IMPROVEMENTS IN PURIFYING GAS, AND IN TURNING SULPHURETTED HYDROGEN, CARBONIC ACID, AND AMMONIA, OR THEIR COMPOUNDS, TO PROFITABLE ACCOUNT
Year: 1858

page_text: LETTERS PATENT to Richard Laming, of Haywards Heath, in the County
of Sussex, for the Invention of "IMPROVEMENTS IN PURIFYING GAS, AND
IN TURNING SULPHURETTED HYDROGEN, CARBONIC ACID, AND AMMONIA, OR THEIR
COMPOUNDS, TO PROFITABLE ACCOUNT."
Sealed the 27th May 1859, and dated the 1st December 1858.
PROVISIONAL SPECIFICATION left by the said Richard Laming at the
Office of the Commissioners of Patents, with his Petition, on the
1st December 1858.
I, RICHARD LAMING, of Haywards Heath, in the County of Sussex, do hereby
declare the nature of the said Invention for "IMPROVEMENTS IN PURIFYING
GAS, AND IN TURNING SULPHURETTED HYDROGEN. CARBONIC ACID, AND AMMONIA; OR
THEIR COMPOUNDS, TO PROFITABLE ACCOUNT," to be as follows:-
It consists in improved processes, and combinations of processes for purifying
gas, and manufacturing soda and ammoniacal products, and is designed to
render those manufactures in combination incidentally subservient to the
purification of the gas by supplying a purifying material.
The first part of this Invention is as follows:-Having collected the ordi-
nary ammoniacal liquor from the condensers which has been used to wash or
scrub the gas, having mixed it with water which has been used for a final
washing or scrubbing of the same gas, having deprived the mixed liquors
[Price 8d.]

page_text: either wholly or in great part of sulphuretted hydrogen by the agency of
metallic oxides, &c., as invented and patented by me (with or without the
subsequent removal of carbonic acid by lime), I then apply the said desul-
phurated solution of ammonia to the gas while on its way from the condensed
liquor washers or scrubbers to the water washers or scrubbers, thus giving it
an intermediate washing or scrubbing. By this combination of processes all
the ammonia of the gas is combined with its sulphuretted hydrogen and carbonic
acid, and those three impurities being thus made extremely soluble are removed
from the gas by the final washing.
The second part of the Invention is for substituting for carbonic acid in
the above liquor sulphuretted hydrogen, thereby reproducing the liquor in
a condition to be again more fully acted upon by the metallic oxides, &c., thus
augmenting to any required extent the quantity of ammonia in solution avail-
able for the purification of the gas. It consists in decomposing sulphuret of
sodium by means of ammonia and carbonic acid at temperatures and under
circumstances more advantageous than hitherto. The ammonia treated in
this way when in excess I make into marketable products, in which case I
sometimes purify it by passing it in a gaseous state through caustic soda or
potash in solution.
The third part of the Invention consists in improved processes for obtaining
sulphate of soda required for making the sulphuret of sodium above needed.
By one process it is obtained simultaneously with muriate of ammonia, by
subliming the latter into cool chambers from a mixture of sulphate of ammonia
and common salt, the ammoniacal muriate afterward acquiring a marketable
form by mechanical compression. By a second process the sulphate of soda
is obtained simultaneously with a metallic precipitate (which spontaneously
changes into a useful desulphurating oxide) by decomposing mixed solutions
of the
the sulphates of soda and manganese by means of sulphuret of sodium.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Laming in the Great Seal Patent Office on the
31st May 1859.
TO ALL TO WHOM THESE PRESENTS SHALL COME I, RICHARD
LAMING, of Haywards Heath, in the County of Sussex, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the First day of December, in the year of our Lord One
thousand eight hundred and fifty-eight, in the twenty-second year of Her

