Ik ben op zoek naar een voorschrift om een ionische vloeistof te synthetiseren voor een project op school. Nu heb ik al gekeken op http://www.orgsyn.org/, maar vind hier alleen een voorschrift om 1-butyl-3-methylimidazolium tetrafluorboraat te synthetiseren, maar hierbij moet 48 uur gerefluxt worden wat niet mogelijk is bij een schoolproject.
Heb google ook geprobeerd, maar geen succes. En orgsyn is eigenlijk de enige database die ik ken om op te zoeken.
Weet iemand waar ik voorschriften voor ionische vloeistoffen kan vinden? Ik ben echt heel dringend op zoek en kan wel wat tips gebruiken of misschien namen van ionische vloeistoffen die misschien wel te vinden zijn op orgsyn, maar wat ik tot nu toe aan ionische vloeistoffen ben tegengekomen, kon ik niet vinden op orgsyn.
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Ionische vloeistoffen
Moderator: ArcherBarry
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- Berichten: 62
Ionische vloeistoffen
Two atoms are walking down the street. One atom says to the other atom, ''I think I have lose an electron!'' The other atom responds, ''Are you sure?'' The first atom replies, ''I'm positive.''
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- Berichten: 6.853
Re: Ionische vloeistoffen
Ionische vloeistoffen zijn nog niet eeuwenoud, ik kan me voorstellen dat daar nog behoorlijk wat nieuwe literatuur op nageslagen moet worden. Ik denk dat je meer succes kunt hebben door direct te zoeken in de wetenschappelijke literatuur via http://scholar.google.com/
Ik zie dan bijvoorbeeld http://pubs.acs.org/....1021/cr980032t ; helaas kan ik niet verder kijken zonder het artikel te kopen....
Of je erg eenvoudige recepten zult vinden weet ik niet!
Ik zie dan bijvoorbeeld http://pubs.acs.org/....1021/cr980032t ; helaas kan ik niet verder kijken zonder het artikel te kopen....
Of je erg eenvoudige recepten zult vinden weet ik niet!
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- Berichten: 49
Re: Ionische vloeistoffen
Op school heb ik een ionic liquid gesynthetiseerd, de quote beschrijft de methode. Ik vond de synthese vrij eenvoudig. Je kan chlorohexane ook vervangen door bromohexane (let wel op dat het gewicht dan veranderd).
The reaction is performed in a 250-mL 1-neck round-bottom flask, fitted with a reflux condenser. The mixture of 0.21 mol (17.24 g) 1-methylimidazole and 0.21 mol (25.33 g) 1-chlorohexane is allowed to stir for 3 h and (100 °C), afterwards cooled down to room-temperature. The work-up procedure is carried out by dissolving the crude reaction mixture in water (20 mL), followed by an extraction of the remaining 1-methyl-imidazole with diethyl ether (3x25 mL). The yield is determined after removal of all volatiles in vacuo (rotary evaporator, water bath T = 80 °C, t = 1.5 h, p = 10 mbar). Because of a small amount of remaining diethyl ether, do not start evaporating at a pressure lower than 600 mbar!
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- Berichten: 49
Re: Ionische vloeistoffen
Een mogelijk ander voorschrift dat je kan gebruiken:
1-butyl-3-methylimidazolium hexafluorophosphate, [C4-mim]PF6.
Place 1.0 mL of water in a 25-mL round-bottom flask, followed by a boiling chip, 1.0 mL of 1-methylimidazole, and 1.35 mL of 1-bromobutane (use the marked pipette to measure both 1-methylimidazole and 1-bromobutane). Reflux for 1.5 hours, swirl gently a few times during this period (don’t remove the flask from the alumina block); by that time a homogeneous solution will be obtained (no oily appearance). Allow the reaction mixture to cool to room temperature, and add 10 mL of distilled water.
Remark: if you would like to change the anion to a different ion than PF6-, you should skip the following part and go to part 2 of the synthetic procedure.
1-butyl-3-methylimidazolium hexafluorophosphate, [C4-mim]PF6.
Add 2.3 g of KPF6 (gently break the chunks of KPF6, if any, with a glass rod) and swirl the resulting mixture for 10-15 min. Two clear phases should appear. Transfer the whole mixture into a 125-mL separatory funnel. Wash the 25-mL round-bottom flask with 25 mL of CH2Cl2, and add it into the separatory funnel. Perform the extraction (don't forget to vent!). Drain the dichloromethane layer into a 125-mL Erlenmeyer flask, and wash to extract the aqueous layer with another 10 mL portion of fresh CH2Cl2. Combine the organic layers; dry with MgSO4 and gravity filter into a 25-mL round bottom flask (wash and dry the round bottom flask beforehand). Use the rotary evaporator to distill CH2Cl2 out. While the distillation flask is still warm, transfer the ionic liquid into a small, pre-weighed test tube with a pipette. Determine the remaining water content by Karl-Fischer titration and the purity by IR and HPLC.
