IMPROVEMENTS IN THE MANUFACTURE OF MINERAL OIL AND AMMONIA, PART OF THE SAID IMPROVEMENTS BEING ALSO APPLICABLE TO THE MANUFACTURE OF COAL GAS
Year: 1881

page_text: LETTERS PATENT to William Young, of Seafield House, Lasswade, in the
County of Midlothian, North Britain, for an Invention of "IMPROVEMENTS
IN THE MANUFACTURE OF MINERAL OIL AND AMMONIA, PART OF THE SAID
IMPROVEMENTS BEING ALSO APPLICABLE TO THE MANUFACTURE OF COAL
GAS"
PROVISIONAL SPECIFICATION left by the said William Young at the Office
of the Commissioners of Patents on the 12th April 1881.
WILLIAM YOUNG, of Seafield House, Lasswade, in the County of Midlothian,
North Britain. "IMPROVEMENTS IN THE MANUFACTURE OF MINERAL OIL AND
AMMONIA, PART OF THE SAID IMPROVEMENTS BEING ALSO APPLICABLE TO THE
MANUFACTURE OF COAL GAS."
The first part of this Invention has for its object improvements in the system
of distilling shale or other similar substances for the production of oil and ammonia,
and consists in distilling the shale in such a manner that the oil shall be liberated
and distilled from the shale at a low uniform temperature, and the remaining
nitrogen liberated at a much higher temperature as ammonia. This is accomplished
by first distilling out the oils from the shale at a low temperature in one retort,
and thereafter transferring the residue into a second retort heated to a considerably
higher temperature; or the operation may be conducted in one long retort, so
divided that the shale shall be distilled free of its oil at one end and the distilla-
tion for ammonia completed at the other end, steam being employed for liberating
the ammonia in the hot end.
The second part of this Invention has for its object the rendering of the resulting
oils more easy of refining, and consists in causing the oily vapours during the
process of refining to pass from the still or stills through a second vessel or still or
stills containing soda, lime, or both combined, such soda or lime or soda-lime being
kept heated to a temperature approaching the volatilizing point of the oil under-
going treatment.
A third part of this Invention consists of an arrangement for economizing the
quantity of chemicals, acid, and alkalis required to refine the oil by applying them
to the treatment of the oil in such a manner that the pure strong acid and alkalis
are first used in the nearly finished oil, and as the acid and alkalis become more
and more saturated with impurities they are applied to more and more crude oils.
This object is attained by so arranging the treating vessels that they consist of
alternate agitators and precipitating vessels. The impure oils enter at one end
into the first agitating vessel, and thence alternately from precipitating vessel to
agitating vessel until they leave the last precipitating vessel at the other end, the

page_text: acid or alkalis being made to flow back against the stream of oil from each alternate
precipitating and agitating vessel, removing the impurities from the oil in the
passage, and passing out from the first precipitating vessel saturated with impuri-
ties, the flow of oil and chemicals being regulated by taps, measuring vessels, or
other equivalent mechanical devices.
A fourth part of this Invention consists in the economical separation of the
ammonia from the ammoniacal liquor derived from the destructive distillation of
shale or other similar substances in the manufacture of gas or oil, and in the
application of the ammonia to the purification of gas or the preparation of ammonia
caustic, or salts of ammonia. When the ammonia in the liquors is to be manufac-
tured into sulphate or similar salts of ammonia, a " Coffey" still or some similar
fractionating system of distilling arrangement is employed, in which the liquors
are treated with steam in the usual manner. There is also employed a saturating
vessel, or a vessel in which the acid to form the salt is brought into contact with
the ammonia in the usual well-known way. This chamber is so formed however
that the steam which accompanies the ammoniacal gas is collected and made
available in the following manner-Instead of connecting the "Coffey" still or
other similar arrangement direct to the steam boiler, and introducing the steam
necessary for the liberation of the ammonia direct into the lower or first compart-
ment, the steam is made to draw or force this steam, by means of jets or other
mechanical contrivances, from the saturating vessel back into the bottom or first
chamber of the distilling-vessel, the steam being thus used over and over again,
and thus a great economy is effected in the quantity of steam required.