page_text: reign, did, for Herself, Her heirs and successors, give and grant unto me, the
said Richard Laming. Her special licence that I, the said Richard Laming.
my executors, administrators, and assigns, or such others as I, the said
Richard Laming. 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,
and
exercise, and vend, within the United Kingdom of Great Britain
Ireland, the Channel Islands, and Isle of Man, an Invention for "IMPROVE
MENTS IN PURIFYING GAS, AND IN TURNING SULPHURETTED HYDROGEN, CARBONIC
ACID, AND AMMONIA, OR THEIR COMPOUNDS, TO PROFITABLE ACCOUNT." upon the con-
dition (amongst others) that I, the said Richard Laming, my executors or
administrators, 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 Seal Patent Office within six
calendar months next and immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said Richard Laming, do. hereby declare the
nature of my said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, that is to say:-
To purify gas from sulphuretted hydrogen, carbonic acid, and ammonia, I
first scrub it with raw gas liquor from the condensers and mains, pumped free
from tar, through an ordinary scrubber as near as possible at the rate in which
it is produced, receiving it after it has passed the scrubber into a small cistern.
The gas after ascending through this first scrubber ascends through three:
others in succession, the fourth of which is supplied with common water.
entering in at least sufficient quantity to keep the. soluble impurities of the gas
from mounting to its upper part, which may be judged of by the usual tests
applied to trial cock's there placed, and I pump away that water as fast as it'
arrives at the lower part of the vessel into the upper part of the third scrubber
in which it becomes a stronger solution of ammoniacal liquor. From the
bottom of the third scrubber the liquor flows out into the small cistern already
mentioned, in which it mixes with the liquor from the first scrubber, and
which is so situated and fitted with communications as to overflow (as may be
determined from time to time) into one or other of a series of large vessels
filled with sawdust or other suitable porous material mixed with a metallic
substance capable of desulphurating either wholly or in part the liquor, and
afterwards of recovering by contact with atmospheric air its power to act

page_text: again in a similar, manner.
The metallic substance which I use for this
purpose is one or other of the following:-A compound of iron which I
obtain by first decomposing any solution of that metal in hydrochloric acid by
sulphuret of calcium, such as may be dissolved out by means of hot water
from what the soda makers call vat waste, and afterwards exposing the
resulting sulphuret of iron, washed or unwashed, to the air to become oxidized,
or a compound of manganese, particularly such as results from exposing to the
air a hydrated sulphuret of that metal, which I make by first using the
sulphuret of calcium in vat waste, or from any other source of decomposing
solution of muriate of manganése (which is a waste or residue in the manu
facture of chlorine), and then collecting the precipitated hydrated sulphuret
and freely exposing it washed or unwashed to the atmosphere, for which
purpose it is convenient to mix it with some porous material; or the compound
of manganese may be an oxide obtained in a hydrated or effective state from
any other source. Other preparations of iron which I have indicated in the
Specification of my Invention for which I obtained a Patent, bearing date the
3rd February 1857, may also be substituted for the different reagents above-
named for desulphurating the liquor to be used in the purification of gas by
this Invention. By the time a desulphurating vessel has become full of liquor
the latter will be either wholly or in part deprived of sulphuretted hydrogen.
according as the porous mixture is more or less rich in effective material
relatively to the impurity of the liquor. If the result be not at first perfect
it will improve with more time. The stream of liquor arriving to be
acted upon I then divert into another desulphurating vessel, and
portion already accumulated I draw off from the first vessel through a filter
of coarse cloth previously spread over a perforated false bottom within it
into a large tank, preparatory to its being used in the second scrubber of
the series. So soon as the desulphurating material has had its liquor
sufficiently drained from it, the vessel containing it is to be connected with
an exhauster or a chimney draught, or other equivalent. contrivance, so
that air may be passed through it for its oxidation, after which revivification it
may be again made use of as before; or instead of revivifying the material by
a current of air through the desulphurating vessels, it may be simply exposed
to the atmosphere either in them or thrown out upon the ground. When the
desulphuration or revivification becomes too slow or imperfect to be satisfactory,
I cause the mass of material to receive an additional quantity of its metallic
ingredient, or I exchange it for other entirely new. Instead of mixing the
metallic ingredients with porous materials, I sometimes stir them into the
liquor to be desulphurated, and then after recovering them by subsidence and
the

