Abstract
#1. Efficient columns have been constructed for the
fractional distillation of bases at atmospheric
pressure and under precisely controlled vacuum.
These include the following -
a. 14 -Plate vacuum column (Eyelet Packing) -
b. 40 -Plate column (Penske Helices)
c. 100 -Plate vacuum column (I.C.I.gauze rings)
d. 14- mm. column (I.C.I. gauze rings)
Column a. was subsequently converted to 30-
Plates by re- packing with I.C.I. gauze rings.
Plate efficiency tests were carried out on
columns a. and 'o. and estimates made of the
efficiency of column c.
A simple type of rotary fractional extraction
apparatus has also been constructed.
#2. A typical sample of "Basic Tar" from Pumpherston
Oil Refinery was examined and found to contain so
40 per cent of volatile bases boiling up to 310°C
at atmospheric pressure.
210 litres of "Basic Tar" were distilled under
vacuum in a 16 -litre pot -still and 25 per cent
(53 litres) of bases boiling up to 190°C at 20 mm.
Hg. recovered. The bases were found to consist substantial
of tertiary heterocyclic nitrogen compounds, the
lower boiling ranges were mainly simple homologues
of pyridine with methyl side chains. Quinolines
are believed to be present in the higher ranges
and more complex compounds are also thought to be
present.
#3. The bases were subjected to a series of systematic
fractional distillations and ultimately bases
boiling up to 210°C at atmospheric pressure were
fractionated in a column of 100-theoretical
plates.
#4. Three ranges have been examined by chemical
methods. These are Range 1, 169.9-171°C /760 mm.Hg
Range 2, 186.1-188°C/760mm.Hg. and Range 3,
134.5-134.6°C/100mm.Hg.
The following compounds were identified,
3:5-lutidine; 2:3:5-collidine; 2:4:5 -collidine;
2:4:6- collidine and 2:3:4:6- parvoline. Several
compounds were isolated as crystalline
derivatives, the identities of which have not
been established. Two oily picrates were
obtained, the bases regenerated from one of which
had an unusually high refractive index and gave no
crystalline derivatives.
#5. Infra red absorption spectrograms have been
obtained from several of the compounds isolated
and these favour the proposed structures.
#6. The dissociation constants of a series of pyridine
and quinoline bases have been determined and
discussed.
#7. A survey has been made of the literature dealing
with separation methods and this has been
included as an appendix.
