SiCl4是光纤制造的关键原材料,其质量的高低决定着光纤的传输性能.SiHCl3是SiCl4中常见的一种含氢杂质,其含量的多少对SiCl4质量产生严重影响.综述了国内外对于SiCl4中SiHCl3去除方法的研究进展,主要有精馏法、等离子体法、光化法,以及吸附法、部分水解法等其他一些方法.国内常用精馏法提纯SiCl4,但由于SiHCl3和SiCl4的沸点较为接近,精馏法对于SiCl4中SiHCl3的去除仍然存在着一定的限度;等离子体法去除SiHCl3效果好,但对于设备、技术要求相对较高;光化法对于SiHCl3的去除十分有效,可将SiHCl3的含量降到1×10-6以下.同时介绍了SiCl4中SiHCl3含量的检测方法,包括气相色谱法、傅里叶变换红外光谱法(FT-IR法)、红外空气参考法.气相色谱法具有取几毫克SiCl4即可检出其中微克级SiHCl3的特点,其检测下限为0.1×10-6;FT-IR法不仅可用于实验室分析,而且可应用于生产现场分析,对SiHCl3的测量下限为0.6×10-6;红外空气参考法对SiHCl3的测量下限为2×10-6.进行SiCl4中SiHCl3的去除工艺、检测技术研究,对于光纤用高纯SiCl4的提纯,进而对于光纤用关键原料国产化,具有重要的意义.
参考文献
| [1] | 胡先志;邹林森;刘有信.光缆及工程应用[M].北京:人民邮电出版社,1998:33. |
| [2] | 袁永春.副SiCl4生产光纤用高纯SiCl4[J].四川有色金属,1999(01):31. |
| [3] | 上海九○一厂.半导体材料硅[M].上海:上海东方红印刷厂,1971:30. |
| [4] | 吕咏梅 .四氯化硅工业应用研究进展[J].江苏氯碱,2007,4:17. |
| [5] | 孙福星,王铁艳,袁琴,韩国华,耿宝利.国内外光纤用SiCl4研究进展[J].稀有金属,2008(04):513-517. |
| [6] | Koho K K .Purification of silicon tetrachloride[P].JP:59-013618,1984. |
| [7] | 周翔;周骏 .光纤用高纯四氯化硅的生产方法[P].CN:1554581,2004. |
| [8] | Spevak .Purification of silicon tetrachloride by fraction[P].USSR:327782,1976. |
| [9] | Ogihara;Tsutomu .Purification of silicon tetrachloride[P].EP:488765,1994. |
| [10] | Hans-Joachim K .Method of purifying chlorosilanes[P].EP:54650,1982. |
| [11] | Popp H P;Nicolai R;Ranleder H;Lang J .Process and apparatus for purifying silicon tetrachloride or germanium tetrachloride containing hydrogen compounds[P].WO:013129,2006. |
| [12] | Lang J;Nicolai R;Ranleder H .Reactor,plant and industrial process for the continuous preparation of high-purity silicon tetrachloride or high-purity germanium tetrachloride[P].WO:025787,2007. |
| [13] | 邢瑞芝;朱中南 .光化学反应工程[J].化学反应工程与工艺,1994,10(02):187. |
| [14] | Huang R L.自由基化学[M].上海:上海科学技术出版社,1983:23. |
| [15] | 穆光照.自由基反应[M].北京:高等教育出版社,1985:38. |
| [16] | David A;Michael P;Patricia A .Ultrapurification of SiCl4 by photochlorination in a bubble column reactor[J].AICHE Journal,1990,36(02):216. |
| [17] | Bams .Purification progress for compounds useful in optical fibre manufacture[P].US:4372834,1983. |
| [18] | 于剑昆.四氯化硅的合成与精制[J].无机盐工业,2007(12):5-8. |
| [19] | 叶启亮,于建国,房鼎业.通信光纤原料SiCl4提纯方法[J].化工生产与技术,2004(01):23-25. |
| [20] | 刘秀喜;林明喜;薛成山.高纯气体的性质、制造和应用[M].北京:电子工业出版社,1997:469. |
| [21] | Kometani;Thomas Y .Method of preparing optical fibers of silica[P].US:4282196,1981. |
| [22] | 张严 .光纤级高纯度四氯化硅生产方法[P].CN:1958445A,2007. |
| [23] | Simons;Dennis .Method of preparing very pure silicon chloride and &sol:or germanium chloride[P].WO:059808,2003. |
| [24] | Kerr J A;Timlin D M .Hydrogen abstraction reactions from organosilicon compounds.The reactions of fluoromethyl radicals with trichlorosilane.The photolyses of di-and tetrafluoroacetone[J].International Journal of Chemical Kinetics,1971,3(01):l. |
| [25] | Kerr J A;Stephens A;Young J C .Hydrogen abstraction reactions from organosilicon compounds.The reactions of methyl,trifluoromethyl,and ethyl radicals with trichlorosilane[J].International Journal of Chemical Kinetics,1969,1(04):371. |
| [26] | Hans R;Aachen .Process for the removal of hydrogen from hydrogen compounds dissolved in silicon tetrachloride or germanium tetrachloride[P].US:4842839,1989. |
| [27] | Yamada M;Ishii M;Miyai A;Nakajima Y,Sato S .Chlorosilane disproportionation catalyst and method for producing a silane compound by means of the catalyst[P].US:4610858,1986. |
| [28] | 李卜森,朱新芳,张琪.光纤原料四氯化硅中微量三氯氢硅的气相色谱分析[J].色谱,1994(02):108. |
| [29] | 朱新芳;李卜森;张琪 .FT-IR法测鼍高纯四氯化硅中的微量三氯氢硅[J].光谱学与光谱分析,1994,14(02):35. |
| [30] | 梁洪 .红外空气参考法测定光纤用SiCl4中的总氢[J].四川有色金属,1999,3:45. |
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