Sesqui-sulphate of Iron, Commonly Called Nitrate of Iron.
Year: 1887

page_text: Date of Application, 21st July, 1887
Complete Left, 19th Apr., 1888
Complete Accepted, 15th June, 1888
or Sesqui-sulphate of Iron, Commonly Called Nitrate of Iron.
We, SAMUEL HALLSWORTH and RICHARD BAILES, of The Copperas Works, Armley,
Leeds, in the County of York, Manufacturing Chemists, do hereby declare the nature
of this invention to be as follows:-
--
This invention relates to improvements in the manufacture of ferric sulphate, or
sesqui-sulphate of iron, commonly called nitrate of iron.
"
Instead of employing the liquor named in the provisional Specification accompany-.
ing our application for Letters patent No. 10144 dated 20th July 1887, we take a
quantity of sulphuric acid and place it in an evaporating tank or liquor boiler similar to
that employed in Copperas Works, and dilute the acid with water to about twenty to
twenty five degrees Twaddle. The diluted solution is then heated to nearly boiling
point and at the same time we gradually add the fine or dry powder portion of what is
known as borings waste or refuse "which is a bye product produced at Aniline
Works or such other suitable material which contains a large per-centage of hydrated
sesqui oxide of iron. The process of evaporation and adding the above named
materials to the diluted solution under treatment is continued until the greater portion
of the acid has become neutralized, and the solution has attained a density of about
sixty five to seventy degrees Twaddle at nearly boiling point. The solution is then
run off into a mixing cistern, and whilst still hot a little per-oxide of manganese in
fine powder is gradually added and well stirred by any suitable means until any proto-
sulphate of Iron that may be formed is changed to sesqui sulphate. The completion
of the process may be known by the solution becoming rather muddy, when this
occurs no more per-oxide of manganese should be added. A few drops of the solution
are then put into a shallow dish or plate and placed in a cool place for a short time.
If no crystals of copperas (sulphate of Iron) appear the process is complete; but if
the contrary the process must be continued and a little more per-oxide of manganese
added, and the same test again applied until the desired result is obtained.
DL 1
Π
"
ST1007
SAMUEL HALLSWORTH.
RICHARD BAILES.
By W. Fairburn Hart,
Agent.

page_text: Improvements in or relating to the Manufacture of Ferric Sulphate
or Sesqui-sulphate of Iron, Commonly Called Nitrate of Iron.
We, SAMUEL HALLSWORTH, and RICHARD BAILES, of The Iron Liquor Works,
Armley, Leeds, in the County of York, Manufacturing Chemists, do hereby declare
the nature of this 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 improvements in the manufacture of ferric sulphate or
sesqui-sulphate of iron.
Instead of employing the liquor or Copperas named in the Specification accompany-
ing our application for Letters Patent No. 10144 dated 20th July 1887, we take a
quantity of sulphuric acid and place it in a strongly lead lined evaporating tank or
liquor boiler, similar to that employed in Copperas Works, and dilute the acid with
water to a density of about twenty to twenty five degrees (cold) Twaddel's
Hydrometer.
The dilute solution is then heated to nearly boiling point in the same manner as is
employed in the manufacture of copperas, and at the same time we gradually add the
fine dry floury or powder portion of what is known as "Iron Borings' Waste or
Refuse" (which is a bye product produced at Aniline Works, and which contains a large
per centage of hydrated sesqui-oxide of iron and some metallic iron) or such other
suitable material that contains a large per centage of hydrated sesqui-oxide of iron,
natural or artificial, for partly neutralizing the solution under treatment.
The process of evaporation and adding one of the above named materials to the
dilute solution under treatment is continued until about three-fourths of the acid has.
become neutralized, which may be ascertained by an ordinary test; and when the
solution has attained a density of about sixty five to seventy degrees Twaddel at nearly
boiling point the solution is then run into a strongly lead lined mixing cistern or tank,
and whilst still hot per-oxide of manganese in fine dry powder is gradually added and
well mixed therewith by any suitable means until any proto-sulphate of iron that may
have been formed is changed to ferric sulphate or sesqui-sulphate of iron.
The completion of the process may be known by taking a few drops of the solution
and placing them in a shallow disli or plate in a cool place for a short time. If no
crystals of copperas (sulphate of iron) appear the process is complete, but if there be
much crystallization of copperas the process must be continued, and a little more
per-oxide of manganese added, and the same test applied until the desired result is
obtained.
When the operation of oxidizing the iron in the liquor is nearly completed it is
absolutely necessary that great care should be taken in the further addition of
per-oxide of manganese so as to avoid taking up too much of the sulphuric acid and
thereby neutralizing and oxidizing the solution to too great an extent. If the process
be carried too far the solution will become thick and gummy which must be avoided.

page_text: Ferric sulphate or sesqui-sulphate of iron made by the above process is applicable
for dyeing purposes.
our said
Having now particularly described and ascertained the nature of
Invention, and in what manner the same is to be performed we declare that what
we claim is
"
1. The process or method of manufacturing ferric sulphate or sesqui-sulphate of
iron from dilute sulphuric acid, which process consists in heating the solution, then
gradually adding as the partially neutralizing agent, either the fine floury portion of
ໄ Iron Borings waste" or hydrated sesqui-oxide of iron, whether in the form of
waste" or not, in fine dry powder to the dilute sulphuric acid during the evaporating
operation, and afterwards running the heated solution into a cistern or tank and
gradually adding and well mixing therewith per-oxide of manganese in fine dry powder
until the proto-sulphate of iron in solution is sufficiently oxidized, substantially as
and for the purposes herein set forth.
"
2. In the manufacture of ferric sulphate or sesqui-sulphate of iron from dilute
sulphuric acid, the use of either the fine floury portion of "Iron Borings' Waste" or
of hydrated sesqui-oxide of iron, whether in the form of "waste or not, in fine dry
powder as the partial neutralizing agent, and of per-oxide of manganese in fine dry
powder as the oxidizing agent, substantially as herein set forth.
Date : Echinouth day at Annil 1800
SAMUEL HALLSWORTH.
RICHARD BAILES.
By W. Fairburn Hart,
1, East Parade, Leeds,
Agent.