Year: 1896

page_text: Date of Application, 22nd Sept., 1896-Accepted, 21st Nov., 1896
Figure 3, an enlarged sectional view partly in elevation of the still, separating
drums, condenser and sweet water drums forming the right hand part of the
apparatus shown in Figure 1; and,
Figure 4, a diagrammatic view partly in section of two valved mechanical
vacuum pumps connected together in accordance with our present invention,
illustrating conventional mechanism for operating
mechanism for operating both of said pumps
simultaneously
In all of the above views corresponding parts are represented by the same
letters of reference.
A, represents a cylindrical still; B, is an eduction pipe therefrom connected
with a separating drum C; D, is a pipe connecting the separating drum C with a
second separating drum E, preferably larger in diameter than the drum C;
F, is a pipe connecting the separating drum E with a third separating drum G;
H, is a pipe connecting the separating drum G with a fourth separating drum 1;
is a pipe connecting the separating drum I with a cooler or condenser K; and
L, is a sweet water drum beneath the condenser or cooler K and supporting the
same, for receiving the material condensed therein.
J,
The still A and separating drums C, E, G and I are carried on a supporting
frame M, made preferably of I-beams, carried at the top of, and bolted to, columns
or pillars N, so as to be elevated a sufficient distance from the floor. The still A
is supported within the frame M by meaus of small brackets a, riveted to the sides
of the still A, and bolted to said frame. The separating drums C, E, G and I,
are supported on said frame, by means of cradles b, which are bolted to I-beams of
said frame. The sweet water drum L is carried on pillars or columns O, by means
of brackets c, riveted to the sides of said sweet water drum, and holted to the tops
of said pillars or columns.
Viewing the apparatus in the position shown, it will be noted that the eduction
pipe B connects with the separating drum C near the front of said separating

page_text: drum, that the pipe D connects the drums C and E near the back of said separating
drums, that the pipe F connects the drums E and G near the front of said
separating drums, that the pipe H connects the separating drums G and I near
the back of said drums, and that the pipe. J connects the separating drum I near
the front thereof, whereby the vapors from the still A are caused to pass from the
eduction pipe B through the entire lengths of the respective separating drums as
will be understood.
A steam pipe d connects with a heating coil which is mounted within the still A
for heating the contents thereof, the water condensed in said steam coil being
removed therefrom by a drip pipe e. Instead of heating the liquid in the still by
means of a steam coil as explained, other means for this purpose may be employed,
such as a steam jacket.
Steam is injected into the liquid treated for the purpose of distilling the same
through a steam pipe f, which connects at its lower end with a perforated injection
pipe or jet g The steam injected may be either live steam, superheated steam,
expanded or reheated steam, or steam prepared in any suitable way, or instead of
steam, air, gas, or any other vapor may be injected,.suitable for the distillation of
the particular material desired."
The material is introduced into the still A by a valved pipe A, and the residuum
in the still may be removed therefrom by the valved pipe i. A man-hole ; with
valved outlet in center at the bottom of the still is employed for cleaning the
interior thereof. A gauge or water column at the side of the still indicates the
height of the liquid therein. The eduction pipe B may be provided with a valve k
therein, for shutting off the still when desired.
1, represents a pipe mounted beneath the separating drums C, E, G and I,
opening at one end into the still as shown, and closed at the other end; and
m, m, m, represent short valved pipes connecting the respective separating drums
with the pipe L.
A pipo n, having a valve o therein, extends down froin the pipe 4, and the tank p
beneath said pipe n, receives the liquid flowing from the same. The sweet water
drum L is provided on its front end with a gauge or water column q, for indicating
the height of the liquid therein, and underneath with a valved draw-off piper, for
drawing off the liquid from said sweet water drum into a tank a placed beneath the
same.
The elements which I have above described, comprise one of the distilling plants
constituting our present apparatus, the other distillation plant comprising the rest
of our apparatus, and shown at the right hand side of Figure 1, consists of the
still P, separating drums Q, R, S and T, a cooler or condenser U, and a sweet
water drum V beneath said cooler or condenser, and connected with the same.
These elements are made preferably in the same way as the corresponding elements
before described, and for convenience and economy, iron or steel may be employed
for their construction.
