AN IMPROVED PROCESS IN THE PRODUCTION OF VOLATILE OIL OF RESIN
Year: 1858

page_text: LETTERS PATENT to Henry Napier, of Hyde Road, Ardwick, in the City
of Manchester and County of Lancaster, Manufacturing Chemist, for
the Invention of "AN IMPROVED PROCESS IN THE PRODUCTION OF VOLATILE
OIL OF RESIN."
Scaled the 23rd July 1858, and dated the 31st March 1858.
PROVISIONAL SPECIFICATION left by the said Henry Napier at the
Office of the Commissioners of Patents, with his Petition, on the
31st March 1858.
I, HENRY NAPIER, of Hyde Road, Ardwick, in the City of Manchester and
County Palatine of Lancaster, Manufacturing Chemist, do hereby declare the
nature of the said Invention for "AN IMPROVED PROCESS IN THE PRODUCTION OF
VOLATILE OIL OF RESIN," to be as follows:-
I take the pinate and sylvate of soda or the colophonate of soda formed
as described below, and put the same into a still such as is used by resin oil
'distillers, or of other convenient form, and apply heat. The still is connected
with a condensing apparatus, and the distillate is condensed and received in
suitable vessels. The heat ranges up to 900° Fahrenheit, and is sufficient to
effect the distinctive distillation of the material. The distillate is a brownish
yellow fluid, consisting of the volatile oil contaminated with a small amount of
tarry matter. By repeated rectifications, which may be conducted in the
ordinary naptha salts, the volatile oil is obtained free from the tarry substance

page_text: as a limpid colourless fluid, fitted for all purposes to which the said volatile
oil is usually applied.
The advantages of this process over the old one (of subjecting resin to a
destructive distillation) are the production of a large amount of valuable oil,
of which only a small per-centage is obtained on the old plan without any
great residuum of little value.
The pinate and sylvate of soda is obtained by putting crude turpentine into
a still, such as turpentine distillers use, and adding to it one-fourth of its
weight of soda ash of commerce dissolved in water.
14
The oil of turpentine is driven off by heat applied to the still, and is
condensed and received in the ordinary way. The residuum in the still after
the whole of the oil of turpentine is expelled, is the pinate and sylvate of soda,
that is, the chemical combination of the pinic and sylvic acids of the crude
turpentine with the alkali employed. If ordinary resin is acted on by the
alkali in proportions similar to those given above, a colophonate of soda is
formed, the pinic acid of the turpentine having been changed in the process
of making the resin into colophonic acid. The yield of volatile oil from this
source is not so great as from the pinate and sylvate of soda, I therefore prefer
to use the latter. Caustic soda or caustic potash or carbonate of potash may
be used instead of soda ash, but I prefer soda ash as being cheaper than the
other alkalies named.
I do not restrict myself to a particular form of apparatus, nor yet to the
precise proportions of ingredients nor degree of heat named, as these may be
varied in some degree without injury to the result of the process. I find the
above proportion of alkali to be amply sufficient to neutralize the acids of the
turpentine or of the resin. If resin is used, then a condensing apparatus is
not required (in the making of the colophonate of soda).
I do not intend in this Specification to claim that portion of the process
which refers to the making of the pinate and sylvate of soda, as that already
forms the subject of a Patent now belonging to me, nor yet do I claim the
making of the colophonate of soda, as that has been practised in soap making.
I claim the improved mode of producing the volatile oil of resin, also known
as "resin naptha," from the substances mentioned above, in the manner above
narrated.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Henry Napier in the Great Seal Patent Office on the
23rd September 1858.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, HENRY
NAPIER, of Hyde Road, Ardwick, in the City of Manchester and County
Palatine of Lancaster, Manufacturing Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Thirty-first day of March, One thousand eight
hundred and fifty-eight, in the twenty-first year of Her reign, did, for
Herself, Her heirs and successors, give and grant unto me, the said Henry
Napier, Her special licence that I, the said Henry Napier, my executors,
administrators, and assigns, or such others as I, the said Henry Napier,
my executors, administrators, and assigns, should at any time agree with,
and no others, from time to time and at all times thereafter during the
term therein expressed, should and lawfully might make, use, exercise, and
vend, within the United Kingdom of Great Britain and Ireland, the Channel
Islands, and Isle of Man, an Invention for "AN IMPROVED PROCESS IN THE
PRODUCTION OF VOLATILE OIL OF RESIN," upon condition (amongst other things)
that I, the said Henry Napier, by an instrument in writing under my hand
and seal, should particularly describe and ascertain the nature of the said
Invention, and in what manner the same was to be performed, and cause
the same to be filed in the Great Seal Patent Office within six calendar
months next and immediately after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Henry Napier, do hereby declare the
nature of my said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, that is to say:-
I take the pinate and sylvate of soda or the colophonate of soda, formed as
described below, and put it into a still such as is used by resin oil distillers, or
of other convenient form, connect the still with a condenser, and apply sufficient
heat to effect the distillation of its contents. The distillate is a brownish
yellow fluid, consisting chiefly of the volatile oil of resin contaminated with a
small quantity of tarry matter. By repeated rectification, which may be
conducted in the ordinary naptha stills, the volatile oil may be obtained free
from its impurities and in the form of a colourless limpid fluid, applicable to
the various purposes for which the volatile oil of resin is required. The other
products of the distillation are water (not in any degree acidulous) and
incondensible gases. The residuum in the still consists of a light coky' mass,

