IMPROVEMENTS IN THE MANUFACTURE OF RESINS AND RESINOUS SUBSTANCES, AND IN THE APPARATUS EMPLOYED THEREIN, PARTS OF SUCH IMPROVEMENTS BEING ALSO APPLICABLE TO THE REFINING OF COAL, PETROLEUM, AND BONE OILS, AND ALSO' PARAFFIN AND ANALOGOUS ACIDS AND HYDROCARBONS
Year: 1864

page_text: LETTERS PATENT to John Ives Vaughan, of Appleton-in-Widnes, in the
County of Lancaster, Chemist, for the Invention of "IMPROVEMENTS
IN THE MANUFACTURE OF RESINS AND RESINOUS SUBSTANCES, AND IN THE
APPARATUS EMPLOYED THEREIN, PARTS OF SUCH IMPROVEMENTS BEING ALSO
APPLICABLE TO THE REFINING OF COAL, PETROLEUM, AND BONE OILS, AND ALSO'
PARAFFIN AND ANALOGOUS ACIDS AND HYDROCARBONS,'
Sealed the 21st March 1865, and dated the 11th October 1864.
PROVISIONAL SPECIFICATION left by the said John Ives Vaughan at,
the Office of the Commissioners of Patents, with his Petition, on the
11th October 1864.
•
I, JOHN IVES VAUGHAN,of Appleton-in-Widnes,in the County of Lancaster,
Chemist, do hereby declare the nature of the said Invention for "IMPROVEMENTS
IN THE MANUFACTURE OF RESINS AND RESINOUS SUBSTANCES, AND IN THE APPARATUS
EMPLOYED THEREIN, PARTS OF SUCH IMPROVEMENTS BEING ALSO APPLICABLE TO THE
REFINING OF COAL, PETROLEUM, AND BONE OILS, AND ALSO PARAFFIN AND ANALOGOUS
ACIDS AND HYDROCARBONS," to be as follows:-
This Invention consists in a continuous process of separating or distilling
the spirit from the crude turpentine and refining the residual resin by dis-
017

page_text: tillation without the necessity of cooling or packing in the interval between
the operations, as hitherto practised; and also in the arrangement of a con-
tinuous distillation by the use of a still or distilling column, whereby the
steam of any required temperature is made to enter a compartment (which
may also be made to serve as a temporary receiver for the residual products)
and passing upwards into another vessel is then compelled, by a bonnet on the
exit pipe or other similar or analogous means, to pass through the material
contained therein, carrying with it therefrom a certain portion of the material
in a volatilized state to the compartment above, prior to its passing to the
condensers to be condensed and fitted for the rket. A series of these
columns may be worked in combination with or without separate condensers
to each column. The apparatus is to be fed by a continuous supply to an
upper compartment, the lower ones being supplied therefrom by a dropping
pipe after the charge has reached the level of the top of the pipe. By this
means the material is kept in the several compartments at an uniform level,
and after the working has been continued a short time the quality of the
material contained will be also uniform and regular in each particular vessel
throughout the working, provided that the supply be properly regulated to the
exhaustion of the substance operated on by its volatilization and withdrawal
of the residual products.
The preceding description will be more clearly understood by reference
to the accompanying Drawing.
A is an inlet pipe to convey steam of any required temperature necessary
to conduct the distillation of the material placed in the vessels connected
therewith; B is the first chamber into which the steam enters, which chamber
may also serve as a receiver for the residual products during the distillation;
C is a pipe or way in the bottom of the chamber above through which the
steam passes to the aperture D, and thence under the hood or bonnet Ethe
periphery of which is serrated at F, or pierced with holes as at G, for the
purpose of dividing the steam into small streams or jets as it rises through
the substance under treatment. This action is repeated in each superior
vessel H, H, H; I is a lute box to form a joint with the pipe K, leading the
vapours arising from the process.to the condensers; L is the inlet pipe for the
supply of material to be distilled; M and M* are dropping pipes, either form
of which may be adopted for the purpose of conveying the contents of the
superior vessel (when they shall exceed the height of the stand pipe) to the
next below; N is a pipe by which the residual products can be drawn off
when convenient or when sufficiently exhausted; O are also openings for