W, is a pipe extending up from the sweet water drum V and connected with the
larger cooler or condenser X beneath which is a second sweet water drum Y. The
sweet water drum V is provided with a draw-off pipe having a valve u at its
lower end, and the sweet water drum Y is provided with a similar draw-off pipe o,
having a valve to at its lower end. A pipe a having a valve y therein connects
the draw-off pipes and t, above the valves u and to respectively. Receiving
tanks z and a are located beneath the draw-off pipes t and as shown.
The separating drunis Q, R, S and T, are connected by short valved pipes to a
pipe b' which enters the still P; and e' is a pipe having a valve d' at its upper end
for drawing off the material froin any or all of said separating drums when desired,
into a large receiving tank el.
The sweet water drums L and Y are connected together at their rear ends by a
pipe, which pipe is provided at its central part with a depressed portion g',
whereby liquids are prevented from flowing from one sweet water drum to the
other. The pipe is provided with valves A, A, therein, and extending down"

page_text: from said pipe between said valves is a small pipe which connects with a vacuum
pump Z, which is preferably a dry vacuum pump.
When a very high vacuum is desired in the apparatus, as is the case when
glycerin is being distilled, we prefer to employ a second vacuum pump j¹ which
connects with the exit pipe of the vacuum pump Z, the two pumps being operated
together. We find that the second vacuum pump supplements the first pump very
materially, and that by its use the desired high vacuum is produced. Both vacuum
pumps are ordinary commercial mechanical valved vacuum pumps of any approved
type.
In Figure 4 the connection of the vacuum pumps is illustrated on a larger scale,
the suction pipe of the pump being connected to the discharge from the pump Z
so as to enhance the action of the latter pump as explained. In this figure we
illustrate conventional means for operating both of the pumps simultaneously,
comprising the horizontal shaft carrying pulley wheels all which connect by
belts with the drive wheels c" of both pumps.
In Figure 1, we show receiving drums o' and o8 connected with the draw-off
pipes n and c¹ of the two series of separating drums, respectively, and provided with
valves o beneath them. Said receiving drums are provided with pet-cocks as
shown for admitting air therein.
The object of these receiving drums is to allow the contents of the separating
drums to be drawn off without destroying the vacuum in the apparatus, this result
being accomplished at the left hand side of the apparatus, for example, by opening
the valve o, the valve o' being closed, thereby allowing the liquid to flow into the
drum o, after which the valve o is closed and valve o' and pet-cock opened to allow
the liquid to flow out of said drum into the tank p. It is obvious that by opening
the valve of any one or more of the separating drums, the contents thereof may
be removed through the receiving drum o or o, independent of the other separating
drums.
In Figure 3, which shows the right hand side of the apparatus on a larger
scale, we illustrate additional features which are of especial importance, when
the crude glycerin contains glycol or other substances more volatile than glycerin
and which it is desired to separate from the glycerin while in the still.
At one side of the still, and below the same, is placed a receiving drum k¹, of
sufficient capacity for the purpose. The draw-off pipe of the still, connects with
this drum by a pipe , having an outlet m² at its other end. A tank n' is placed
beneath this outlet m¹. Valves o' and pl are placed in the pipe, on each side of
the draw-off pipe of the still. A pipe q', having a valve r³, connects the interior
of the drum with the still. Said drum is provided with a valved draw-off pipe s',
and with a pet cock t'.
In said Figure 3, we also show a drum connected to the pipe x, and provided
with a valved draw-off pipe vl, beneath which is a receiving tank to. Valves a, x',
are mounted in the pipe, on each side of the drum u', and said drum is preferably
provided with a pet-cock y'.
This drum u is of importance for use in connection with the druni ³, when the
apparatus is employed in fractionating as will be explained.
The operation of our complete apparatus for the distillation of crude glycerin is
as follows:-
The material is introduced into the still P, so as to fill the same to about one-
third of its capacity, either by pumping the same, or by the suction produced by
the operation of the vacuum pump Z and . The vacuum pumps continue to
operate and produce the desired degree of vacuum in the sweet water drums V
and Y, separating drums T, S, R, and Q, and still P. The material in the still P
is independently beated, such as by a steam coil, corresponding to the coil d of the
still A, and steam or other vaporizing agent of sufficient temperature to rapidly
distil the liquid therein is injected therein.
The vapors evolved from the still P pass successively through the separating
drums Q, R, S and T, thenee through the condenser U, sweet water drum V

page_text: pipe W, condenser ✗, and sweet water drum Y. The vapors evolved from the
still in passing through the separating drums Q, R, S and T, will be partially
condensed therein.