When the ammonia is to be made into caustic ammonia, or used to remove the
impurities from coal gas, a similar fractionating distilling arrangement is employed,
but the process is so conducted that in the upper or terminal fractionating vessels
the sulphuretted hydrogen and carbonic acid and other impurities combined with
the ammonia are liberated. This is accomplished by heating the liquors to be
therein treated, and allowing only such a quantity of steam to pass through them
as will drive the impurities out, combined with small quantities of ammonia. This
ammonia is recovered as sulphate by passing through a vessel containing sulphuric
acid. The sulphur in the sulphuretted hydrogen may also be recovered by passing
through oxide of iron in the usual well known manner. The ammoniacal liquors,
after being denuded of impurities in the upper and terminal vessels of the distilling
arrangement, are subjected to the further action of steam to liberate the ammonia
in the caustic state, which can be used for the purification of coal gas by passing it
in the vapourous state, either combined with the water vapour or dry, into the
condenser or before entering the scrubbers; or the coal gas to be purified may be
passed through the hot ammoniacal liquors after they have (as described) been
denuded of the impurities. The gas thus carries away the caustic ammonia, which
on cooling absorbs the impurities and is precipitated with the accompanying water
vapours, or removed from the gas in the scrubbers with water in the usual well
known manner.
The ammonia so condensed may be again réturned to the distilling arrangement
and again used for the same purpose time after time.
When it is desired to prepare caustic ammonia, it is necessary to employ a
supplementary vessel, in which there are placed chemicals, such as caustic lime,
soda, and oxide of iron or manganese, to absorb the carbonic acid and sulphuretted
compounds.
In the manufacture of sulphate from the ammoniacal liquors, should the presence
of gases liberated in the saturating vessel interfere with the proper working and
circulation of the steam alternately from still to saturater, and from saturater to
still, the arrangement described for the preparation of caustic ammonia may be
employed.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said William Young in the Great Seal Patent Office on the 12th October
1881.
WILLIAM YOUNG, of Seafield House, Lasswade, in the County of Midlothian,
North Britain. "IMPROVEMENTS IN THE MANUFACTURE OF MINERAL OIL AND
AMMONIA, PART OF THE SAID IMPROVEMENTS BEING ALSO APPLICABLE TO THE
MANUFACTURE OF COAL GAS."
The first part of my Invention has for its object improvements in the system of
distilling shale or other similar substances for the production of oil and ammonia,
and consists in distilling the shale in such a manner that the oil shall be liberated
and distilled from the shale at a low uniform temperature, and the remaining
nitrogen liberated at a much higher temperature as ammonia. This is accomplished
by first distilling out the oils from the shale at a low temperature in one retort, and
thereafter transferring the residue into a second retort, heated to a considerably
higher temperature; or the operation may be conducted in one long retort, so
divided that the shale shall be distilled free of its oil at one end, and the distillation
for ammonia completed at the other end, steam being employed for liberating the
ammonia in the hot end.
The second part of this Invention has for its object the rendering of the resulting
oils more easy of refining, and consists in causing the oily vapours during the
process of refining to pass from the still or stills through a second vessel or still or
stills containing soda, lime, or both combined, such soda or lime, or soda-lime, being
kept heated to a temperature of or approaching the volatilizing point of the oil
undergoing treatment.
A third part of this Invention consists of an arrangement for economizing the
quantity of chemicals, acids, and alkalis required to refine the oil, by applying them.
to the treatment of the oil in such a manner that the pure strong acids and alkalis
are first used in acting upon the nearly finished oil; and as the acids and alkalis
become more and more saturated with impurities they are applied to more and
more crude oils. This object is attained by so arranging the treating vessels that
they consist of alternate agitators and precipitating vessels. The impure oils enter
at one end into the first agitating vessel, and thence pass alternately from
precipitating vessel to agitating vessel until they leave the last precipitating vessel
at the other end, the acids or alkalis being made to flow back against the stream
of oil passing from each alternate precipitating and agitating vessel, removing the
impurities from the oil in the passage, and passing out from the first precipitating
vessel saturated with impurities, the flow of oil and chemicals being regulated by
taps, measuring vessels, or other equivalent mechanical devices.
A fourth part of this Invention consists in the economical separation of the
ammonia from the ammoniacal liquor derived from the destructive distillation of
shale or other similar substances in the manufacture of gas or oil, and in the
application of the ammonia to the purification of gas or the preparation of ammonia
caustic or salts of ammonia. When the ammonia in the liquors is to be manu-
factured into sulphate or similar salts of ammonia, a "Coffey" still, or some similar
fractionating system of distilling arrangement is employed, in which the liquors
are treated with steam in the usual manner. There is also employed a saturating
vessel, or a vessel in which the acid to form the salt is brought into contact with
the ammonia in the usual well known way. This chamber is so formed however
that the steam which accompanies the ammoniacal gas is collected and made
available in the following manner:-Instead of connecting the "Coffey" still or
other similar arrangement direct to the steam boiler, and introducing the steam

page_text: necessary for the liberation of the ammonia direct into the lower or first com-
partment, the steam from the boiler is made to draw or force this collected steam
by means of jets or other mechanical contrivances from the saturating vessel back
into the bottom or first chamber of the distilling-vessel, the steam being thus used
over and over again, and thus a great economy is effected in the quantity of steam
required.