page_text: containing the alkali employed and charcoal. In distilling the above-mentioned
pinate and sylvate or the colophonate of soda, it is desirable to fill the still
to not more than one-fourth of its capacity, so as to render it less liable to
" run foul."
The advantages of this method over the old process of distilling resin consist
in the production of a largely increased per-centage of the "resin naptha" at
the expense of the ordinary fixed oil of resin and other less valuable products.
The pinate, and sylvate of soda is formed by the action of an alkali on crude
turpentine, as follows:-I melt and strain into a still such as is in use by
turpentine distillers as much crude turpentine as I intend to operate upon for
one charge, and add to the mass one-fourth of its weight of soda ash of
commerce (in solution with water); I connect the still with a condenser,
apply heat, and the essential oil of turpentine comes over and is condensed;
and is received in suitable vessels. When the whole of the oil of turpentine is
expelled, which is known by its ceasing to appear along with the condensed
steam, the operation may be considered concluded, the mass in the still being
the pinate and sylvate of soda, that is, the pinic and sylvic acids of the turpen-
tine in chemical combination with the alkali.
Colophonate of soda is formed when ordinary resin of commerce is combined
with soda; similar proportions of alkali may bo used in this case as are given
above, and the condensing apparatus may of course be dispensed with. In the
distillation of crude turpentine to form resin in the usual way, the pinic acid is
decomposed, being changed into colophonic acid, hence the change of terms.
In using soda ash to form the above combinations, care must be observed in
its addition, as a considerable quantity of carbonic acid gas is discharged from
the mass, creating an effervescence and a liability to cause the still to "run
foul." I add the solution of alkali by degrees during the progress of the dis-
tillation at a strength of about thirty degrees of Twaddell's hydrometer, and
thus I obtain sufficient water to give vapour, and also prevent any violent and
extensive effervescence. Other alkalies may be employed to effect the above
purposes, such as carbonate of or caustic potash or caustic soda; but as their
properties are well known and easily adapted by those skilled in the art,
I refrain from entering into a lengthened description of them.
.I do not wish to bind myself to the particular form of apparatus, nor to the
precise proportions of ingredients mentioned, as these may be varied in some
degree without injury to the result of the process, or departure from the
principle of my Invention; neither do I give the strength of the alkaline
solution as to be acted on without variation, for the same obvious reason.
. I do not intend. to claim the manufacture of oil of turpentine by treating

page_text: crude turpentine with alkaline solutions, nor the combination of the said crude
turpentine with an alkali, as that forms the subject of a Patent already
belonging to me; neither do I claim the combination of resin with an alkali,
as that has long been practised by soap makers and others; but what I claim
as my Invention, and desire to secure by Letters Patent, is, the production of
the volatile oil of resin, known also as "resin spirit" or "resin naptha," from
the substances and in the manner substantially as above described.
In witness whereof, I, the said Henry Napier, have heretofore set my
hand and seal, the Twenty-first day of September, in the year of
our Lord One thousand eight hundred and fifty-eight.
HENRY NAPIER. (L.S.)