In practice we find that in the first drum Q, glycerin with impurities are collected
and condensed which sometimes require to be returned to the still P through the
pipe b for redistillation; that in the separating drums R and S, glycerin generally
of high specific gravity and of sufficient purity for dynamite purposes is collected
and does not require subsequent treatment; and that in the separating drum T,
glycerin with varying quantities of water are condensed, which may therefore
require concentration.
The vapors passing through the condensers U and ✗ respectively, are condensed
therein, the resulting sweet waters consisting of condensed steam carrying from
one per cent. to ten per cent. or more glycerin, are collected in the drums V and Y.
By employing two or more separate condensers U and X as explained, any
condensable vapors are caught in the apparatus and prevented from passing
through the vacuum pump Z.
The sweet water collected in the drums V and Y are removed therefrom into
the tanks a¹ or z, and the dilute glycerin caught in the separating drum Tis
removed therefrom through the pipe b and c, and these products are then
concentrated. The glycerin collected in the separating drums R and S as
stated, is generally of sufficient purity for dynamite purposes, and therefore may
not need to be further treated, although when great purity is desired, it may be
redistilled alone or with the concentrated sweet waters. These concentrated sweet
waters are distilled in the still A, being introduced therein, preferably by means of
the suction produced by the vacuum pumps.
It will be understood that both distilling plants may be operated at the same
time, the vacuum in each being maintained by the vacuum pump or pumps. The
concentrated sweet waters introduced into the still A are now maintained at a
temperature approximating to their boiling point, and steam or other vaporizing
agent is introduced of sufficient temperature for the purpose, through the injection
pipe g, so as to rapidly distil the material.
Products from the still A pass through the pipe B, into the separating drum C
in which glycerin, and the impurities, if any, carried over with the vapors, are
caught. From this drum the products pass through the pipe D, into the separating
drum E, thence through the pipe F, into the separating drum G.
glycerin generally of great purity and excellent quality is collected, the temperature
maintained in said drums being sufficient to prevent condensation of almost no water
therein.
In these drums
From the drum G the products pass through the pipe H into the separating
drum I, the temperature of which is generally sufficiently low to cause water to
condense, more or less, with glycerin, and which may therefore, require to be
concentrated. From the separating drum I, the products which now consists of
water carrying varying proportions of glycerin, pass into the condenser or cooler K,
by which the remaining water and glycerin is condensed and collected in the sweet
water drum L.
The dilute glycerin separated in the drum I and the sweet water condensed and
collected in the drum L, are now concentrated in a copper or other suitable
concentrating apparatus, to the desired specific gravity, the resulting product
being glycerin of great purity. The glycerin separated in the drums E and G
as stated, is generally of an excellent quality, and require no concentration. It
will therefore be seen that we have produced an apparatus particularly designed
for the distillation of glycerin from crude glycerin, which is simple in construction,
is very compact, efficient in use, and wherein a single vacuum pump or other vacuum
device is required.
The products condensed and collected in the drum V, consists of water with
varying proportions of glycerin, and ordinarily any products which pass through
the pipe W and condenser X into the drum Y, carry little or no glycerin, but

page_text: consists almost entirely or wholly of condensed steam. This water may therefore
be removed from the drum Y into the tank a', and allowed to run to waste, but, if
upon test it is found that the products condensed in the drum Y contain glycerin,.
it may be allowed to flow into the tank z, through the pipe a, the valve w being
closed.
We have found in practice that crude glycerin obtained from the waste soap
lyes of some manufacturers contains varying quantities of glycol, which is more
volatile than the glycerin and should be separated therefrom. By means of the-
additional appliances shown in Figure 3, we are enabled to use our apparatus as
a fractionating plant for the separation of glycol from the glycerin and for the
subsequent distillation of the glycerin. These operations are carried out as
follows:-
The crude glycerin is placed in the still P as heretofore, and the valves in the
draw-off pipes of the drums Q, R, S and T, are left open, the other valves being
closed. The vacuum pump being started, steam is injected into the liquid and the
liquid is preferably independently heated by a steam coil.