Synthesis of ionic liquids (part 2)
[C4-mim]NTf2:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in water (1.0 mL) and an aqueous solution (1 g/mL) of LiNTf2 (0.66 g, 2.29 mmol) was added. Formation of a biphasic system was noted upon swirling. The resulting biphasic mixture was transferred into a separatory funnel, and extracted with two portions of CH2Cl2 (25 mL and 10 mL). The organic fractions were combined, dried (MgSO4), and the volatiles were distilled out to yield [C4-mim]NTf2 (0.89 g, 93 % yield) as a pale liquid.
[C4-mim]BPh4:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in water (5.0 mL) and NaBPh4 (0.78 g, 2.29 mmol) was added. The mixture was swirled or shaken for 10-15 minutes, after which it was gravity filtered, and the solid was washed with water (3 x 25 mL). The solid was dissolved in CH2Cl2 (20 mL) and dried with MgSO4, filtered, followed by the removal of CH2Cl2 to afford [C4-mim]BPh4 (0.84 g, 80% yield) as a white solid (m.p. 124°C).
[C4-mim]NO3:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in ethanol (1.0 mL). AgNO3 (0.39 g, 2.29 mmol) was added, and the mixture was swirled and shaken for 5 min. The mixture was gravity filtered, and methanol was removed by distillation to yield [C4-mim]NO3 (0.39 g, 85 % yield) as a pale liquid.
1-butyl-3-methylimidazolium hexafluorophosphate, [C4-mim]PF6.
Place 1.0 mL of water in a 25-mL round-bottom flask, followed by a boiling chip, 1.0 mL of 1-methylimidazole, and 1.35 mL of 1-bromobutane (use the marked pipette to measure both 1-methylimidazole and 1-bromobutane). Reflux for 1.5 hours, swirl gently a few times during this period (don’t remove the flask from the alumina block); by that time a homogeneous solution will be obtained (no oily appearance). Allow the reaction mixture to cool to room temperature, and add 10 mL of distilled water.
Remark: if you would like to change the anion to a different ion than PF6-, you should skip the following part and go to part 2 of the synthetic procedure.
1-butyl-3-methylimidazolium hexafluorophosphate, [C4-mim]PF6.
Add 2.3 g of KPF6 (gently break the chunks of KPF6, if any, with a glass rod) and swirl the resulting mixture for 10-15 min. Two clear phases should appear. Transfer the whole mixture into a 125-mL separatory funnel. Wash the 25-mL round-bottom flask with 25 mL of CH2Cl2, and add it into the separatory funnel. Perform the extraction (don't forget to vent!). Drain the dichloromethane layer into a 125-mL Erlenmeyer flask, and wash to extract the aqueous layer with another 10 mL portion of fresh CH2Cl2. Combine the organic layers; dry with MgSO4 and gravity filter into a 25-mL round bottom flask (wash and dry the round bottom flask beforehand). Use the rotary evaporator to distill CH2Cl2 out. While the distillation flask is still warm, transfer the ionic liquid into a small, pre-weighed test tube with a pipette. Determine the remaining water content by Karl-Fischer titration and the purity by IR and HPLC.
Synthesis of ionic liquids (part 2)
[C4-mim]NTf2:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in water (1.0 mL) and an aqueous solution (1 g/mL) of LiNTf2 (0.66 g, 2.29 mmol) was added. Formation of a biphasic system was noted upon swirling. The resulting biphasic mixture was transferred into a separatory funnel, and extracted with two portions of CH2Cl2 (25 mL and 10 mL). The organic fractions were combined, dried (MgSO4), and the volatiles were distilled out to yield [C4-mim]NTf2 (0.89 g, 93 % yield) as a pale liquid.
[C4-mim]BPh4:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in water (5.0 mL) and NaBPh4 (0.78 g, 2.29 mmol) was added. The mixture was swirled or shaken for 10-15 minutes, after which it was gravity filtered, and the solid was washed with water (3 x 25 mL). The solid was dissolved in CH2Cl2 (20 mL) and dried with MgSO4, filtered, followed by the removal of CH2Cl2 to afford [C4-mim]BPh4 (0.84 g, 80% yield) as a white solid (m.p. 124°C).
[C4-mim]NO3:
[C4-mim]Br (0.50 g, 2.29 mmol) was dissolved in ethanol (1.0 mL). AgNO3 (0.39 g, 2.29 mmol) was added, and the mixture was swirled and shaken for 5 min. The mixture was gravity filtered, and methanol was removed by distillation to yield [C4-mim]NO3 (0.39 g, 85 % yield) as a pale liquid.