When the ammonia is to be used to remove the impurities from coal gas a similar
fractionating distilling arrangement is employed, but the process is so conducted
that in the upper or terminal fractionating vessels the sulphurretted hydrogen and
· carbonic acid and other impurities combined with the ammonia are liberated. This
is accomplished by slightly heating the liquors to be therein treated, and allowing
only such a quantity of steam to pass through them as will drive out the impurities
combined with small quantities of ammonia. This ammonia is recovered as
sulphate by passing through a vessel containing sulphuric acid. The sulphur in
the sulphuretted hydrogen may also be recovered by passing through oxide of iron
in the usual well known manner. The ammoniacal liquors, after being denuded of
impurities in the upper and terminal vessels of the distilling arrangement, are
subjected to the further action of steam to liberate the ammonia in the caustic
state, which can be used for the purification of coal gas by passing it in the
vapourous state, either combined with the water vapour or dry into the condenser,
or before entering the scrubbers; or the coal gas to be purified may be passed
through the hot ammoniacal liquors after they have (as described) been denuded of
the impurities. The gas thus carries away the caustic ammonia, which on cooling
absorbs the impurities, and is precipitated with the accompanying water vapours,
or removed from the gas in the scrubbers with water, in the usual well-known
manner.
The ammonia so condensed is preferably again returned to the distilling
arrangement, and again used for the same purpose time after time.
In the manufacture or sulphate from the ammoniacal liquors, should the
presence
of gases liberated in the saturating vessel interfere with the proper working and
circulation of the steam, alternately from still to saturater, and from saturater to
still, the arrangement described for the preparation of caustic ammonia may be
employed.
And in order that my said Invention may be properly understood I now proceed
more particularly to set forth the system, mode, or manner in or under which the
same is or may be used or practically carried into effect, reference being had to
the accompanying Drawings, and to the letters and figures marked thereon, that is
to say :-
Figure is a transverse section of a bench of retorts, shewing two of the best
forms of retorts with which I am acquainted for carrying out the hereinbefore
described first part of my Invention. Figures 2 and 3 are horizontal sections of a
pair of retorts, the said sections being respectively taken on the lines 1, 2, and 3, 4,
Figure 1 for shewing the arrangement of the flues, the said flues and the parts
which lie on the lines of section only being shewn in these Figures. The same
letters are employed to denote the same parts of the apparatus in these Figures,
and the retorts of the two different forms are shewn in one bench only for the
purpose of explaining this part of my Invention. In practice it would be pre-
ferable to have all the retorts of one form or the other. The mode of heating as
shewn is by the use of the fixed carbon in the coke or residue from the shale, and
by means of devices similar to those described in Patent No. 1578, granted to me
as of the 17th April, A.D. 1880, but any other convenient kind of fuel or mode of
heating may be employed.
The retorts A, A¹, A, A', B, B1, B, B¹, are very long retorts, or consist of two
retorts, one (A or B) above the other (A¹ or B¹), and communicating therewith, and
they may be arranged as shewn, four in an oven, or in other suitable number, and
surrounded by a brick wall in the usual manner, but the space around the upper
retorts A, B, in which the shale is subjected to a low red heat for the distillation

page_text: of the oil is separated by a mid-partition or division wall C¹ from the space around
the lower retorts A¹, B¹, in which the .shale is subjected to a much higher
temperature, approaching cherry-red heat, for the elimination of the nitrogen in the
form of ammonia. Each retort (A, A¹, or B, B¹) is preferably placed over its own
combustion chamber, into which the shale coke from the retort is dropped and
consumed in heating the next charge. The retorts of the form A, A', have the
outlet D for the oil vapours and ammonia, constructed as shewn in communication
with the interiors of the upper retort A. and lower retort A¹ at their junction. A
sliding valve or damper d is arranged to be slidden inwards to form a division
separating the two retorts A, A', the lower retort A¹, of sufficient capacity to
accommodate the contents of the upper retort A when reduced in volume by having
been deprived of their oil vapours. The outlet D' of the other form of retorts (B, B¹)
is placed at the top of the upper retort B. Both forms of retorts are provided with
an arrangement at the lower end consisting of a circular chamber E furnished with
numerous openings e into the retort, into which chamber steam is introduced by
means of the steam pipe F placed preferably in a coil in the main flue G leading to
chimney-stalk. Both forms of retorts are also provided with suitable openings (a, b)
at top and bottom for the charging of the shale and the discharging of the residue
or coke. The heated products of combustion pass from the combustion chambers H
through the ports h into the lower chamber or oven, and around the lower
retorts (A, B), the said products thence passing through the ports h² in the
partition wall C¹ into the upper chamber oven and around the upper retorts (A, B),
thence by the flues h³ down into the main flue G leading to the chimney stalk.
