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

• Environment and Ecology • Previous Articles     Next Articles

Synthesis of chlorinated paraffins with different chlorination degrees

LI Hui-juan1, LIU Lan-qi1, ZHAO Mei1, SONG Shan-jun2, CHEN Xiang-feng1*   

  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

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

CLC Number: 

  • X502