Iм- PROVEMENTS IN UTILIZING A CERTAIN WASTE OR RESIDUAL PRODUCT OBTAINED · M ABOUT
Year: 1874

page_text: LETTERS PATENT to George James Hinde, of Wolverhampton, in the
County of Stafford, Manager of Works, for the Invention of "Iм-
PROVEMENTS IN UTILIZING A CERTAIN WASTE OR RESIDUAL PRODUCT OBTAINED ·
M
ABOUT "
Sealed the 8th May 1874, and dated the 11th March 1874.
PROVISIONAL SPECIFICATION left by the said George James Hinde at
the Office of the Commissioners of Patents, with his Petition, on
the 11th March 1874.
I, GEORGE JAMES HINDE, of Wolverhampton, in the County of
Stafford, Manager of Works, do hereby declare the nature of the said:
Invention for "IMPROVEMENTS IN UTILIZING A CERTAIN WASTE OR RESIDUAL
PRODUCT OBTAINED IN THE MANUFACTURE OF ANILINE DYES," to be as
follows:-
In the manufacture of aniline dyes iron borings or turnings or filings,
or iron otherwise finely divided, is used in considerable quantity. During
use in the manufacture of the said dyes the said finely divided iron is

page_text: oxidized, and constitutes a waste or residual product of little commercial
value.
My Invention consists in utilizing the said waste or residual product
in the ways herein-after described whereby it becomes revivified or
restored or nearly restored to its original condition of finely divided
metallic iron, and can be used again in the manufacture of the said
dyes or for other purposes where finely divided iron is required.
By my Invention the said finely divided iron can be used many times
by treating it in the way herein-after described after each time it has
been used. The revivified finely divided iron obtained according to my
Invention may be used alone or mixed with other unused iron borings or
filings or finely divided iron.
In treating the said waste or residual product according to my
Invention I mix it with about an equal weight of crushed charcoal or
other carbonaceous matter, and I heat the mixture either in crucibles,
muffles, or other vessels, in which the said mixture can be raised to a
red heat and protected from the action of the air. By this heating of
the mixture the oxide of iron is reduced to the metallic state under the.
deoxidizing or reducing action of the heated carbonaceous matter. The
crucible or vessel in which the mixture is heated is provided with an
outlet at which the gaseous matter formed may escape. The mixture is
allowed to cool before it is exposed to the air, when the metallic iron
and the unconsumed carbon may be separated. As the carbon is not in-
so finely divided a state as the metallic iron the two materials be
separated by the process of screening or sieving. I do not however
confine myself to any particular process for separating the reduced iron
from the carbonaceous matter.
gas
may
in con-
Instead of solid carbon carbonic oxide or hydrogen or coal
junction with heat may be employed for revivifying the iron. I prefer
however the use of carbon or carbonaceous matter, as herein first
explained.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said George James Hinde in the Great Scal Patent
Office on the 3rd September 1874.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, GEORGE
JAMES HINDE, of Wolverhampton, in the County of Stafford, Manager
of Works, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters.
Patent bearing date the Eleventh day of March, in the year of our
Lord One thousand eight hundred and seventy-four, in the thirty-
seventh year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said George James Hinde, Her special
license that I, the said George James Hinde, my executors, admini-
strators, and assigns, or such others as I, the said George James Hinde,
my executors, administrators, and assigns, 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 "IM-
PROVEMENTS IN UTILIZING A CERTAIN WASTE OR RESIDUAL PRODUCT OBTAINED IN
THE MANUFACTURE OF ANILINE DYES," upon the condition (amongst others):
that I, the said George James Hinde, my executors or admini-
strators, by an instrument in writing under my, or their, or one of their.
hands and seals, should particularly describe and ascertain the nature of
the said Invention, and in what manner the same was to be performed;
and cause the same to be filed in the Great Scal Patent Office within
six calendar months next and immediately after the date of the said
Letters. Patent.
NOW KNOW YE, that I, the said George James Hinde, 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, that is to say:
. In the manufacture of aniline dyes iron borings or turnings or filings,,
or iron otherwise finely divided, is used in considerable quantity; the
said divided iron being employed.in treating nitro-benzol in the process
by which aniline is obtained therefrom, During use in the said manu-

page_text: facture the said finely divided iron is oxidised, and constitutes a waste or
residual product of little commercial value.
My Invention consists in utilizing the said waste or residual product
for the purpose of manufacturing aniline or aniline dyes, which I prefer
to do in the ways herein-after described whereby it becomes revivified or
restored or nearly restored to the condition of finely divided iron, and
can be used again in the manufacture of aniline or aniline dyes.
By my Invention the said material can be used many times after
treating it in the way herein-after described after each time of using
it. The iron obtained according to my Invention may be used mixed
with other and unused iron filings or borings or finely divided iron.
In treating the said waste or residual product according to my
Invention I mix it with about an equal part by measure of crushed
charcoal or other carbonaceous matter, and I heat the mixture either in
crucibles, muffles, or cylinders, fixed or moveable, or other vessels in
which the said mixture can be raised to a red heat and protected from
the action of the air. The crucible or vessel in which the mixture is
heated is either open or provided with an outlet at which the gaseous
matter formed may escape. The mixture is allowed to cool before it is
exposed to the air, when the iron and the unconsumed carbonaceous
materials may be separated. As the iron is not in so finely divided a
state as the charcoal, coke, breeze, or other carbonaceous matter the two
materials may be separated by a process of screening or sieving. I do
not however limit myself to any particular process for separating the
iron from the carbonaceous matter.
Instead of solid carbonaceous materials carbonic oxide or hydrogen
or coal gas in conjunction with heat may be employed in the process. I
prefer however the use of charcoal, coke, or breeze as herein first
explained..
Having explained the nature of my Invention I will proceed to
describe the manner in which the same is carried into effect.
I take the residual product from the manufacture of aniline or aniline
dyes commonly called "black oxide." The said residual product consists
mainly of oxide of iron, and is produced by the oxidation of the iron
filings or borings employed in the manufacture of aniline or aniline dyes.
I calcine this "black oxide" in the manner in which oxides or ores of iron

