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重结晶技术(Recrystallization technique)
重结晶技术(Recrystallization technique)
Principle and experience of solvent selection
1. Common solvents: DMF, chlorobenzene, xylene, toluene, acetonitrile, ethanol, THF, chloroform, ethyl acetate, cyclohexane, butanone, acetone, petroleum ether.
2, the commonly used solvent: DMSO, six methylphosphoramide, N- methyl pyrrolidone, benzene, cyclohexanone, butanone, cyclohexanone, chlorobenzene, pyridine, two acetic acid, two oxygen ring six, ethylene glycol monomethyl ether, ethyl ether, ethyl chloride, 1,2- two octane.
3. A good solvent treats crystalline substances near the boiling point and has a high solubility at low temperatures. DMF, benzene, two oxygen, six ring and cyclohexane are near freezing point at low temperature and have poor solubility. They are ideal solvents. Acetonitrile, chlorobenzene, xylene, toluene, butanone and ethanol are also ideal solvents.
4. The boiling point of the solvent is preferably 50 degrees lower than the melting point of the crystalline substance. Otherwise prone to solute liquefaction stratification.
4, the higher the boiling point of solvent, boiling, the stronger the solubility, for high melting point substances, it is best to choose high boiling solvent.
5, containing hydroxyl, amino, and melting point is not too high, as far as possible not to select oxygen containing solvents. Because the solute and solvent form intermolecular hydrogen bonds, it is difficult to precipitate.
6, containing oxygen, nitrogen substances, as far as possible do not choose alcohol as a solvent, the reasons for ibid.
7, solute and solvent polarity do not differ greatly. Water formic acid methanol acetic acid ethanol isopropyl alcohol acetonitrile DMSODMF acetone HMPACH2Cl2 pyridine chloroform chlorobenzene THF two oxygen six ring ether benzene toluene CCl4 octane cyclohexane petroleum ether.
About recrystallization
Crystallization and recrystallization knowledge sets crystallization in the operation of crystalline and recrystallization purifi
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