Improvements in and Connected with Apparatus for Distilling Ammoniacal Liquors.
Year: 1887

page_text: Date of Application, 31st Aug., 1887
Complete Left, 31st May, 1888
Complete Accepted, 6th July, 1888
Improvements in and Connected with Apparatus for Distilling
Ammoniacal Liquors.
I, ROBERT WYLLIE, of 50 Bewsey Street, Warrington, in the County of Lancaster,
Chemical Engineer, do hereby declare the nature of my said invention to be as
follows:-
This invention relates to the distillation of ammoniacal liquors such as chloride of
ammonia for the extraction of ammonia therefrom and has particular reference to such
ammoniacal liquors as are produced, or used in the ammonia soda process.
According to this invention the ammoniacal liquor, for example, chloride of
ammonia, such as that produced in the ammonia soda process is subjected to heat,
such heat being imparted to the liquor in the form of steam and the liquor is sub-
jected to the steam in finely divided, or distributed quantities. The streams of the
liquor are obtained by bringing the liquor onto a succession of trays arranged in a
vertical apparatns. The edges of these trays are serrated and the liquor in flowing
over the edges is through such serrations broken up, or divided into streams. This
overflow is caught by lower or catch trays which constitute diaphragms. A central
hole is provided in each catch tray such hole having a rim round it and serrated in a
similar manner to the rim of the trays just described. The liquor overflowing from
the lip of the uppermost tray falls onto the catch tray below it and then flows over the
lip of this tray onto the next, and so on throughout the series of trays. The steam
flows in the opposite direction to the liquor, that is to say it passes through the
central hole of the lowest catch tray and through the streams of the liquor overflowing
the lip of the dividing trays. In its repeated passage through the falling finely
divided streams or showers of the liquor, the liquor becomes heated and free ammonia
is taken up and the steam and ammonia finally finding its way to the outlet of the
apparatus. By the above it will be observed that one dividing tray and one catch
tray which forms an annular diaphragm-constitute a series; and any suitable
number of such series may be employed.
Previously to the above described process the steam is passed repeatedly through
the same liquor in another, or prior series of trays which form diaphragms. In these

page_text: trays the liquor has added to it a quantity of milk of lime. This addition is made in
the first tray of this portion of the apparatus which by preference is of cylindrical
shape and vertically arranged, the first described portion being arranged directly
above the latter portion.
Each of these trays is provided with a man-hole and lid and several pipes of an
inverted form, through which the steam and gaseous ammonia ascend in their flow
upwards. The exits of these pipes are arranged to deliver the steam and gas in a
horizontal direction to, and at, the bottom of the trays and the liquor contained in
them. The force of the steam used and the direction of its issue from the inverted
tubes together cause a very active circulating, or circular motion of the liquor. The
liquor descends from one tray to another by overflow pipes, the mouths of which are
movable for flushing purposes and are placed at such a distance from the bottom of
the trays as will maintain the required depth of liquor within them, and their lower
ends dip into the liquor of the tray next below; thus each pipe is sealed and the space
between the trays constitute closed. compartments. The exits of these dip pipes are
also formed to direct the delivery of the liquor so as to aid in the formation of the
circular motion of it.
The inverted U pipe for the ascending steam and gaseous ammonia and the dip
pipes for the descending liquor are provided with non return check valves.
The milk of lime used in the process of distillation is delivered by a pipe into the
top tray, of the bottom part of the apparatus, where it is thoroughly mixed with the
chloride of ammonium as it descends from the upper part of the apparatus in a hot
condition. In the lower trays it is subjected afresh to the agitation and heating
action of the steam. When the liquors have reached the bottom compartment and all
the ammonia has been liberated they are discharged through a suitable pipe at, or
near the bottom of the said compartment.
The steam is passed into the lowest compartment of the bottom part of the apparatus
above described and ascends from one tray to another by the inverted U pipes above
described after having passed through the bottom part of the apparatus it ascends
the upper part of the apparatus, carrying with it the free ammonia.
I would have it understood that this invention is not limited to the exact details.
herein described as these may be varied without departing from the substance of my
invention.
Ր A L 1007