page_text: are commonly calcined. The said calcining causes the "black oxide"
to become wholly or mainly red oxide. During the calcining process the
particles of oxide of iron become more or less agglutinated.
After calcination I reduce when cold the oxide of iron to pieces by
pounding or crushing it until the pieces are so reduced in size that none
are larger than one-eighth of an inch in diameter. In order to separate
the larger pieces I pass the pounded oxide through a sieve having sixty.
four meshes to the inch. I then take cinders from an ordinary fire, or
coke, or the small coke called breezes, or charcoal, or other solid car-
bonaceous materials, and I pound, crush, or grind the cinders, coke, or
breezes, or charcoal or other solid carbonaceous materials, until the
particles are very much smaller than those of the calcined oxide.
"
In order to secure the required degree of fineness in the pounded coke
or cinders, breezes, charcoal, or other solid carbonaceous materials, I pass
them through a sieve having one thousand meshes to the superficial
square inch.
I mix the pounded coke or other solid carbonaceous
materials with the calcined oxide in about equal proportions by measure.
I put the mixture of calcined oxide and pounded coke or other solid.
carbonaceous materials into pots or saggers made of fire-clay or other
material which will sufficiently resist the action of fire. After charging.
the pots I put a layer of pounded coke or other solid carbonaceous.
materials three or four inches deep on the top of the mixture of calcined.
oxide and ground coke or other solid carbonaceous materials, so that
when cooling the air would have to pass through a stratum of ground
coke or other solid carbonaceous materials before it could reach the
mixture of calcined oxide and ground coke or other solid carbonaceous.
materials.
After filling the pots or saggers in the manner described I place them,
in a kiln and heat them to such a temperature that the whole contents
mi

page_text: .
After the pots and their contents are sufficiently heated I allow them
to cool without opening them: This I effect either by letting the heat
of the kiln go down or by withdrawing the pots from the kiln and
allowing them to cool. When the pots and their contents are cold I
empty the contents on to fine sieves of sufficiently fine meshes to allow
the unconsumed finely pounded carbonaceous material to pass through;
but too fine to allow the pieces of iron to pass through: The sieve
having one thousand meshes to the inch which is used for sieving the
pounded coke answers for sieving the cooled contents of the pots. The car-
bonaceous matter is sufficiently separated by sieving or riddling, and the
iron so obtained can be used again in the process of manufacturing aniline.
This reduction of the oxide and use of the iron so obtained by the.
processes described can be repeated over and over again without limit
provided the iron so obtained be mixed with more or less of fine iron
borings, such as are ordinarily used in the manufacture of aniline or
aniline dyes.
Although I prefer to separate the converted iron from the particles of
carbonaceous matter by pounding the latter finely so that its particles.
shall pass through the sieve, while the larger particles of iron shall be
retained thereon, yet the contrary method may be employed, that is, the
particles of carbonaceous matter may be the larger and be retained on
the sieve, while the particles of iron may be the smaller and pass
through it..
-
Although I use by preference the carbonaceous substances that I have
described, yet I do not confine myself thereto, as other carbonaceous
substances can be used in lieu thereof, neither do I limit myself to the
particular method described of heating the pots containing the mixture
of oxide and carbonaceous matter, as other methods of heating may be
used. Nor do I confine myself to the use of pots for the purpose, as
ovens or retorts or cylinders fixed or moveable may be employed with
like effect.
Although I have described the resulting product of my process as iron.
it must be understood that the product is not pure iron, as it contains
more or less of carbon or other matters in combination or mixture. For.
effecting the reduction of the oxide of iron to iron gases of a deoxidising.
character, as hydrogen; carburetted hydrogen; or carbonic oxide, may

page_text: be used, but I prefer to use the carbonaceous matters in the solid
form.
Although I prefer to calcine the black oxide obtained in the manu-
facture of aniline previous to subjecting it to heat in contact with
carbonaceous substances in the manner described, I wish it to be under-
stood that the calcining process is not essential, as the black oxide may
be heated with carbonaceous matter without having been previously
calcined, but I do not consider the result equally satisfactory.
Having now described the nature of my Invention, and the manner
in which the same is to be performed, I wish it to be understood that I
claim as my Invention of improvements in utilizing a certain waste or
residual product obtained in the manufacture of aniline dyes, utilizing
the residual product called black oxide of iron obtained in the manu-
facture of aniline or aniline dyes for the purpose of making iron in a
state of division and using the iron thus made in the process of manu-
facturing aniline or aniline dyes.
In witness whereof, I, the said George James Hinde, have here-
unto set my hand and seal, this First day of September, in
the year of our Lord One thousand eight hundred and seventy-
four.
Witness,
ALLAN WEIR,
Wolverhampton.
GEORGE JAMES HINDE. (L.S.)