The temperature of the liquid in the still is maintained above the distilling point
of the glycol, but below that of the glycerin, so that the glycol distils off and
passes through the various separating drums, being collected in the drums V
and Y. The objects of keeping the valves in the draw-off pipes of the separating
drums open, are to allow said drums to be heated to a sufficiently high temperature.
so that after a while no glycol can condense and accumulate therein, and also to
allow any glycerin which may be mechanically carried over with the glycol, to be-
intercepted by said separating drums and flow back into the still. This operation
is continued until all the glycol has distilled off, whereupon the valve o' is opened
and the glycerin from the still runs into the drum k¹.
The still is again partially filled with crude glycerin, and the operations above.
described are repeated, until the drum k¹ is entirely full. The glycol condensed in
the drums V and Y is removed therefrom from time to time and flows into the-
drum u', the valves ¹, a, being opened and the valves u and to being closed; or
instead said valves may be left continuously opened or closed as required, so that
the glycol will accumulate continuously in the drum u. When the drum ul is to be
emptied, the valves a¹, x, are closed and the valve and pet cock y¹ opened, so
that the liquid flows out of said drum without affecting the vacuum in the
apparatus.
The glycerin which has accumulated in the drum k¹, is now drawn therefrom
into the still by suction through the pipe q', the valve r¹ and pet cock t¹ being
opened, and the temperature of the liquid increases so that the glycerin will be
distilled in the way we have described above.
Any foots in the still, are preferably removed through the outlet pipe m¹,
although if it is desired to keep the vacuum unbroken, the foots may be drawn off
into the drum k¹, and thence removed through the pipe s¹.
By these means we are enabled to employ our improved apparatus as a
fractionating plant, and the distillates produced may be separately removed
therefrom without destroying the vacuum therein.
Although we have above described the use of four separating drums with each
still, it is, of course, to be understood that a greater or lesser number of such
drums may be employed.
Having now particularly described and ascertained the nature of our said
invention, and in what manner the same is to be performed, we declare that what
we claim is :-
1. In a distillation or other vacuum apparatus, the combination with a closed
vessel, of a valved mechanical vacuum pump connected therewith, and a second
valved mechanical vacuum pump connected with and supplementing the action of
the first vacuum pump, substantially as set forth.
2. In a distillation or other vacuum apparatus, the combination with two closed

page_text: vessels, of a valved mechanical vacuum pump common to both vessels for
maintaining a vacuum therein, and a second valved mechanical vacuum pump
connected with and supplementing the action of the first vacuum pump, substantially
as set forth.
3. In a vacuum apparatus for distilling glycerin and other decomposable
materials, the combination of a closed vessel for containing the material, au
injection pipe for injecting steam into the material for the purpose of distilling the
same, a mechanical valved vacuum pump connected with the closed vessel for
constantly maintaining a vacuum therein, a second mechanical valved vacuum
pump connected with the exit of the first pump and supplementing the action of
the same, whereby the valves of both of said pumps will be interposed between
the atmosphere and the closed vessel, and means for constantly and simultaneously
operating both of said mechanical pumps, substantially as set forth.
4. In a vacuum apparatus for distilling glycerin and other decomposable
materials, the combination of two closed vessels for containing the material, an
injection pipe in each vessel for injecting steam into the material therein for the
purpose of distilling the same, a mechanical valved vacuum pump connected with
both of said vessels for constantly maintaining a vacuum therein, a second
mechanical valved vacuum pump connected with the exit of the first pump and
supplementing the action of the same, whereby the valves of both of said pumps
will be interposed between the atmosphere and the closed vessel, and means for
constantly and simultaneously operating both of said mechanical pumps,
substantially as set forth.
5. In an apparatus for the distillation of glycerin and other materials, the
combination with the still P, separating drums Q, R, S and T, connected together
and with said still, cooler or condenser U, and sweet water drum V, of the still A,
separating drums C, E, G and I, connected together and with said still, cooler or
condenser K, and sweet water drum L, and a vacuum pump Z connected with the
sweet water drums L and Y, for maintaining a vacuum in the stills A and P,
substantially as set forth.
6. In an apparatus for the distillation of glycerin and other materials, the
combination with the still P, separating drums Q, R, S and T, connected together
and with said still, couler or condenser U, and sweet water drum V, of the still A,
separating drums C, E, G and I, connected together and with said still, cooler or
condenser K, and sweet water drum L, a pipe f¹ communicating with the sweet
water drums L and Y, a depressed section gl in said pipe, valves h¹, h', therein,
and a vacuum pump Z connected to said pipe f¹ between said valves, substantially
as set forth.