The ports h² in the partition-wall C₁ are enlarged or diminished by means of a
brick damper h. This has the effect of adjusting the relative temperatures of the
products of combustion around the retorts in the upper and the lower chambers, the
necessary heat being brought up upon the retorts in the usual manner by ineans-of
coal or other fuel. The process of operating with the form of retorts A, A', is as
follows: The door a² on the bottom of the retort is closed and the sliding damper
or door d pushed in to form a division between the retorts A and A¹. The retort A
is then charged with shale and the upper cover or door a closed and the distillation
for oil is allowed to proceed till completion. The sliding door or valve d is then
withdrawn and the shale-coke dropped into the lower retort A¹. The damper d is
then replaced and a fresh charge of shale introduced into the upper retort A and
the upper door a again closed. Steam is now admitted to the lower retort A' by
opening the valve f on the pipe F, the steam then passing into the passage E and
by the openings e into the retort and up through the shale, getting in part
decomposed; the hydrogen passing to the nitrogen and combining with it to form
ammonia, and the oxygen forming carbonic acid and carbonic oxide gas. The
mixed gases, ammonia, and steam pass up and out below the door or damper d to
the outlet pipe, and are passed away along with the oil vapour to the condensers
and treated in the usual way for their condensation and recovery. So soon as the
volatile hydrocarbonaceous matter has been distilled from the shale in the upper
retort A a large quantity of steam is admitted by the valve f into the circular
chamber and through the orifices at and around bottom for the purpose of
preventing the ingress of air to the retort during the process of drawing the
charge. The door a² is then opened and the shale coke dropped from the retort A¹
into the combustion chamber H to apply the heat necessary for the next charge of
shale. The said door a² is again closed and the sliding plate d is withdrawn,
allowing the shale-coke to drop from the retort A into the retort A¹. The plate d
is then replaced and a fresh charge of shale is immediately introduced into the
retort A, the steam being partially checked at the valve f and the distillation
proceeded with as before.
With the second form of retort B, B', the process is slightly different, there
5 being no valve or door d between the retorts B and B'. The retort B¹ must at
first be filled up with shale, coke, or other similar loose carbonaceous matter so as
to support the charge of fresh shale introduced into the upper retort B, and a

page_text: piece of perforated iron or piece of brick or other foreign substance is placed on
top of the said loose carbonaceous matter. So soon as this first charge is distilled
off its volatile oily matters, steam is let into the bottom of the retort by means of
the valve through the passage E and perforations f, as described with regard
to the retorts A, A, and the lower door 62 opened, and the spent coke or other
carbonaceous matter previously charged into the retort B' discharged into the
combustion chamber till the piece of iron, brick, or other foreign matter which
was as before stated placed on the top of the carbonaceous matter is found,
shewing that the charge in the upper chamber B has descended into the lower
chamber B. The lower door 62 is then closed and the steam slightly checked, and
a fresh charge of shale immediately introduced into the upper retort B, the piece
of iron or other foreign matter having been previously placed on the top of the
charge which had descended to the retort B₁. So soon as this second charge of
shale is exhausted of its volatile oily matters the steam is again turned on to the
bottom of the retort a little stronger for the purpose before mentioned, and the
door 62 is opened and the coke discharged from the lower retort B¹ into the com-
bustion chamber H (the ashes from which have been previously removed), the
piece of iron, brick, or other substance indicating when this has been accomplished.
Or instead of iron, brick, or other foreign matter, an iron rod the length of the
upper retort may be passed through a hole in the upper door and allowed to
descend as the retort is discharged, which will at once shew when it is empty. Or
the extent to which the combustion chamber is filled by the spent shale from the
lower retorts may be the means by which to ascertain when the complete discharge
of the said lower retorts has taken place. The bottom door a² is now again closed
and a fresh charge of shale put into the upper retort B. As the outlet from this
form of retort is at the top, the steam, ammonia, and gases from the lower retort
have to pass up and through the shale.
