화학공학소재연구정보센터
홈 로그인 로그아웃 연락처 사이트맵
Journal of Industrial and Engineering Chemistry, Vol.109, 275-286, May, 2022
DOI10.1016/j.jiec.2022.02.015  Export Citation
Simultaneous distillation-extraction for manufacturing ultra-high-purity electronic-grade octamethylcyclotetrasiloxane (D4)
Wenhui Guo1, Shuhu Guo2, 3, Xu Zhao3, Zhenjun Yuan3, Yu Zhao3, Xin Chang3, Hong Li1, Xiong Zhao1, 2, †, Ye Wan2, 3, †, Dazhou Yan2, 3, Zhongyuan Ren4, †, Xiaolei Fan5, and Xin Gao1, 6, †
  • 1School of Chemical Engineering and Technology, National Engineering Research Center of Distillation Technology, Tianjin University, Tianjin 300072, China
  • 2China ENFI Engineering Co., Ltd., Beijing 100038, China
  • 3National Engineering Research Center of Silicon-based Materials Manufacturing Technology, Luoyang 471023, China
  • 4Jilin Institute of Chemical Technology, No. 45 Chengde Street, Jilin 132022, China
  • 5Department of Chemical Engineering, School of Engineering, The University of Manchester, Oxford Road, Manchester M13 9PL, United Kingdom, UK
  • 6Haihe Laboratory of Sustainable Chemical Transformations, Tianjin 300192, China
E-mail:, , ,
Ultra-high-purity (UHP) electronic-grade octamethylcyclotetrasiloxane (D4) is the key precursor of lowdielectric constant (low-k) SiCOH films to manufacture integrated circuits (IC), meeting the stringent requirements of the rapidly developing semiconductor industry. Commonly, metallic impurities in D4 were removed by multiple unit operations of adsorption, filtration, and distillation, which could reduce the concentration of a single metallic impurity below 1 ppb. However, D4 with higher purity is required by semiconductor production due to an increase in transistor density. Herein, a novel method based on the integrated simultaneous distillation–extraction (SDE) was developed for manufacturing UHP electronic-grade D4. The lab and pilot scale experiments showed that the purity of water and D4 has a positive correlation. Based on the experimental data, a double-column process, consisting of azeotropic/ extractive distillation column and precision distillation column with UNIQUAC method, was established to access the feasibility of scaling up the SDE process. According to the simulation results, D4 with the purity > 99.999 wt.% and total metallic impurities (TMI) content below 1 ppb could be obtained using ultra-pure water.
Keywords:Octamethylcyclotetrasiloxane (D4);Process integration;Simultaneous distillation-extraction;Electronic-Grade
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