7. In an apparatus for the distillation of glycerin and other materials, the
combination of a still, a condenser connected with said still, a sweet water drum
beneath said condenser, a second condenser connected with said sweet water drum,
and a second sweet water drum beneath said second condenser, substantially as set
forth.
8. In an apparatus for the distillation of glycerin and other materials, the
combination of a still P, a condenser U connected with said still, a sweet water
drum V connected with said condenser U, a draw-off pipe t for said drum, a tank z
beneath said draw-off pipe, a condenser X connected with said drumn V, a sweet
water drum Y connected with said condenser X, a draw-off pipe v for said drum Y,
and a valved pipe a connecting said draw-off pipes t and v, substantially as set
forth.
9. In an apparatus for the distillation of glycerin and other materials, the
combination of a stiil P, a condenser U connected with said still, a sweet water
drum V connected with said condenser U, a draw-off pipe t for said drum, a
condenser X connected with said drum V, a sweet water drum Y connected with
said condenser X, a draw-off pipe v for said drum Y, a valved pipe a connecting
said draw-off pipes t and v, and a drum u' connected with said pipe x, substantially
as set forth.

page_text: 10. In an apparatus for the distillation of glycerin and other materials, the
combination of a still P, a series of connected separating drums for said still, a
condenser U connected with said separating drums, a sweet water drum V con-
nected with said condenser U, a draw-off pipe t for said drum, a tank z beneath
said draw-off pipe, a condenser X connected with said drum V, a sweet water
drum Y connected with said condenser X, a draw-off pipe for said drum Y, and
a valved pipe x connecting said draw-off pipes t and v, substantially as set forth.
11. In an apparatus for the distillation of glycerin and other materials, the
combination of a still P, a series of connected separating drums for said still, a
condenser U connected with said separating drums, a sweet water drum V con-
nected with said condenser U, a draw-off pipe t for said drum, a tank beneath
said draw-off pipe, a condenser X connected with said drum V, a sweet water
drum Y connected with said condenser X, a draw-off pipe v for said drum Y, a
tank a' beneath said draw-off pipe, and a valved pipe connecting said draw-off
pipes t and v, substantially as set forth.
12. In a vacuum apparatus for the distillation of glycerin and other materials,
the combination with a still and draw-off pipe therefor, of a closed drum adjacent
to the still and connected with said draw-off pipe, and a valved pipe connecting
said drum with the still, substantially as set forth.
13. In a vacuum apparatus for the distillation of glycerin and other materials,
the combination with a still and draw-off pipe therefor, of a closed drum adjacent
to the still and connected with said draw-off pipe, and a valved pipe connected
with the still and extending inside of said drum, substantially as set forth.
14. In a vacuum apparatus for the distillation of glycerin and other materials,
the combination with a still and draw-off pipe therefor, of a closed drum adjacent
to the still and connected with said draw-off pipe, a valved pipe connected with the
still, and extending into said drum, and a pet-cock on said drum, substantially as
set forth.
15. In a vacuum apparatus for the distillation of glycerin and other materials,
the combination with a still and draw-off pipe therefor, of a closed drum adjacent
to the still and connected with said draw-off pipe, a valved pipe connected with
the still at a point above the bottom thereof, and extending into said drum,
and a pipe connecting the bottom of said still with said drum, substantially as set
forth.
16. In a vacuum apparatus for the distillation of glycerin and other materials,
the combination with a still and draw-off pipe therefor, of a closed drum adjacent
to the still and connected with said draw-off pipe, a valved pipe connected with the
still at a point above the bottom thereof and extending into said drum, a pipe
connecting the bottom of said still with said drum, and a pet-cock on said drum,
substantially as set forth.
17. In an apparatus for the distillation of glycerin and other materials, the
combination with still, of a series of separating drums connected with said
still and with each other, a draw-off pipe for each separating drum, a pipe
connecting said draw-off pipes, a pipe communicating with the latter pipe, a
closed drum in said pipe, and valves in said pipe above and below said closed drum,
substantially as set forth.
Dated this 31st day of August 1896.
JOSEPH VAN RUYMBEKE.
WILLIAM FREDERICK JOBBINS.
Haseltine, Lake & Co.,
45 Southampton Buildings, London, W.C., Agents for the Applicants.