In order to facilitate the removal of any hardened accumulation of shale at the
lower end or outlet of the retorts, the bottom of each retort may be formed as
shewn with regard to the retort B'. The outlet end of the retort is enlarged, as at
ts, so as to leave a space around the lower end of the column of the charge which
enters this outlet end. This space enables the ready insertion of a tool to remove
any hardened accumulation of shale, and allows the contents to be regularly
discharged. Figure 4 is a section of the lower part of the retort B¹ taken upon the
line 5, 6, Figure 1. The outlet end of the retort A¹ is protected from the direct
action of the heat by the brickwork of the arch and by an extension surrounding
its lower end. The outlet end of the retort B₁ is similarly protected by an
extension, and its lowest part protected by the brickwork at g, a flue h³ being
formed in the wall for the passage of the products of combustion to the chamber
surrounding the lower retorts.
Figure 5 is a diagram illustrating an arrangement for carrying out the herein-
before described second part of my Invention. The oil to be subjected to the
alkali is placed in still I, which may be of any convenient form, that shewn
representing an ordinary malleable iron boiler still heated in the usual manner, but
the hot products of combustion from the furnace i after heating the still I are not
allowed, as is usually the case, to pass direct into the flue leading to the chimney-
stalk, but are conveyed by a special flue to a second still J. This still J is the
still into which the caustic soda or soda-lime is placed, and which is thus kept hot
by the spent products of combustion from the furnace of the still I after heating
that still. Should however the heat of these products not prove quite sufficient to
keep this still to the necessary heat the small auxiliary furnace j is provided to
supplement the spent heat. The oil to be subjected to the action of the alkalis or
alkaline earths being placed in the still I, and the caustic soda, lime, or soda-lime
placed on the plate at the lower part of the still J, or being dissolved and run
into the said still, the fire in the furnace i is kindled, which soon brings up the
oil to the boiling. point, the waste heat from the said furnace i at the same time
heating the caustic soda or other alkali in the still J to a similar temperature.

page_text: The oil vapours pass by the pipe k from the still I to underneath the perforated
plate in the still J. These oil vapours in bubbling underneath the said plate j²
and passing up through the perforations therein and amongst the caustic alkali
are brought intimately into contact with the said alkali, which has the effect of
rendering the said oil vapours much more easy of refining, requiring less chemicals
and giving a larger yield of refined products. The oil vapours after having been
subjected to the action of the alkalis or alkaline earths pass through the pipe / to
the condensing tubular coil 7, and are condensed in the usual manner.
This arrangement shews only one treating vessel or still J in which the caustic
alkali is made to act upon the oil vapours, but should the oil not be sufficiently
acted upon by treatment in one such still two or more stills or treating vessels
may be employed, the vapour passing from the first into the second, from that to
the third, and so on till the last, when it is passed to the condensers in the usual
manner.
Instead of using stills a vertical retort or chamber may be employed having a
series of trays on which the soda-lime may be placed. Figure 6 shows such an
arrangement in which an oil still, similar to that marked I in Figure 5, is used,
but connected by the pipe k to a vertical retort or chamber J¹ fitted with a series
of shelves j, j³. This retort or chamber J¹ is provided with doors at top and
bottom for charging and discharging the soda lime or alkali.
The oil vapours
pass from the chamber J¹ by the pipe l at top; or the oil vapours may be admitted
at the upper part of the chamber J' and pass off at the bottom if desired.
outlet for any liquid oil which may condense in the chamber J¹.
* is an
To regulate the temperature in the various vessels it is desirable to employ
thermometers inserted in the oil stills and treating vessels in the usual well known
ways.
Any convenient form of still and treating vessel may be used and the oil still
may be fed up with oil as the oil passes over in vapour, and the process may be
applied, if so desired, at successive stages of refining. Although only one still is
shewn as supplying vapour to one treating still or vessel, yet any convenient
number of oil-stills may be made to distil into one or more treating vessels or stills
containing caustic alkali or alkaline earths, the Invention consisting in subjecting
the oils whilst in the form of vapour to the action of soda lime, or soda-lime in a
vessel or vessels separate from the oil still proper. The soda-bottoms from the
treatment of oils in washing vessels may, with advantage, be used in the still or
stills J in the first treatments or stages of refining.
Figure 7 is a diagram illustrating an apparatus for carrying the third part of
my Invention into effect. The arrangement as shown consists of three agitating
vessels M, M, M, and three precipitating or settling vessels N, N, N, placed
alternately over each other and communicating with each other by the passages q.
Stirring blades m, m, are situated in the three agitating vessels, being attached to
the vertical shaft m² receiving motion of rotation through the bevel gearing c from
any suitable motor. The oil to be acted upon and refined by the chemicals, acid,
or alkali is supplied to the small vessel o, and the acid or alkali to the vessel p
either by any of the well known automatic measuring arrangements, or by hand in
the proper proportions to each other. The oil passes by the pipe of into the
lower agitator M, and the acid passes by the pipe p¹ into the upper agitator M.