page_text: decantation or by filtration, I put them in the air to revivify, but, this mode is
less convenient than the other.
Amoniacal liquor thus or otherwise deprived of sulphuretted hydrogen, either
altogether or in great part, I pump into the second scrubber with a speed at
least great enough to convert all the sulphuretted hydrogen and carbonic acid
which the gas contains while passing through the second scrubber, into soluble
salts of ammonia, preparatory to their removal by the two scrubbers further
on. This may be judged of by trial cocks and tubes communicating with the
second scrubber near to its upper part, and plunging below into a little fresh
water; the gas on escaping from that water will not affect the ordinary lead or
lime tests, if the desulphurated liquor be in sufficient quantity, should it do so
the quantity must be increased. If a larger supply of desulphurated ammonia
be required than is furnished by the joint products of the first and third
scrubbers, it may be obtained by allowing part of the liquor from the second
scrubber again to enter the desulphurating vessels, or what is better these
joint products may be strengthened by hydrosulphate of ammonia, which may
be obtained as herein-after described. I prefer to distribute the liquor used
in each scrubber over the surface of its scrubbing materials by means of a
perforated pipe or pipes revolving within it as is well understood, and so
much of it from the second scrubber as is not returned to the desulphurating
vessels runs into a covered tank, from whence it is drawn to be made by any
known means into either a concentrated solution or a solid form of ammo-
niacal salts for use in the subsequent parts of the Invention.
This part of the Invention may be modified. When there is an abundant
supply of hydrosulphate of ammonia, it may be dissolved in the product. of
the water scrubbing, treated with the desulphurating material, and then
used on the gas without the latter being previously treated with raw gas
liquor. In this case the scrubbing with the desulphurated liquor should be
done in the first scrubber, and the second made to receive the water washings
from the third, mixed or not with raw gas liquor. When the raw gas liquor
is not used for purifying, it is to be distilled, either alone or with the used
purifying liquor, to form concentrated liquid or solid ammoniacal products
wanted for the subsequent parts of the Invention. Instead of the scrubbers
other kinds of washing apparatus may be substituted, and some insufficiency
of fluid purification may so far as sulphuretted hydrogen is concerned be
compensated for by causing the gas to pass on its way from the final scrubber
or washer to the gas holders through one or more ordinary dry purifiers
charged with the oxidized sulphuret of iron or of manganese above mentioned,
and which, mixed with porous material and used as dry lime, is adapted to

page_text: deprive the gas of any sulphuretted hydrogen that may have passed over
along with it. All the pumps should be in duplicate, made independent
of one another by separating valves easily got at and well protected from the
ingress of foreign matter. Each scrubber should be furnished with a bye-
pass, and such other arrangements made that either the first or second scrubber
may be used with desulphurated liquor, in case of the second or first respec-
tively being thrown out of action, and also that the third may be set to work
with fresh water during any temporary inaction of the fourth.
I turn sulphuretted hydrogen, carbonic acid, and ammonia, or their com-
pounds, to profitable account as follows:- take sulphuret of sodium, either
alone or with the carbonaceous matter by which it is contaminated in the
process of manufacture, and I thoroughly mix it with about an equivalent
proportion of carbonic acid in combination with ammonia, prefering to
use for that purpose the rough products which result from the distillation of
the ammoniacal liquors herein-before mentioned. If the carbonate of ammonia
be in the solid form it may be ground with the sulphuret of sodium with
or without admixture of carbonaceous matter; if the ammoniacal salt be
in solution, then so much of the carbonaceous matter should be mixed with
the sulphuret of sodium as to absorb all the water that will be present, which
admixture may be made either in manufacturing the sulphuret or afterwards.
I put the mixture with its equivalent dose of carbonic acid combined with
ammonia into iron pans; slide them into iron retorts, lute on the doors, and
expose it to a gentle heat (which may be about 300 degrees of Fahrenheit),
so long as ammonia or hydrosulphate of ammonia continues to come off.
It is important to observe that if the temperature be near a red heat, much
carbonate of ammonia will be driven out of the mixture without having
effected decomposition of the sulphuret of sodium, and that if the mixture
of reagents be in a pasty or fluid condition, it will either swell and overflow
by the eduction pipe, or by boiling undergo only a partial and unsatisfactory
amount of decomposition: The quantity of ammoniacal carbonate needs not
to be very accurately adjusted to the quantity of sulphuret, and excess will do
no harm, and enough may be known to have been present when at the end
of the operation the soluble part of the solid matter in the pans dissolved
in water does not blacken lead test paper. The retorts in which the de-
composition is effected are furnished with eduction pipes, sloping downwards
to conduct the volatile matters which escape from it into the lower part of a
scrubber or open cylinder filled with small coke, brick, or other solid materia
continually sprinkled with cold water, by which they are dissolved and washed
down into a close tank arranged for receiving them; when vapours cease to

