IMPROVE- MENTS IN REVIVIFYING ANIMAL BLACK, IN APPARATUS EMPLOYED THEREIN, IN RECOVERING A PRODUCT EMPLOYED IN THE REVIVIFICATION
Year: 1862

page_text: LETTERS PATENT to Richard Archibald Brooman, of 166, Fleet Street,
in the City of London, Patent Agent, for the Invention of "IMPROVE-
MENTS IN REVIVIFYING ANIMAL BLACK, IN APPARATUS EMPLOYED THEREIN,
IN RECOVERING A PRODUCT EMPLOYED IN THE REVIVIFICATION."—A
communication from abroad by Absalon Hippolyte Leplay and Jules
François Joseph Cuisinier, both of Paris, France.
Scaled the 16th January 1868, and dated the 19th July 1862.
PROVISIONAL SPECIFICATION left by the said Richard Archibald
Brooman at the Office of the Commissioners of Patents, with his
Petition, on the 19th July 1862.
I, RICHARD ARCHIBALD BROOMAN, of 166, Fleet Street, in the City of
London, Patent Agent, do hereby declare the nature of the said Invention
for "IMPROVEMENTS IN REVIVIPYING ANIMAL BLACK, IN APPARATUS EMPLOYED
THEREIN, AND IN RECOVERING A PRODUCT EMPLOYED IN THE REVIVIFICATION,"
(communicated to me from abroad by Absalon Hippolyte Leplay and Jules
François Joseph Cuisinier, both of Paris, France,) to be as follows:-
This Invention is for improvements upon a former Invention for which
Letters Patent were granted to me, in consequence of a communication
from the said Leplay and Cuisinier, the 31st December 1861, No. 3275.
The Invention consists in treating the black, as hereafter explained, in a
series of revivifying cylinders, by preference four in number, as hereafter

page_text: stated. Each cylinder contains a perforated false bottom, for permitting tho
inlet of steam from a steam supply pipe; each cylinder communicates with
that next to it by a pipe extending from beneath the perforated false
bottom of one to the upper part of the next. There is also a pipe leading
directly from the upper part of the first cylinder to the lower part of the
last in the series. The animal black to be operated on is washed with
hot water before being placed in the cylinders; steam is admitted through the
perforated false bottom in the first cylinder, and a solution of caustic soda
in a boiling state is admitted at the top of the cylinder; the steam meeting
the solution of caustic soda causes a bubbling and agitating action, and a
general motion of all the particles of black; the caustic soda solution being
continued to be added passes into the second, third, and finally into the last
cylinder in the series. When the action has been continued long enough
in the first cylinder, the admission of caustic soda is prevented, and com-
munication closed to the next cylinder; hot water is now admitted, then
hydrochloric acid, after which a solution of bi-phosphate of lime, then water
to wash the black. The black is now completely revivified, is withdrawn,
and dried. The like process is continued in all the other cylinders, and
finally the caustic soda is made to deposit in the last cylinder in the series.
The caustic soda is fully charged with coloring matter from the black, and
is drawn off into a separate vessel, where it is evaporated. It is next
removed in a dry state, and is treated with nitrate of soda under heat, which,
driving off the coloring matter, leaves caustic soda.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Archibald Brooman in the Great Seal Patent Office :
on the 19th January 1863.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RICHARD
ARCHIBALD BROOMAN, of 166, Fleet Street, in the City of London, Patent
Agent, send grecting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Nineteenth day of July, in the year of our Lord One
thousand eight hundred and sixty-one, in the twenty-sixth year of Her reign,
clid, for Horself, Her heirs and successors, give and grant unto me, the said
Richard Archibald Brooman, Her special licence that I, the said Richard
Archibald Brooman, my executors, administrators, and assigns, or such others &
as I, the said Richard Archibald Brooman, my executors, administrators, and