In starting the operation the two lower precipitating vessels N, and the two
lower agitating-vessels M, and half of the third agitating vessel M, must be filled
with oil. The stirrer blades m are then set in motion and the acid or alkali and
oil are set flowing into the apparatus. The acid or alkali and oil commingled in
the upper agitating vessel M are carried upwards through the passage q into the
upper precipitating-vessel N, the acid and impurities settling out, and the pure oil
overflowing by the piper into any convenient tank or into the bottom of the second
similar arrangement, to be there treated with other chemicals. The acid or alkali
fouled by the impurities which it has extracted from the oil flows down from the
upper precipitating vessel N by the pipe n, through the syphon-bend n³ (which has

page_text: the effect of preventing the oil from flowing through the same pipe as the chemicals,
and thus ensuring their action on the oils) into the middle agitator M, where it is
at once mingled with the oil by the rotating blades m and carried up through the
passage q into the middle settling vessel N. In this vessel the tars, acid, or alkalis
and impurities quickly precipitate, the oils flowing upwards through the opening q
into the upper agitator M, to be there treated with the purer acid or alkali supplied
to this vessel. The tars not quite saturated with impurities pass from the second
precipitating vessel N by the pipe n³ and syphon n into the lower agitating
vessel M, and are at once commingled with the impure oil entering by the pipe o¹
by means of the stirring blades m. The commingled oil and acid or alkali
saturated with impurities pass up by the passage q into the lower precipitating
vessel N, where the acid or alkali quickly settles out, and is drawn off continuously
or intermittently through the valve on the pipe no, the oils passing upwards through
the passage q into the second agitating vessel M to be treated with the partially
fouled acid or alkali from the upper precipitating vessel. It will thus be seen that
the process is a continuous fractionating one, the acid (or the alkali) flowing down-
ward, and as it becomes more and more saturated with impurities, meeting and
acting upon more and more impure oils; and on the other hand the oil is
continuously flowing upwards, becoming gradually purer as it ascends.
Figure 8 illustrates an essentially similar arrangement, but each pair of agitating
vessels M and precipitating vessels N are placed alongside of each other. The oil
and chemicals are similarly supplied and drawn off, and the current of oil and
chemicals similarly made to flow in opposite directions, the oil entering by the
pipe o into the last agitating vessel M of the series, and the acid or alkalis flows
or flow into the finishing agitating vessel M of the series by the pipe p². The
commingled oil and acid or alkalis pass from the finishing agitating vessel M through
the passage q into the finishing precipitating vessel N, the pure oil passing away
by the piper and the acid or alkalis settling out, partially fouled with impurities,
pass by the pipes n back into the central agitating vessel M, thence up the passage q
and by the pipe n³ into the first agitating vessel, and thence by the passage q to
the precipitating vessel above, from which they are drawn off in a fouled condition
by the pipe n³. The passages marked q* are the equivalents of every alternate
passage q in Figure 7. Although in the arrangements shown there are three
agitators and three precipitating vessels, two or any greater number may be
employed, the process consisting of the fractionating and continuous application of
the acid or alkalis to the oil.
Figure 9 is a diagram illustrating the manner in which the herein before described
fourth part of my Invention may be carried into effect, where the ammonia has to
be manufactured into salts of ammonia, such as sulphate, R is the fractionating
still arrangement, consisting of a series of vessels or compartments placed over
each other, the bottoms of those vessels having a large number of tubular openings
or short vertical pipes which are covered by thin metal cups ³, held in position
by means of a wire or rod fixed to the centre of the cup and hanging into
the tubular openings. The cups ³ are corrugated or perforated round the margin
to break up the steam into as numerous streams as possible. The ammoniacal
liquor is supplied to the still R from a tank at an elevation or by means of
a pump through the pipe s, and passes down from vessel to vessel of the
still by overflow pipes, like those shown at 4, communicating from vessel to
vessel, and projecting upwards into each vessel to a sufficient distance to maintain
the right level of liquor in each vessel. The ammonia and steam pass down by the
pipe t into the saturater or vessel T, in which the sulphuric acid is placed. This
vessel may be constructed of wood, iron, or other suitable material lined with lead
in the usual way. The curtain or partition 2 prevents the steam from finding its
way to the air, and causes it to pass from the top by the pipe t³ into the bottom
of the still R. On this pipe 3 is placed a powerful steam jet (or its equivalent)
of any suitable construction, as indicated at t, the steam being led thereinto by
the pipe from the boiler V, the said pipe being provided with a stop cock at v²,

page_text: having a branch pipe v³ leading into the lower part of the still R and provided
with a stopcock at to enable steam to be led directly into the still when required.
