| 升华提纯法制备三氯叔丁醇高纯试剂的研究 |
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| 引用本文： | 李清洁,费荣杰,丁春玉,王志刚,成义祥.升华提纯法制备三氯叔丁醇高纯试剂的研究[J].化学试剂,2017,39(10). |
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| 作者姓名： | 李清洁 费荣杰 丁春玉 王志刚 成义祥 |
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| 作者单位： | 1. 南京化学试剂股份有限公司,江苏南京,210047;2. 南京大学化学化工学院,江苏南京,210023 |
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| 摘 要： | 采用升华提纯法制备半水合三氯叔丁醇高纯试剂,探索了升华温度和升华时间对工艺的影响。利用气相色谱仪(GC)和电感耦合等离子体质谱(ICP-MS)测试升华前后半水合三氯叔丁醇的纯度和金属离子含量的变化。参照美国西格玛试剂指标对样品进行检测分析,结果表明半水合三氯叔丁醇在100℃下升华14 h,收率达98.2%,不出现分解,所得试剂纯度高达99.96%,并具有较低的金属离子含量。
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| 关 键 词： | 升华提纯 半水合三氯叔丁醇 高纯试剂 升华温度 |
Preparation of High Purity Reagents of Chlorobutanol by Sublimation Purification Method |
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| LI Qing-jie,FEI Rong-jie,DING Chun-yu,WANG Zhi-gang,CHENG Yi-xiang.Preparation of High Purity Reagents of Chlorobutanol by Sublimation Purification Method[J].Chemical Reagents,2017,39(10). |
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| Authors: | LI Qing-jie FEI Rong-jie DING Chun-yu WANG Zhi-gang CHENG Yi-xiang |
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| Abstract: | The preparation of high purity reagent of hemihydrate chlorobutanol was investigated by changing sublimation temperature and sublimation time.The purity of hemihydrate chlorobutanol and the change of metal ions content were measured by gas chromatography (GC) and inductively coupled plasma mass spectrometry (ICP-MS) before and after sublimation,respectively.The purity of the obtained hemihydrate chlorobutanol can reach 99.96％ and the yield is 98.2％ with lower metal ions content at 100 ℃ for 14 h sublimation time. |
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| Keywords: | sublimation purification hemihydrate chlorobutanol high purity reagent sublimation temperature |
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