page_text: Improvements in and Connected with Apparatus for Distilling
Ammoniacal Liquors.
I, ROBERT WYLLIE, of 50 Bewsey Street, Warrington in the County of Lancaster,
Chemical Engineer, do hereby declare the nature of the said invention and in what
manner the same is to be performed, to be particularly described and ascertained
in and by the following statement :-
This invention relates to the distillation of ammoniacal liquors such as chloride of
ammonia for the extraction of ammonia therefrom, and has particular reference to
such ammoniacal liquors as are produced, or used in the ammonia soda process.
According to this Invention the ammoniacal liquors, for example chloride of
ammonia, such as that produced in the ammonia soda process is subjected to heat,
such heat being imparted to the liquor in the form of steam and the liquor is
subjected to the steam in finely divided or distributed quantities. The streams of the
liquor are obtained by bringing the liquor onto a succession of trays arranged in a
vertical apparatus. The edges of these trays are serrated and the liquor in flowing
over the edges is through such serrations broken up, or divided into streams. This
overflow is caught by lower or catch tray, which constitute diaphragms. A central
hole is provided in each catch tray, such hole having a rim round it and serrated in a
similar manner to the rim of the trays just described. The liquor overflowing from
the lip of the uppermost tray falls onto the catch tray below it and then flows over
the lip of this tray onto the next, and so on throughout the series of trays. The steam
flows in the opposite direction to the liquor, that is to say, it passes through the
central hole of the lowest catch tray and through the streams of the liquor, over-
flowing the lip of the dividing trays. In its repeated passage through the falling
finely divided streams, or showers of the liquor, the liquor becomes heated and free
ammonia is taken up, and the steam and ammonia, finally finding its way to the outlet
of the apparatus. By the above it will be observed that one dividing tray and one
catch tray-which forms an annular diaphragm-constitute a series, and any suitable
number of such series may be employed.
Previously to the above described process the steam is passed repeatedly through
the same liquor in another or prior series of trays which form diaphragms. In these
trays the liquor has added to it a quantity of milk of lime. This addition is made
in the first tray of this portion of the apparatus, which by preference is of cylindrical
shape and vertically arranged, the first described portion being arranged directly above
the latter portion.
Each of these trays are provided with a manhole and lid and several pipes of an
inverted form, through which the steam and gaseous ammonia ascend in their flow
upwards. The exit of these pipes are arranged to deliver the steam and gas in a
horizontal direction to and at the bottom of the trays and the liquid contained in them.
The force of the steam used and the direction of its issue from the inverted tubes
together causo a very active circulating or circular motion of the liquor. The liquor
descends from one tray to another by overflow pipes, the mouths of which are moveable
for flushing purposes and are placed at-such a distance from the bottom of trays as

page_text: will maintain the required depth of liquor within them, and their lower onds dip into the
liquor of the tray next below; thus each pipe is sealed and the space between the
trays constitute closed compartments. The exits of these dip pipes are also formed
to direct the delivery of the liquor so as to aid in the formation of the circular motion
of it.
The inverted U pipe for the ascending steam and gaseous ammonia and the dip
pipes for the descending liquor are provided with non return check valves.
The milk of lime used in the process of distillation is delivered by a pipo into the
top tray of the bottom part of the apparatus, where it is thoroughly mixed with the
chloride of ammonia as it descends from the upper part of the apparatus in a hot
condition. In the lower trays it is subjected afresh to the agitation and heating action
of the steam. When the liquors have reached the bottom compartment and all the
ammonia has been liberated they are discharged through a suitable pipe at, or near
the bottom of the said compartment.
The steam is passed into the lowest compartment of the bottom part of the apparatus
above described and ascends from one tray to another by the inverted U pipes above
described after having passed through the bottom part of the apparatus it ascends
the upper part of the apparatus, carrying with it the free ammonia.
;
The above sets forth generally the naturo object and purposes of this invention, but
in order that the same may be more clearly understood I have hereunto annexed
2 sheets of Drawings illustrative thereof, and forming a part of this specification.
DESCRIPTION OF THE DRAWINGS.
Figure 1 is an elevation in section of distiller embodying improvements according
to my invention.
Figure 2 is an outside view of the apparatus.
Figures 3 and 4 shows the apparatus in cross section in the horizontal plane at the
lines XX and Y Y respectively.
Figures 5 and 6 are details in vertical section to a larger scale of the upper and
lower portions respectively of the apparatus.
Figure 7 is a cross sectional plan of the apparatus at the line ZZ Figure 6.
Figure 8 is a modification illustrating the upper portion of the apparatus having the
same construction as the lower part.
With reference in the first instance to Figures 1 to 4 of the drawings, A designates
the casing of the apparatus having a number of manholes p therein, B and C denoto
a number of alternate trays over which the liquor is passed a number of times in the
upper portion, and D are the trays over and round which the liquor is passed in the
lowor portion of the apparatus. E is the chloride of ammonia inlet, F the steam
inlot, G the milk of lime supply pipe, H the chloride of calcium outlet, and J the
steam and ammonia outlet all of which are provided in the ordinary way with con-
trolling valves. L designates a central hollow column to which the inner edge of tho
trays B are secured, and around which the liquor circulates in the trays. I are the
pipes through which the steam passes from one tray to another. These pipes are bent
in the form of a U or syphon pipe (see particularly Figure 7) their bend being above
the liquor level, and their delivery orifice being immersed in the liquor and provided
with a non return valve . This valve prevents at all times any liquor being forced
back from one tray to another. A number of pipes I are used in each tray and their
exit orifices are all arranged at an angle to the diameter of the plane of the circle in
which they lie (see Figures 3 and 7). K are the conduits through which the liquor
flows from one tray D to another. They consist of two portions, one, the upper,
being the feed portion, and the other, the lower, being the delivery portion, its
delivery orifice being provided with a non return valve k¹ and immersed in the liquor,
and arranged in the same manner as the delivery orifices of the pipes I. The upper
portion of a pipe K is separable from its lower part, the joint which is designated
being a conical friction joint. By lifting out the upper parts of the pipe Kit
will be evident all the trays D can be emptied of their contents. The trays B are