U represents a supplementary saturating vessel, similar to that just described, the
use of which will be evident when describing the mode in which the process. is
conducted, which is as follows:-
The whole of the chambers or vessels of the still R, with the exception of two or
three lower ones, having been filled with the ammoniacal liquor to be treated, and
acid having been placed in the two saturating vessels T and U, the valve u³ on the
pipe u leading from the top of the stilling arrangement to the supplementary
saturator U is opened, and the valve to on the pipe t is closed. The valve v² is.
closed and the valve is opened, and steam is admitted from the boiler V by the
pipe v and branch v³ directly to the bottom of the still R, which steam soon raises
the temperature of the ammoniacal liquor contained in the still, causing it to give
off gases, carbonic acid, and sulphuretted hydrogen, which it contains partly in
solution and in combination with the ammonia. These gases, together with any
little ammonia accompanying them, pass by the pipe u into and through the acid
in the supplementary saturating vessel U, the ammonia being absorbed by the acid
and the gases passing away by the pipe us to a box containing hydrated oxide of
iron which absorbs the sulphuretted hydrogen, the carbonic acid being allowed to
escape. So soon as the temperature reaches about 180° Fahrenheit in the division
or vessel of the still R above the pipe t, the valve on this pipe is opened, and
steam turned on to the jet t. This causes the ammonia and steam in the still R
to pass down the pipe t into and through the acid in the saturator T, where the
ammonia and accompanying steam are both at first absorbed by the cold acid;
but the acid soon becomes heated by the absorption of the gaseous ammonia and
the hot steam when only the ammonia is absorbed, and the pure steam is drawn
by the steam jet and again passed back and up through the ammoniacal liquor in
the chamber of the still R. The steam entering by the pipe is now turned off,
and a continuous supply of ammoniacal liquor turned on by the pipe 8, the quantity
being such that it shall keep the last or upper vessel of the stilling arrangement
comparatively cold, at least under 90° Fahrenheit, at the time that each of the
successive lower vessels of the arrangement is hotter and hotter till the vessel
above the outlet contains liquor of at least 180° Fahrenheit. This adjustment of
the temperature may be also modified by turning on or off more or less steam
entering the bottom of the stilling arrangement.
The liquor denuded of the ammonia having reached the lower vessel of the
stilling arrangement is drawn off by the pipe provided with a cock and syphon-
bend. Should the ammoniacal liquor contain ammonia in such a form as cannot
be volatilized by steam-heat alone, caustic lime is added to the ammoniacal liquor
in the lower vessel in the usual well known way.
It will be evident that the advantages of this process are that the gases, carbonic
acid, and sulphuretted hydrogen are disassociated from the ammoniacal liquor by
the treatment in the upper vessels, and that the sulphur may be recovered; that
the ammonia liberated from the liquor in the lower vessels of the arrangement is
mostly in the caustic state, and that the same steam is by means of the steam jet
made to circulate continuously, repeatedly acting upon fresh quantities of liquor
and thus greatly economizing fuel.
Figure 10 shows another modification by which the same steam may be used
more than once for the elimination of ammonia from ammoniacal liquor in the
manufacture of salts of ammonia. R¹, R³, represent two fractional stills constructed
similarly to that described with reference to Figure 9. The steam for the treatment
of the liquor enters by the pipe 3 into the bottom vessel of the still R' and passes.
up through the liquor contained therein, eliminating and carrying forward the
ammonia by the pipe w into the saturating box W containing acid. The ammonia
is here absorbed, and the steam passes by the pipe w' into the second distilling
arrangement R2, where it again acts upon the descending liquors carrying over the
ammonia by the pipe w³ into the second vessel or saturator W where the ammonia

page_text: is absorbed by the contained acid. The steam from this saturator W' may be
allowed to escape or may be carried to another stilling arrangement by the
pipe w³
The ammoniacal liquor is fed into the stills R' and R2 through the pipe x, and
the relative quantity regulated by the valves x, x². The hot denuded liquor is
drawn off from the bottom of the stilling arrangement by the pipes 75 and may be
passed through any convenient heat interchanging arrangement, as indicated at Y,
so as to heat the ammoniacal liquor entering the still. In operating with such an
arrangement as this it is found most convenient to completely cover all but the
last saturating vessel, and only salting down or crystallizing in the last vessel,
drawing off the solution of the salts of ammonia from the other vessel or vessels
into it for this purpose. w is the valve shewn on the Drawing for this purpose.