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said John Ives Vaughan in the Great Seal Patent Office on the
10th April 1865.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JOHN
IVES VAUGHAN, formerly of Appleton-in-Widnes, in the County of Lancaster,
but now of No. 4, Brabant Court, Philpot Lane, in the City of London,
Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Eleventh day of October, in the year of our Lord
One thousand eight hundred and sixty-four; in the twenty-eighth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said John Ives Vaughan, Her special licence, that I, the said John Ives.
Vaughan, my executors, administrators, and assigns, or such others as I, the
said Jolin Ives Vaughan, my executors, administrators, and assigns, should at
any time agree with, and no others, from time to time and at all times there-
after 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 "IMPROVE-
MENTS IN THE MANUFACTURE OF RESINS AND RESINOUS SUBSTANCES, AND IN THE
APPARATUS EMPLOYED THEREIN, PARTS OF SUCH IMPROVEMENTS BEING ALSO APPLI-
CABLE TO THE REFINING OF COAL. PETROLEUM, AND BONE OILS, AND ALSO PARAFFIN
AND ANALAGOUS ACIDS AND HYDROCARBONS," upon, the condition (amongst others)
that I, the said John Ives Vaughan, my executors or administrators, by an
instrument in writing under.my, or their, or one of their hands and seals,
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.
J
NOW KNOW YE, that I, the said John Ives Vaughan, do hereby declare
the nature of my said Invention, and in what manuer the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, reference being had to the Drawings hereunto annexed, and to the
figures and letters marked thereon, that is to say:

page_text: The first part of my said Invention relates to an improvement in the
manufacture of or mode of obtaining products from resinous substances,.and
consists in carrying on continuously the process of separating the spirit from
the heavier substances contained in the crude turpentine or similar balsams:
and refining the residual resin by distillation without cooling or packing in
the interval between the operations.
The mode of effecting the separation of the turpentine or spirituous olls
from the crude substance is not material in this part of my Invention, but
may be accomplished either by the use of free steam or superheated steam, or
by boiling in a still containing water in accordance with the method hitherto
adopted for the drawing or distilling turpentine. The residuum or resin from
the material under treatment, after the spirit and light oils have been
extracted, is to be run into other apparatus for the purpose of refining the
the same by distillation.
The form of apparatus or mode of refining the residual resin, in the first
part of my said Invention is not of moment or importance, the improvement
consisting in the economy of heat and labour by using the material already
in a heated state, and also in the opportunity afforded thereby to pre-
vent the access of air to the material under treatment, the quality of the
articles being rapidly deteriorated, when in a heated state, by the action of
oxygen.
:
The second part of my said Invention consists in the arrangement or con-
struction and working of apparatus for the purpose of distillation, affording
thereby a means of supplying the crude substance in a continuous stream,and
obtaining therefrom a continuous flow of the volatilized or distilled product
and residuum therefrom, which may be intermittent at the will of the
operator, and in accordance with the requirements of the article under treat-
ment. The apparatus also economizes in a very high degree those distilling
or subliming agents, such as steain or gases of various temperatures which
have hitherto been employed to distil, sublime, or volatilize resinous, fatty, 'or
mineral acids or hydrocarbons.
1 ...
In order that my said Invention may be more fully understood, I will now
describe the apparatus by which the distillation is conducted."
In the Drawings hereunto annexed is shewn a still or distilling head or
column, Figure 1 being an elevation, and Figure 2 a section of the same.
A ie an inlet pipe for the admission of steam or gases of the required
temperature, to be governed in the usual manner by a stop-cock or suitable
valve; B is the first chamber into which the steam, gas, or vapour enters,

