Cooley's Cyclopædia of Practical Receipts and Collateral Information in the Arts, Manufactures, Professions, and Trades..., Sixth Edition, Volume ICooley, Arnold James
Science
Cooley's Cyclopædia of Practical Receipts and Collateral Information in the Arts, Manufactures, Professions, and Trades..., Sixth Edition, Volume I
Cooley, Arnold James
Formulas, recipes, etc.; Industrial arts -- Dictionaries; Technology -- Dictionaries
3. (M. Mollerat’s process——without distillation.) Pure commercial acetate
of soda, in coarse powder, is placed in a hard glazed stoneware or glass
pan or receiver set in a cool situation, and 35% or 36% of concentrated
sulphuric acid, of the sp. gr. 1·843, added, in such a manner that the
acid may flow under the powder, and little heat be generated by the
operation; the whole is then allowed to remain in contact (covered) for
some hours, when crystalline grains of sulphate of soda are found covering
the bottom and sides of the vessel, and hydrated acetic acid, partly
liquid and partly in crystals, the upper portion. The temperature being
now slightly raised to a point just sufficient to cause the liquefaction
of the crystals of acetic acid (_i.e._, to from 62° to 65° Fahr.), the
fluid is poured off, and a very small quantity of pure acetate of lime
added to it gradually, until it ceases to yield any trace of free
sulphuric acid on evaporation. After sufficient repose it is carefully
decanted for use. An excellent commercial strong acetic acid is thus
obtained, without distillation, owing to the insolubility of sulphate of
soda in acetic acid; and from which glacial acid may be procured by
refrigeration. If, however, the process be badly managed, or the
proportions of the ingredients be not carefully observed, the product will
be contaminated with either a little sulphuric acid or saline matter. It
is also important to the success of this process that it be performed in a
cool apartment, and in well-cooled vessels. Perfectly pure acetic acid may
easily be obtained by rectification from this acid. The above plan of
superseding a troublesome distillation is one of the greatest improvements
yet introduced into the manufacture of acetic acid.
4. (Liebig’s process.) Pure acetate of soda, thoroughly dried and finely
powdered, 3 parts, is placed in a capacious retort, and pure concentrated
sulphuric acid, 9·7 parts, poured over it through the tubulature. One
eighth of the acetic acid passes over by the heat developed by the
reaction of the ingredients. The heat of a sand bath is next applied and
continued until the contents of the retort become quite liquid. The
distillate, carefully rectified, yields two parts of pure acid, containing
only 20 per cent. of water. On exposing the latter portion which comes
over in a closed vessel to a temperature below 40° Fahr., crystals of
hydrated acetic acid are deposited. The weaker, or liquid portion, being
poured off, the crystals are again melted and re-crystallised by cooling.
The crystals of the last operation, separated from the liquid, and
carefully drained in a cool and closed vessel, are perfectly pure hydrated
acetic acid.
_Obs._ The above is an excellent process for obtaining a chemically pure
acid. The excess of sulphuric acid left from the process may be recovered
by distillation; or the whole residuum may be employed in a second
distillation with fresh acetate.
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