page_text: circular and placed concentrically within the casing A, leaving thereby an annular
space between their perepheries and the case; whilst the trays C are provided with
a central aperture of less diameter than the tray B. Both trays B, and C, are shallow
and provided at that part of them, from which the liquor overflows, with serrated
edges and respectively.
The operation with respect to the flow of liquor through the apparatus is as
follows: The chloride of ammonia enters the uppermost tray by the pipe E and flows
over the serrated edges of one tray B to C, and from C to B, and so on through the.
whole series in finely divided streams. At the point at which the milk of lime is
introduced, namely by the pipe G', the action of flow becomes different (as will be
presently described) as the combined liquors fall into the first of the trays D. From.
one of these trays to another the liquor passes by the pipes K. The lip of the upper part of
cach pipe over which the liquor falls determines the level of liquid in each tray, and the
delivery from the exit orifice of each pipe is directed by the position and arrangement
of such exit orifice. Having arrived in the bottom of the apparatus the chloride of
calcium leaves it by the pipe H. The heating fluid, steam, traverses the apparatus
in the reverse direction to the liquid, that is, it passes upward through the apparatus,
due to pressure, whilst the liquor falls downwards, by gravity. The steam first enters
the apparatus by the pipe F, and then passes seriatim through the pipes I of each
tray D. The exit orifices of the pipes I are arranged horizontally or nearly so as
shown, and the direction of the steam leaving these orifices will consequently be
horizontal and will assume the direction in which the exit ends of the pipes I lic.
Then if the steam leaves the orifices at any considerable velocity the liquor will
thereby be put in motion, and will assume a circular motion about the centre of the
apparatus. By this motion and the rising of the steam through the liquor towards
its surface a thorough and complete circulation and agitation of it will be secured.
The circulation and agitation which will be carried on in each of the trays D, together
with the heat of the steam will, in the presence of the milk of lime, effectually free
ammonia from the liquor, which passes with the steam to the outlet J. The steam
however before leaving this outlet has after leaving the uppermost tray D to pass
through the ammonia chloride as it falls from the trays B and C, and C and B ; and
in so doing heats it thoroughly and also drives off any free ammonia in the liquor.
It is preferred that the apparatus shall be so operated that when the liquor arrives at
that point where the milk of lime is added, it shall be thoroughly heated, say to about
200° Fahr., and that by the time the steam and ammonia leave the apparatus they
shall be comparatively cool.
In Figure 8 a modified arrangement of the upper portion of the apparatus is shown,
that is to say that portion of the apparatus in which the preparatory heating of the
Ammonia Chloride and the driving off of the free ammonia is effected. Here in lieu
of the trays B and as shown in Figures 1 and 5, I use the construction of trays D,
pipes I, and pipes K set forth with reference to Figures 1 and 6; the action of the
steam overflow and circulation being exactly similar as that set forth with reference
to those trays.
Having now particularly described and ascertained the nature of my said inven
tion and in what manner the same is to be performed, I would state in con-
clusion that I am aware that prior to my invention it was a common practise in the
distillation of ammonia from its chloride to use the upper part of the apparatus as a
heater and to drive off the free ammonia, and to complete the process in its lower
portion, and that a series of trays over which the liquid falls or is passed are commonly
employed; I therefore make no claim to those generally, nor do I claim as new the
agitation of the liquor in the apparatus; but what I do claim in respect of my
invention is :-
First. In distilling apparatus of the type herein described, effecting the circulation
and agitation of the liquor by steam, substantially in the manner described, such
steam being delivered into the liquor below Its level by pipes having their outlets
arranged so as to put the liquor in motion as described.

page_text: Second. The employment in connection with apparatus for distilling ammonia
of steam pipes I having a bend standing above the level of the liquor in the trays in
which they are used.
Third. The use in combination with steam pipes, such as I, of apparatus for dis-
tilling ammonia, of non return valves, such as ¹, for the purposes set forth.
Fourth: In an ammonia distilling apparatus, a communicating pipe K consisting of
an upper and lower portion, said portions being provided with a connecting joint
such as described; also providing the delivery orifice of said lower portion with a
non return valve; substantially as and for the purposes set forth.
Fifth. An apparatus for distilling ammonia from its chloride comprising the
vessel A, trays D, steam pipes I, communicating pipes K, and trays B and C shown
in Figures 1 and 5, or, trays D, pipes I and K shown in Figure 8 the said parts
being arranged, operating and constructed substantially as set forth with reference to
the drawings.