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Liquid-lquid equilbrium(LLE)data of water-caprolactam-benzene-(NH4)2SO4 system

at 303K were measured for extraction of caprolactam from aqueous ammonium


sulfate solution.The influence of fluid flow rate,pulsation intensity on flooding
velocity and mass transfer was studied for extraction of caprolactam from
ammonium sulfate solution in a laboratory pulsed packed column.The flooding
velocities and overall apparent heght of a transfer unit were given under various
operation conditions.An industrial column developed based on above study is
operated well.The scale-up effect is discussed.

In a process for continuously extracting caprolactam from an aqueous solution,


containing caprolactam and its oligomers, with organic solvents, by introducing the
aqueous solution into the upper part of an extraction zone and organic solvents into
the lower part, and taking off a solution of caprolactam in organic solvents at the
upper end and an aqueous phase containing caprolactam oligomers at the lower
end, the improvement that liquid aromatic hydrocarbons are used and the
extraction is carried out at a pH of from 2.0 to 6.0. The aqueous solution would be
ammonium sulfate solution and the organic solvent is benzene.
The preparation of caprolactam by a Beckmann rearrangement gives a crude
lactam which is purified by extraction with benzene. The resulting benzene/lactam
phase is worked up to give caprolactam. A brown solution, containing ammonium
sulfate, impurities and a small amount of caprolactam, is obtained as the aqueous
phase.

About Caprolactam
Caprolactam is an organic compound which is a lactam of 6-aminohexanoic acid (eaminohexanoic acid, aminocaproic acid).
Caprolactam is produced as clear liquid form and as a crystalline form.
Caprolactam occurs as white, hygroscopic flakes or crystals with a distinctive odour.
Caprolactam is soluble in water, cyclohexane, chlorinated hydrocarbons.

Benzene and Aromatic Solvents

Aromatic compounds such as benzene, toluene and xylene have quadrapole


moments that
tend to have attractive forces on the amide group of caprolactam. These solvents
have
reasonable capacities for caprolactam solubility with benzene having the higher
capacity and
xylene having the lower capacity. The methyl groups on the aromatic ring are
activating electron donating substituents that produce a permanent dipole moment
in the molecule however these groups reduce packing capabilities due to steric
hindrance. Less ability for the molecules to pack more closely reduces the
intermolecular forces. The partition coefficient of caprolactam dissolved in the
aqueous phase versus caprolactam dissolved in the organic phase also follows the
same pattern with benzene having the largest partition coefficient and xylene
having the lowest. Nitrobenzene has an electron withdrawing group which is a
zwitterion that has more attractive forces with caprolactam in comparison to
toluene and xylene, however the functional group also reduces packing abilities;
therefore toluene and xylene do not have the caprolactam solubility capacity of
benzene.