农残级正己烷的产业化制备纯化工艺研究  

Purification process of industrialization preparation of pesticide residue grade n-hexane

作　　者：鄢雄伟[1] 全灿[2] 金君素[1] 黄挺[2] 李红梅[2] 

机构地区：[1]北京化工大学化工学院,北京100029 [2]中国计量科学研究院化学计量与分析科学研究所,北京100013

出　　处：《化学试剂》2012年第6期545-548,551,共5页Chemical Reagents

基　　金：国家科技支撑计划资助项目(2009BAK61B02)

摘　　要：以工业级正己烷为原料,通过脱色-连续精馏-过滤等一系列纯化工艺制备农残级正己烷,用紫外吸光度、纯度(GC-FID)和杂质峰高(GC-ECD)等检测值作为农残质量控制指标。产品质量与占当前国内垄断市场的进口试剂水平相当。通过试验确定了较为合适的工艺条件:二氧化硅为脱色剂,用量是原料质量的2%,然后用10%的蒸馏水水洗一次,连续精馏装置的导热油加热温度为88℃,脱轻塔和成品塔的回流比分别为10∶1和4∶1,重组分放料速率20 mL/min,产率可达70%左右。Pesticide residue grade solvents have the character- istic of ultra high purity, low UV value, low pH value, low moisture content and low evaporation residue, which do not have those controlled impurity peak in pesticide chromato- graphic detection. This project funded by the China govern- ment, in which the industrialization process of pesticide resi- due grade n-hexane was studied, the industrial n-hexane as crude after purification approaches including decoloration, dis- tillation and filtration. The optimized process parameters are： firstly utilizing 2% of silicon dioxide as decoloration agent then is rinsed with distilled water before distillation. The heat- ing temperature of two distillation towers is 88℃ with reflux ratio of 10：1 and 4：1 for both respectively ,the discharge rate of heavy component is 20 mL/min,the yield is approximately 70%. This patented technique will meet pesticide residue grade n-hexanc market in China or globally.

关 键 词：农残分析 正己烷 纯化 脱色 精馏 

分 类 号：TQ421[化学工程]