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yibaigood

新虫 (著名写手)

[交流] 请问,DMSO如何纯化?

请问,DMSO如何纯化?
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xiazaibaobao

至尊木虫 (职业作家)


chemcccc(金币+1):thx
沸点189℃,熔点18.5℃,折光率1.4783,相对密度1.100。二甲基亚砜能与水混合,可用分子筛长期放置加以干燥。然后减压蒸馏,收集76℃/1600Pa(12mmHg)馏分。蒸馏时,温度不可高于90℃,否则会发生歧化反应生成二甲砜和二甲硫醚。也可用氧化钙、氢化钙、氧化钡或无水硫酸钡来干燥,然后减压蒸馏。也可用部分结晶的方法纯化。二甲基亚砜与某些物质混合时可能发生爆炸,例如氢化钠、高碘酸或高氯酸镁等应予注意。
2楼2006-10-17 20:07:51
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smilefish1227


chemcccc(金币+1):thx
详细的处理步骤

Dimethyl sulfoxide (DMSO) [67-68-5] M 78.1, m 18.0-18.5°, b 75.6-75.8°/12mm,
190°/760mm, d 1.100, n 1.479. Colourless, odourless, very hygroscopic liquid, synthesised from dimethyl sulfide. The main impurity is water, with a trace of dimethyl sulfone. The Karl-Fischer test is applicable. It is dried with Linde types 4A or 13X molecular sieves, by prolonged contact and passage through a column of the material, then distd under reduced pressure. Other drying agents include CaH2, CaO, BaO and CaSO4. It can also be fractionally crystd by partial freezing. More extensive purification is achieved by standing overnight with freshly heated and cooled chromatographic grade alumina. It is then refluxed for 4h over CaO, dried over CaH2, and then fractionally distd at low pressure. For efficiency of desiccants in drying dimethyl sulfoxide see Burfield and Smithers [/ Org Chem 43 3966 1978\ Sato et al. / Chem Soc, Dalton Trans 1949 1986].
Rapid purification: Stand over freshly activated alumina, BaO or CaSO4 overnight. Filter and distil over CaH2 under reduced pressure (~ 12 mm Hg). Store over 4A molecular sieves.
3楼2006-10-17 23:45:45
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yibaigood

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多谢各位的帮助

多谢各位的帮助
4楼2006-10-18 16:40:47
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