page_text: and which chamber may also serve as a receiver for the residual products
during the distillation, which may be thence continuously or occasionally run
off as required. C is a pipe or way to the chamber above, through which the
steam passes, and thence under D, the deflecting hood or. bonnet, the lower
flange of which, E, may be pierced with holes or serrated, as shewn in the
first or lower hood for the purpose of dividing the vapours.into sinȧll streams
or jets so as to be more effective in action in rising through the substance or
substances under treatment; or upon or in place of the deflecting hood.a
series of perforated plates or sieves may be placed under the fluid, that both
the steam or vapour may be minutely divided, and also that an electrical
action may be thereby set up, which I believe materially assists the distil-
lation. This action is repeated in each superposed vessel or chamber F, F*,
G, H, I. J is a lute box to form a joint with the issue pipe K, which leads
the vapours to the condenser; any other usual form of joint may be substi-
tuted for this arrangement. L is the inlet pipe for the supply of the material
to be distilled. M is the dropping pipe fitted internally for the purpose of
conveying, the superfluous contents of the superposed vessel (when they
exceed the height of the stand pipe) to the next beneath. Over the top of
the dropping pipe; M, and leaving a space between the two, it may be
necessary to place a cap.of considerably larger internal diameter than the
external diameter of the pipe M, having a small hole in the top to prevent
any syphoning action when the steam may be shut off; this cap should reach
nearly to the top of the flange of the bonnet, so. that the material shall run
from below the surface into the vessel below, as the higher vessels contain the
lighter substances which might rise to the surface of the material in the
lower vessels into which it flows, notwithstanding the ebullition caused by
the ascending steam. M, Figure 1, is another form of dropping pipe fitted
externally, which may be used in the same manner.as the last-mentioned;
thicse pipes must be fitted so that the charge shall not be carried upwards by
the bubbling of the steam near its base. In this plan a stop-cock may be
inserted in the dropping pipe that the contents of any lower vessel may be
run off while working. In M, Figure 1, this arrangement may be modified
by constructing a bend dipping below the surface of the fluid, having a
small hole in its apex; N is a pipe by which the residual products may be
drawn off continuously or occasionally as required, or an inverted syphon may
be fitted thereto that the residuum may run off continuously and automatically
without the escape of, steam or vapour. O are holes tapped for the
insertion of pipes or stop-cocks, to draw off the whole of the charge when

page_text: necessary, or for occasionally observing the condition of the contents of the
vessels.
Having thus described the apparatus employed in the second part of my
said Invention, I will now proceed to relate the mode of working the same.
The crude material is supplied. in a liquid. state, or heated to a proper
degree and freed from extraneous matter, or otherwise suitably prepared for
distillation in the usual manner, to one of the chambers, by preference one
of the upper vessels, by a pipe L, filling the compartments attached thereto
to the level of the top of the dropping pipe. M. The excess of the measure-.
ment which may be admitted falls through the dropping pipe M into the
vessel immediately beneath, filling that vessel also, and so on. The steam or
other distilling agent is then admitted bythe pipe A, which pipe may be fitted
to any convenient part of the lower chamber, preferably the lowest, and
thence passing upwards and under the deflecting bonnet D,or by other means
under the material, volatilizes a certain portion of the contents of that
chamber, the vapour from which is carried with the steam again upward
and under the deflecting bonnet D of the next chamber, and passing through
the fluid there contained is partially deposited, and a fresh portion again
taken up and carried forward in like manner, until having passed through all
the vessels it reaches the issue pipe K in a more highly purified state. It
is then ready for condensation and removal in any convenient manner; and
in the case of refined resin, to be cooled rapidly by exposure in thin layers
to prevent crystallization, and to allow any surplus or uncombined aqueous
vapour to escape. When the working is in full train the attendant will be
enabled by observing the amount distilled and the condition of the residuum
running from the pipe N to supply, with ordinary judgment, the exact
amount required to keep the work regular and efficient in all points.
The apparatus may be attached to an ordinary still, which may be heated
by fire heat; in which case the still will constitute and take the part of the
lower vessel of the series in the foregoing arrangement, the steam or other
agent. being likewise admitted either above or beneath the material in the
still or lower vessel.
When it is desirable to retain the constitution of the material as nearly as
possible in its normal state with but little decomposition or atomic change,
the use of steam in considerable amount is necessary and advisable, the
change of substance to a secondary compound of a less specific gravity being
the general effect produced when the matter has been acted upon by dry
external heat. In the distillation of substances which are not only required

