We are having an initial mixture containing TetraHydro Furan + Isopropyl Acetate + Methanol in the HPLC as 52% + 32% + 16% . We tried to separate this mixture using water as media to separate THF+MeOH which are purely soluble in water and IPAc in the ratio of 4%(and if we maintain temp<20 °C it is <1%) .
We have given two water washings to the mixture separating
1)The first aqueous layer HPLC result(THF 71.4% + IPAc 17.45% + MeOH 6.60%) and
2)The organic layer HPLC result(THF 45.8% + IPAc 52.8% + MeOH 0.34%)
given second water washing
3)The second aqueous layer HPLC result(THF 78.5% + IPAc 18.8% + MeOH 1.6%) and
4)the organic layer HPLC result(THF 36.55% + IPAc 62.3% + MeOH 0.1%)
As we add the methanol in less quantity there is no need to recover the methanol. Is there any method to kill the methanol other than using flakes (or) any other solvent in which only the methanol is miscible so we can separate it from the mixture in the initial stage and send the mixture for column separation?