page_text: assigus, should at any time agree with, and no others, from time to time and at
all times thereafter during the term therein expressed, should and lawfully
might make, use, exercise, and vend, within the United Kingdom. of Great
Britain and Ireland, the Channel Islands, and Isle of Man, an Invention for
"IMPROVEMENTS IN REVIVIFYING ANIMAL BLACK, IN APPARATUS EMPLOYED THEREIN,
AND IN RECOVERING A PRODUCT EMPLOYED IN THE REVIVIFICATION," (communicated
from Absalon Hippolyte Leplay and Jules François Joseph Cuisinier, both of
Paris, France,) upon the condition (amongst others) that I, the said Richard
Archibald Brooman, my executors, or administrators, by an instrument in
writing under my, or their, or one of their hands and seals, should particu-
larly describe and ascertain the nature of the said Invention, and in what
inanner 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 imme-
diately after the date of the said Letters Patent.
⚫ NOW KNOW YE, that I, the said Richard Archibald Brooman, 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 thereof, reference being had to the Drawings
hereunto annexed, that is to say:-
This Invention is for improvements upon a former Invention, for which
Letters Patent were granted to me, in consequence of a communication from
the said Leplay and Cuisinier, the 31st December 1861, No. 3275.
The Invention consists in treating animal black, as hereafter explained, in
a series of revivifying cylinders, by preference four in number, as hereafter
stated. Each cylinder contains a perforated false bottom, for permitting the
inlet of steam from a steam supply pipe; each cylinder communicates with
that next to it by a pipe extending from beneath the perforated false bottom
of one to the upper part of the next. There is also a pipe leading directly
from the upper part of the first cylinder to the lower part of the last in the
series. The animal black to be operated on is washed with hot water before
.being placed in the cylinders; steam is admitted through the perforated false
bottom in the first cylinder, and a solution of caustic soda in.a.boiling state-is
:admitted at the top of the cylinder; the steam meeting the solution of caustic
'soda causes a bubbling and agitating action, and a general motion of. all the
5 particles of black; the .caustic soda solution being.continued to be- added,
passes into the second, third, and finally into the last cylinder in. the series.
When the action .has: been continued long enough in the first cylinder, the
-admission of caustic soda is prevented, and communication closed to the next
cylinder; hot water is now admitted, then hydrochloric acid, after which a

page_text: solution of bi-phosphate of lime, then water to wash the black. The black is
now completely revivified, is withdrawn, and dried. The like process is con-
tinued in all the other cylinders, and finally the caustic soda is made to
deposit in the last cylinder in the series. The caustic soda is fully charged
with coloring matter from the black, and is drawn off into a separate vessel,
where it is evaporated. It is next removed in a dry state, and is treated with
nitrate of soda under heat, which, driving off the coloring matter, leaves caustic
soda.
Figure 1 of the accompanying Drawings is a vertical section; and
Figure 2 is a plan of the apparatus employed for carrying this Invention into
effect.
A, A', A", A, are metal cylinders or vessels, open at top, and placed
from 8 to 10 inches above the ground; B, B', B", are other cylinders or
vessels, set at a higher level, and to the rear of but parallel with the
cylinders A, in order to allow of free access to the top of the latter cylinders;
C is a pipe for leading steam into the cylinders B, B', and A, A¹, A", A¹;
D, D, are tubes extending into the cylinders B, B'; E is a pipe for conveying
water into the cylinders B, B, B", the flow of which is regulated by the taps
K, K, K; F, F, are troughs above the cylinders A, A', A", A, fitted with
valves for distributing in the said cylinders the liquid contained in the upper
cylinders B, B', B; G is a trough made of sheet iron, stone, or masonry, set
on the ground or on a level with the ground, to receive the liquid from the
cylinders A, A¹, A", A; H is a reservoir sunk in the ground; I is a boiler set
in a furnace; J, J, are steam taps; L, L, are emptying taps for the cylinders
B, B', B", the mouths of which are free to turn to either of the troughs F, F;
M, M, are emptying taps for the cylinders A, A, A", A; N is a pipe forming
a communication between the lower part of the cylinder A and the upper part
of the cylinder A¹; N' is a pipe forming a communication between the lower
part of the cylinder A' and the upper part of the cylinder A"; N" is a pipe
establishing communication between the lower part of the cylinder A" and
the upper part of the cylinder A"; N is a pipe forming a communication
between the lower part of the cylinder A and the upper part of the
cylinder A. The pipes N, N', N", N, should be fixed at such a height in
the upper part of each cylinder as to leave at least 10 inches or one foot of the
cylinder above the pipe; P is a perforated falso bottom, fitted to each of the
.cylinders A. It is supported at its edge by angle irons, and at other parts
by metal props placed on the bottom of the cylinder; Q, Q, Q", Q, are
taps for establishing communication between the cylinders A, A', A", A¹¹; R
is a boilor, set in a furnace on a level with the boiler I; S is a perforated