Figure 11 is a diagram illustrating the arrangement which I employ when the
ammonia in the ammoniacal liquor is to be used to remove the gaseous impurities
from illuminating coal gas. The arrangement and its mode of operation are
substantially identical with those described for the manufacture of ammonia salts,
with the exception that the steam is not made to circulate, but is supplied from
any convenient source by the pipe t³. When high pressure non-condensing engines
are used to exhaust the gas, pump liquor, and the like, the exhaust steam may be
very conveniently employed. The caustic ammonia and steam produced, as before
described, on leaving the stilling arrangement R³ by the pipe t, may be conveyed
direct to the condenser and commingled with the impure coal gas, and thus allowed to
absorb the gaseous impurities, but I prefer first to cool the mixed steam and caustic
ammonia by passing through a cooling-coil of pipes, indicated at Z, immersed in
water, where they are condensed, and the caustic liquor with any uncondensed
ammonia gas is passed direct into a scrubbing arrangement, similar in construction
to the fractional distilling arrangement previously described, only, of course, larger
in proportion to the volume of gas it has to pass, preferably entering at about the
middle vessel or compartment of such scrubbing arrangement.
Or the ammonia and steam may be fractionally cooled and separated to a large
extent by means of the supplementary stilling arrangement R*, the ammoniacal
gas passing away by the pipe 75, and introduced into the coal gas as it enters the
scrubber or washer. The syphon bend is for conveying condensed water from the
fractionater R back into the fractionating still R³.
The passing of the ammonia into the gas in either of these modes leads to the
absorption of the impurities from the gas by the caustic ammonia, and the pro-
duction of a very strong solution of ammoniacal liquor. By re-using the concentrated
solution of ammonia in the fractional stilling arrangement, a small amount of heat
is required to liberate the impurities, rendering the ammonia caustic, and again
revolatilizing the caustic ammonia, to be again passed into the coal gas and used
to remove impurities.
The ammoniacal liquor may be thus made so strong as to make it impossible
to render it caustic without the simultaneous passage of a considerable volume of
ammonia; and when desirable this process can be very conveniently combined with
the production of salts of ammonia such as the carbonate or bicarbonate by passing
the mixed gases and ammonia from the top of the stilling arrangement R³ by the
pipe u into any convenient crystallizing chamber placed between the stilling
arrangement R³ and the saturater U, as indicated at Z³, and then allowing the
carbonized salts of ammonia to settle out.
Having now described and particularly ascertained the nature of my said
Invention, and the system, mode, or manner in or under which the same is or
may be used or practically carried into effect, I would observe in conclusion that
what I consider to be novel and original, and therefore claim as the Invention
secured to me by the herein before in part recited Letters Patent is,-
First. Effecting the destructive distillation of shale or other similar substances
at two temperatures, namely, first, at a low equal temperature for the production of
mineral oil; and, secondly, at a considerably higher temperature for the production

page_text: of ammonia, either in two separate retorts or in one very long retort, essentially
as herein described with reference to Figures 1, 2, 3, and 4 of the accompanying
Drawings.
Second. Subjecting oils containing impurities to the action of caustic soda, lime,
or soda-lime whilst the said oils are in the hot or vapourous state, all essentially
as herein described with reference to Figures 5 and 6 of the accompanying
Drawings.
-
Third. The process of and apparatus for subjecting the oils to the action of acids
and alkalis in such a manner that the pure acid and alkalis are used to treat the
nearly or comparatively pure oil, and that as the acid and alkalis become more and
more saturated with impurities they are successively applied to treat or act upon
more impure oil, all substantially as hereinbefore described with reference to
Figures 7 and 8 of the accompanying Drawings.
Fourth. The economical separation of the ammonia from ammoniacal liquor by
causing the steam which has been used to eliminate the ammonia from the liquor
and to convey the ammonia to the saturating vessel to be used over again for a
like purpose, according to the manner and by means of the arrangement, essentially
as hereinbefore described with reference to Figures 9 and 10 of the accompanying
Drawings.
Fifth. Treating ammoniacal liquor for obtaining ammonia for use in the
purification of coal gas, essentially as and by means of the arrangement of
apparatus described with reference to Figure 11 of the accompanying Drawings,
and the employment of ammonia so obtained in the purification of coal gas,
essentially as hereinbefore described.
In witness whereof, I, the said William Young, have hereunto set my hand
and seal this Tenth day of October, in the year of our Lord One thousand
eight hundred and eighty one.