page_text: to be separated, but the composition of which is desired to be much changed,
the same arrangement of apparatus may be attached to the still, and the still
heated by fire or dry heat only; the vapour of the material under treatment
passing through the column or upper vessels in like manuer. When it is
found advisable to distil the material to dryness, as in the case of candle tar
or pitch, petroleums, oils, oil foots, and other greases, it may be desirable to
connect more than one primary vessel, still, or retort to the colum, that
the connection between a retort and column may be shut off while the coke
or hard pitch is removed from the lower retort, while another such retort is
at work to supply the column with vapour.
It may, in some cases, also be advisable to admit superheated steam direct
to one or more of the upper vessels, in case the temperature be too rapidly
lowered by volatilization or the admission of the fresh material insufficiently
heated. This plan can be adopted for the continuous fractional distillation of
other analogous substances where a greater number than two products are
obtained by the employment of one set of chambers or column. for cach
product. Each column being supplied by its own particular heat, is
calculated to produce the substance distillable at that temperature in an
uniform manner.
The apparatus in the foregoing arrangements may be superposed or
conjoined in any convenient manner, and when it may appear advisable to
assist the action by fire heat, it may be conducted round the vessels by flues
arranged in the brickwork, but I prefer to enclose the vessels as far as
possible in a non-conducting material, and to depend solely upon the heat
directly applied internally by the means previously described.
It will be perceived that by the process above described, as the material in
the vessels is gradually exhausted of its finer volatile constituents, and
becomes more foul and dense by the removal of the lighter portion, the
remainder will require more heat to distil it. This is provided by the
exhausted charges gradually falling towards the greatest heat supplied to and
contained in the lower vessel. At the same time the heavy and foul contents
of the lower vessels yield but an inferior distillate, hence, in passing upwards
the distillate is purified, deposited, repurified, and passed on. The level in
each vessel being at all times uniform, with ordinary vigilance on the part of
the attendant who manages the supply of the crude material and heating
power, it follows that the distillation will be continuous and the product
uniform in colour, quantity, and quality, a result which, I believe, has not
been hitherto obtained in the distillation of hydrocarbons or fatty vegetable or

page_text: mineral acids. To obtain a constant and regular working, I insert thermo-
meters or pyrometers in convenient parts of the apparatus to indicate to the
attendant the exact temperature employed.
A considerable saving is effected by this mode of treating the before.
mentioned substances, both in labour and material, by reason of the immediate
and consecutive distillation without loss of heat or exposure to atmospheric
influence, thereby securing the most highly purified product as a result,
with a minimum of residuum, and also when operating on paraffin or animal
and vegetable fats I obtain a maximum of solid product having a com-
paratively high melting point.
I may observe that for the successful performance of the operations above
described it is absolutely necessary that the superheating apparatus be of
sufficient power and of good construction, as I am aware that most of the
superlieaters employed in this country for the purposes of distillation are
comparatively far too small and inefficient for the amount of work assigned
to them, and hence the general necessity for the use of additional heat
applied to the still externally.
Having thus fully declared and ascertained the nature of my said Inven-
tion, and also the manner in which it is to be performed, I wish it to be
distinctly understood that. I do not claim the use of any part thereof for the
purpose of the distillation of ethylic alcohol, or analogous substances similarly
soluble in water; nor do I claim the use of superheated steam for the dis-
tillation of resin and resinous substances, or fatty animal or vegetable matters
and hydrocarbons, for all which purposes it has been long since employed;
neither do I in regard to the second part of my said Invention claim the
exact form or size of the apparatus before described, as the same must
necessarily be in some degree varied with the nature of the substances to
be operated upon, but what I consider novel and original, and therefore
claim as constituting my said Invention, are,-
Firstly, the treatment of resins and resinous substances by continued or
connected operations, whereby the spirit is distilled from the crude substances,
and the residual resin volatilized or distilled into a product which becomes
solid at the ordinary temperature of the atmosphere without packing or
cooling the resin between the operations, as herein before substantially set
forth and described, or any mere modifications thereof.
And, secondly, the construction, combination, arrangement, and method of
working of the apparatus for the continued distillation of resin and resinous
substances, coal, petroleum, and bone oils, paraffin, and other analogous acids

page_text: and hydrocarbons, as herein-before substantially set forth and described, or
any mere modifications thereof.
In witness whereof, I, the said John Ives Vaughan, have hereunto set
my hand and seal, this Tenth day of April, in the year of our Lord
One thousand eight hundred and sixty-five.
Witness,
E. P. H. VAUGHAN,
54, Chancery Lane,
JOHN IVES VAUGHAN. (L.S.)
Agent for the Patentee.