)分五次洗涤,取乙酸乙酯样品,测丙酮含有量低于千分之三即盐析终点。
乙酸乙酯溶液中加入无水硫酸钠脱水干燥回用,硫酸钠干燥后回用。
丙酮溶液经分馏塔处理,用无水氯化钠处理后回用,氯化钙干燥后回用,盐析液回用。
3.残余液用生物、化学法处理后,达标排放。
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