高纯度氧硫化碳的制备
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摘要
在对目前氧硫化碳(COS)合成方法进行分析的基础上,开发了一种新的可用于工业生产高纯度COS的技术。该合成工艺以一氧化碳和单质硫为原料,二硫化铁(FeS_2)为催化剂,通过预纯化控制原料杂质含量,催化剂干燥脱水,设备预处理(钝化、吹扫、脱水),反应后粗纯化(冷冻分离、吸附)和低温精馏等过程,制得的产品φ(COS)>99.95%,质量完全能满足市场要求。该COS制备过程被介绍,通过实验确定了较为适宜的工艺参数,并对过程中出现的现象及存在的问题进行了描述和讨论。
On the basis of analyzing existing synthetic methods of carbonyl sulfide(COS), a novel high purity COS preparation process which could be used for commercial production was developed. This gas phase synthesis process used carbon monoxide and elemental sulfur as raw material and FeS_2 as catalyst, by which, through pretreating the raw materials to reduce their impurities contents, catalyst drying, equipment pretreatment(passivation, purging and dehydration), resultant pre-purification(freezing and adsorption) and cryogenic distillation, a product with COS volume fraction of above 99.95% could be obtained, which would meet the requirements of the market. The process was expounded and the proper technical parameter was determined by experiments.Moreover, phenomena and existing problems of the preparation process were described and discussed.
On the basis of analyzing existing synthetic methods of carbonyl sulfide(COS), a novel high purity COS preparation process which could be used for commercial production was developed. This gas phase synthesis process used carbon monoxide and elemental sulfur as raw material and FeS_2 as catalyst, by which, through pretreating the raw materials to reduce their impurities contents, catalyst drying, equipment pretreatment(passivation, purging and dehydration), resultant pre-purification(freezing and adsorption) and cryogenic distillation, a product with COS volume fraction of above 99.95% could be obtained, which would meet the requirements of the market. The process was expounded and the proper technical parameter was determined by experiments.Moreover, phenomena and existing problems of the preparation process were described and discussed.
引文
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[6]Almond M J,Cockayne B,Cooke S A,et al.Carbonyl sulfide(OCS)as a sulfur-containing precursor in MOCVD:a study of mixtures of Me2Cd and OCS in the gas and solid phases and their use in MOCVD[J].J Mater Chem,1996,6:1639-1642.
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[8]唐英.国外羰基硫研究概况[J].辽宁化工,1987,(4):49-52.
[9]Bartholomaeus A R,Haritos V S.Review of the toxicology of carbonyl sulfide,a new grain fumigant[J].Chem Toxicol,2005,43:1687-1701.
[2]郭汉贤,谈世韶,李春虎.羰基硫的研究动向[J].山西化工,1988,(3):22-26.
[3]Ferm R J.The chemistry of carbonyl sulfide[J].Chem Rev,1957,57:621-640.
[4]孙福楠,冯庆祥,吴江红.高纯羰基硫的生产[J].低温与特气,2004,22(3):32-34.
[5]Svoronos P D N,Bruno T J.Carbonyl sulfide:A review of its chemistry and properties[J].Ind Eng Chem Res,2002,41:5321-5336.
[6]Almond M J,Cockayne B,Cooke S A,et al.Carbonyl sulfide(OCS)as a sulfur-containing precursor in MOCVD:a study of mixtures of Me2Cd and OCS in the gas and solid phases and their use in MOCVD[J].J Mater Chem,1996,6:1639-1642.
[7]Takahashi N,Ogawa S,Uchiyama M,et al.Process for preparation of carbonyl sulfide[P].US:42243000,1980.
[8]唐英.国外羰基硫研究概况[J].辽宁化工,1987,(4):49-52.
[9]Bartholomaeus A R,Haritos V S.Review of the toxicology of carbonyl sulfide,a new grain fumigant[J].Chem Toxicol,2005,43:1687-1701.