page_text: coiled pipe, for distributing steam under the false bottoms in the cylinders
A, A¹, A", A!!!
better, with hot water,
The working of the method of and apparatus for revivifying the animal
black with caustic soda, is as follows:-The animal black is placed in the
cylinders A, A¹, A", A", on the perforated false bottoms P until it reaches to a
short distance below the top of the communication pipes N, N', N", N. The
cylinder B is filled with water by the pipe E and tap K, sufficient caustic soda
being added to the water to cause it, while cold, to mark 5 degrees Beaumé;
steam is then admitted through the tap J until the solution is carried to the
boiling point. The cylinder B is filled with cold, or
which is carried to boiling point by steam introduced through the tube D, at
the same time the steam tap J is opened to admit steam into the cylinder A
charged with animal black. This steam soon passes through the black and
heats it, and when it has attained the temperature of the steam the flow
of the latter into the cylinder A is diminished, and the caustic solution is
allowed to flow through the tap L and one of the troughs F into the cylinder A
on to the surface of the black as long as the valve in the trough corresponding
with the cylinder A is kept open. During the in-flow of the caustic soda.
solution a small current of steam is maintained in the cylinder A to keep up a
continual agitation until the soda covers the black. Steam is then cut off
from the cylinder A and is admitted into the cylinder A', which is also charged
with black, and when the black is sufficiently heated (which is known by the
steam passing through it without becoming condensed) the valve Q on the
communication pipe N is opened and the flow of the soda solution is continued,
into the cylinder A; the liquid therein above the perforated bottom P escapes,
owing to the difference in the level, into the cylinder A' by the pipe N as long
as the caustic soda solution continues to flow into the cylinder A. The action,
of the steam in the cylinder A¹ is continued until the liquid issuing from tho,
lower part of the cylinder A has covered the top of the black in the cylinder A¹.,
During the time occupied by the preceding operation a current of steam has
been admitted and passed through the black contained in the cylinder A",
and thus heated it; the tap Q' is then opened to establish a communication.
between the cylinders A¹ and A" by means of the pipe N'; the flow of the.
caustic soda solution is then stopped and boiling water from the cylinder B¹ is,
admitted on to the surface of the black in the cylinder A until the cylinder A",
is completely filled. It must be understood that as soon as each cylinder is,
sufficiently filled with the caustic soda solution to completely cover the black
the flow of steam into the same cylinder must be arrested. All the soda;
solution which has flowed from the reservoir B into the cylinder A must be at.

page_text: the boiling point. When the cylinder A is filled with water and the cylinders
A and A" are filled with boiling caustic soda solution the black contained in
A is heated by a current of steam, the communication tap Quis opened, and
about 22 gallons of boiling water are thrown on the surface of the black in
the cylinder A, whereupon a quantity of highly-colored caustic soda solution,
corresponding in quantity to that of the water introduced into the cylinder A,
passes into the cylinder A". A supply of steam is maintained in the cylinder
A sufficient to keep the greater portion of the liquid at the top of the black,
then the flow of steam is suddenly stopped by closing the tap, the colored
liquid, being no longer supported by the steam, descends to the lower part of
the cylinder A. Steam is then again admitted, which causes the liquid to
again ascend into the upper layers of the black, the steam is again turned off
until the same liquid has returned to the lower part of the cylinder. This
operation is repeated three or four times until the liquid is impregnated to its
maximum with coloring matter. The emptying tap M of the cylinder A¹¹¹ is
then opened and all the liquid it contains is run into the trough G and thence
to the reservoir H. When the liquid has all run out the tap M is closed,
and fresh boiling water (22 gallons, for example) is run into the cylinder A,
when an equal quantity of colored caustic soda solution flows into the
cylinder A. Then this colored caustic solution is caused to rise and fall
through the black as before, until it contains its maximum of coloring matter,
when it is run off by the tap M into the reservoir H. This operation is
repeated several times with 22 gallons of water, or even more, according to
circumstances, until the last caustic soda solution admitted into the cylinder
A is not so highly colored, on issuing therefrom, as the preceding. The
tap is then closed to shut off the cylinder A, the outlet tap M therefrom
opened, and all the water tho cylinder A contains is run away to waste or
otherwise, fresh boiling water is admitted on to the surface of the black in the
cylinder A until the water which runs off by the tap M ceases to be colored.
At this point 'the boiling water is replaced by cold water, or hot water acidu-
lated with hydrochloric acid in the proportion of about a quart of acid to about
22 gallons of water contained in the cylinder B", and the washing is continued
with the acidulated water until that which runs off by the outflow tap is
neutral. The flow of the acidulated water is then stopped, all is allowed to
run off to wasto or otherwise, and cold or hot water is run on the black until
the escaping water has no salt flavor and no longer sensibly precipitates a
solution of nitrate of silver. After these different operations the black con-
tained in the cylinder A is completely revivified as far as its properties for
absorbing coloring matter are concerned. It is then removed from the cylinder

