不同氯化度的氯化石蜡制备方法研究

doi:10.3976/j.issn.1002-4026.2021.05.012

山东科学 ›› 2021, Vol. 34 ›› Issue (5): 97-103.doi: 10.3976/j.issn.1002-4026.2021.05.012

不同氯化度的氯化石蜡制备方法研究

李慧娟¹，刘兰畦¹，赵梅¹，宋善军²，陈相峰^1*

1.齐鲁工业大学（山东省科学院）山东省分析测试中心，山东济南 250014；2.中国计量科学研究院，北京 100029

收稿日期:2020-11-30 出版日期:2021-10-14 发布日期:2021-10-18
通信作者: 陈相峰，男，研究员，研究方向为食药安全与风险评估。E-mail: xiangfchensdas@163.com
作者简介:李慧娟（1987—），女，博士，助理研究员，研究方向为污染物分析与风险评估。E-mail:ldlihuijuan@163.com
基金资助:
国家自然科学基金(21906096)

Synthesis of chlorinated paraffins with different chlorination degrees

LI Hui-juan¹, LIU Lan-qi¹, ZHAO Mei¹, SONG Shan-jun², CHEN Xiang-feng^1*

1. Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, China; 2. National Institute of Metrology, Beijing 100029, China

Received:2020-11-30 Online:2021-10-14 Published:2021-10-18

摘要/Abstract

摘要： 通过自行搭建的实验装置（包括回流反应装置、干燥装置、碱液吸收装置和抽真空惰性气体置换保护装置），将癸烷（decane）与磺酰氯（SO₂Cl₂）试剂在汞灯（10 W, 254 nm）照射下进行自由基取代反应，合成了不同氯化度的碳链长度为10个碳原子的氯化石蜡标准品（C₁₀-chlorinated paraffins, C₁₀-CPs）。合成的粗产品通过硅胶和弗罗里硅土复合柱的净化吸收去除未反应的癸烷，实现反应产物的纯化。将纯化后的氯化石蜡标准品通过气相色谱/质谱进行产物纯度分析和不同单体组成模式分析。结果表明，净化后的标准品中不含癸烷和其他杂质，氯化石蜡单体主要以Cl₇、Cl₈单体为主。光照、温度和反应时间对产物的氯化度有一定的影响，通过计算得到合成产物的纯度在98%以上，氯化度在55.6%~66.9%。结果表明此方法可以用来制备不同氯化度的氯化石蜡标准品。

关键词: 氯化石蜡, 合成, 反应装置, 氯化度, 标准品

Abstract: An experimental equipment, which included a reflux reaction device, a drying device, a lye absorption device, and a vacuum inert gas replacement protection device, was set up to synthesize chlorinated paraffins (CPs) with different chlorination degrees. CPs with a carbon chain length of 10 (C₁₀-CPs) were synthesized through radical substitution reaction by refluxing decane with sulfuryl chloride (SO₂Cl₂) in the presence of a mercury lamp (10 W, 254 nm). Purification of reaction products was achieved via adsorption chromatography on silica gel and Florisil composite column to remove the unreacted decane. The products′ purity and their congener profiles were characterized via gas chromatography/mass spectrometry (GC/MS) operated in electron ionization (EI) and in the electron capture negative ionization (ECNI) modes. The results showed that the purified product does not contain decane and other impurities. The C₁₀-CPs with seven and eight chlorine atoms were the most abundant congeners. It was found that the light intensity, reaction temperature, and reaction time influence the chlorination degree of the product. The calculated purity of the synthesized product was above 98%, and the chlorination degree was between 55.6% and 66.9%. The results showed that this method can be used to produce CPs with different chlorination degrees.

Key words: chlorinated paraffins, synthesis, reaction equipment, degree of chlorination, standard product

中图分类号:

X502

李慧娟, 刘兰畦, 赵梅, 宋善军, 陈相峰. 不同氯化度的氯化石蜡制备方法研究[J]. 山东科学, 2021, 34(5): 97-103.

LI Hui-juan, LIU Lan-qi, ZHAO Mei, SONG Shan-jun, CHEN Xiang-feng. Synthesis of chlorinated paraffins with different chlorination degrees[J]. Shandong Science, 2021, 34(5): 97-103.

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不同氯化度的氯化石蜡制备方法研究

Synthesis of chlorinated paraffins with different chlorination degrees

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