page_text: it
and immediately taken to the filter, where it can be used in a damp state after
baving been treated as bereafter described. The empty cylinder A is filled with
black to be revivified, and while these operations have been proceeding boiling
water is run on the black contained in the cylinder A¹. This water has dis-
placed all the caustic soda solution which was in the cylinder A', and has made
pass sinto the cylinder A", and that which was in A" has filled the cylinder A¹¹¹:
The cylinder A¹ is then cut off from the others, the outlet tap M is opened to
allow the liquid contained in A¹ to run away to waste. The cylinder A³ is con-
tinued to be supplied with hot water until the liquid escaping by the emptying
tap is no longer colored. The supply of hot water is then stopped and water
acidulated with hydrochloric acid is substituted as before in the case of the
cylinder A, and after the acidulated water the black is washed with boiling
water until the water flowing out from the bottom of the cylinder is no longer
salt. At the same time that this operation is being carried on in the
cylinder A', a current of steam has been made to pass through the black
contained in the cylinder A, and then the valve Q is opened to establish
communication between A and A. About 22 gallons of boiling water have
been run into the cylinder A", and in falling in A", which is already filled;
have caused an equal volume of colored caustic soda solution to pass into the
cylinder A. This liquid is made to rise and fall through the black by
means of a current of steam, as described with reference to the cylinder
A, and when the liquid ceases to extract the coloring. matter from the
black it is run off by its outlet tap M into the trough G, from whence it enters
the reservoir H. This.operation is repeated. in the cylinder A as long as
the caustic soda solution becomes saturated with coloring matter, the operation
taking place either with 22 gallons of water, or more. The cylinder A is now
emptied of its revivified black and filled with fresh black to be revivified, and
consequently ready to receive the action of the caustic sorla solution as before
practised in the cylinders A and A. The same treatment with caustic soda
solution by successive charges in the cylinders filled with black to be revivified,
the same washing with water of the black thus treated with the caustic soda
solution until the water runs off uncolored, the same washing with cold or hot
acidulated water after the washing with water, and the same washing with cold
or hot water after the acidulated water, are carried on. All these successive
operations are repeated in each cylinder filled with black, as before described,
and they should be performed in such manner that three cylinders are
continually in work while the fourth is being emptied or filled. According
as the black is more or less charged with coloring matter so the process
may be modified in the following manner :-Instead of running a small

page_text: .
quantity of colored soda into the cylinder which is charged with black to bo
revivified, and of climinating the soda saturated with coloring matter sue-
cessively in portions, the colored soda is run into the cylinder until it is
filled, and all the soda, considered sufficiently saturated with coloring matter
is drawn off by the tap at the bottom. By thus operating, the dissolving
action of the coloring matter takes place layer by layer, without the different
layers becoming mixed by the up and down motion imparted to it by the
steam: In the revivification of refinery black it is well, before treating the
black with the soda solution, to wash the black with a small quantity of water
acidulated with hydrochloric acid, afterwards with cold water, to eliminate
the salt formed by the acid; the soda is then found to dissolve the coloring
matter moro rapidly. Animal black revivified as herein-before described may
be put into the filter damp as it issues from the revivifying apparatus, but
before pouring in the syrup care must be taken to introduce hot water
charged with from 1 to 2 per cent. of bi-phosphate of lime. The filter is
filled with this water, which is then allowed to run off, hot water equal in volume
to that of the black is run into and through it, and the black is ready for
use. Sometimes the treatment with the bi-phosphate and the washing which
follows take place in the revivifying cylinder and the black is dried.
Recovery of the soda used in the process.-The chief expense in revivifying
animal black is the cost of the soda. There are certain chemical agents
possessing the property of decolorizing the caustic soda solution charged with
coloring matter from the operations before described. Chlorine and its
compounds possess this property. I prefer to destroy the coloring and other
matters mixed with the soda by subjecting the solution to a sufficient tempora-
ture and to an oxidizing agent; I use nitrate of soda by preference because
it is cheap and in no way injuriously affects the soda. I proceed thus:-Tho
solution of caustic soda charged with coloring matter which has been received
in the reservoir H is clarified and placed in the boiler I, where it is concen-
trated until the liquid becomes very thick. The fire is then withdrawn from
below or cut off from the boiler I, and the thick liquid or material is transferred
from the boiler I into the boiler R, where it is subjected to the heat of the
furnace. By degrees the material becomes of a pasty consistence, and then
nitrate of soda is by degrees well stirred into the mass, which destroys all the
organic matters extracted from the black by the soda. The nitrate of soda
must be added in small quantities, allowing time for its action between each
addition, and so on until the process is complete.
And having now described the nature of the said Invention, and in what
manner.the same is to be performed, I declare that I claim,-

page_text: First, revivifying animal black by means of caustic soda solutions and
washings, as herein-before described.
Second, the apparatus for effecting the revivification of animal black, com-
bined and acting substantially in manner herein-before described.
And third, recovering the soda employed in the process, as herein-beforo
described.
In witness whereof, I, the said Richard Archibald Brooman, have here-
unto set my hand and seal, this Nineteenth day of January, One-
thousand eight hundred and sixty-three.