page_text: leave a retort, I withdraw from it the pans, put others already charged into
their places and treat the solid product by known means for obtaining in any
marketable shape the carbonate of soda that it contains.
The ammonia having been made thus instrumental in purifying the gas
and in putting into a marketable combination the carbonic acid originally
contained both in the impure gas itself and in the liquors condensed from it,
now presents itself dissolved in water and in combination chiefly with
sulphuretted hydrogen, in which state it is particularly useful for affording,
by treatment with metallic substances, as already directed with respect to the
condensed gas liquor and washings, a solution of ammonia in great part or
altogether caustic. After thus treating it I use it in any required quantity for
saturating and making soluble the two above-named acid impurities of gas,
or I reuse its ammonia for the making of carbonate of soda, as above described,
after having recombined it with carbonic acid, by receiving that gas into
its solution, for which purpose it is not absolutely necessary that it should
have been first desulphurated; or I use the desulphurated liquor mixed or
not with condensed gas liquor or washings that have also undergone the
process of desulphuration, or even either or both the last-named liquors
unmixed with the first for obtaining solution of caustic ammonia of various
degrees of purity serviceable for various purposes in the arts. In this case
1 first treat the desulphurated liquor with lime if it contain carbonic acid,
and then I submit it to distillation in any manner competent to disengage
its ammonia nearly free from watery vapour, receiving the ammonia into
cold water, sometimes after first passing it through one or more baths of
caustic soda or potash in solution, with or without an intermediate bath of
fixed oil.
.
Another part of the Invention relates to the known application of sulphate
of ammonia to the production of sulphate of soda and muriate of amonia by
its action on common salt, and consists in an improved manner of operating.
Having mixed together about eleven parts by weight of dry sulphate of
ammonia and ten parts of dry salt, I subject the mixture to a decomposing
temperature as usual, but I substitute for the ordinary apparatus a heated clay
retort communicating freely with a lead or other chamber so capacious as to
remain cool enough to condense the vapours as they arrive in a state of flowers
or separate crystals instead of the hard cake ordinarily produced at a much
higher and less productive condensing temperature. When the vapours from
the charge cease, I withdraw from the retort sulphate of soda, and from the
chamber I obtain nuriate of ammonia, which I afterward dry if necessary,

page_text: and submit in any convenient manner to powerful mechanical pressure, and
thus form it into hard and dry cakes, fit to take the place in the arts of sal-
ammoniac, for which it may be made an economical substitute.
Another part of the Invention consists in adding about a chemical equivalent
of sulphuret of sodium to a waste residue obtainable in the making of chlorine,
and which consists chiefly of sulphate of manganese mixed with sulphate of
soda, the whole being in solution properly diluted with water sulphuret of
manganese precipitates, which being separated and exposed to the air
becomes oxidized, and of use as herein-before explained; from the solution I
obtain by evaporation sulphate of soda.
Having thus described the nature of my Invention and the, manner of putting
it into practice, I claim,-
Purifying gas by scrubbing or washing it first with raw ammoniacal liquor,
finally with water, and intermediately with the mixed products of those two
scrubbings or washings, subsequently to their desulphuration by any means,
either wholly or in part.
Purifying gas by passing it through three or more scrubbers or washers in
succession, the first being used with a solution of ammonia sufficiently free
from saturating acids to convert both, the carbonic acid and the sulphuretted
hydrogen of the gas into soluble salts, and the remainder in succession with
the same portion of water for finally washing out the ammonia and its
compounds, combining the alternate oxidation of hydrated sulphuret of
manganese by atmospheric air, with the use of the resulting compound for
the total or partial desulphuration of solutions containing hydro-sulphate of
ammonia.
Preparing a compound of iron or of manganese for desulphurating solutions
containing hydrosulphate of ammonia, or for purifying gas, or other useful
purposes, by decomposing a solution of any muriate of either of those
metals by means of sulphuret of calcium, or available mixture or compound
thereof, and afterwards exposing the precipitate to the air to become
oxidized.
Decomposing mixtures of sulphuret of sodium and a carbonate of ammonia
by heat in the absence both of fluidity and of temperatures high enough to
drive off the carbonate of ammonia undecomposed. Also the presence in such
mixtures, when submitted to decomposition by heat, of carbonaceous or other
suitable absorbent matter for enabling one or both of the reagents to be
added in solution without the prejudicial interferances of fluidity or pastiness.
Recombining the ammonia given off in the reciprocal decomposition
of sulphuret of sodium and a carbonate of ammonia with fresh carbonic acid,

page_text: whereby it is made serviceable for a repetition of the process many times in
succession.
Manufacturing solution or water of amonia more or less pure by receiving
into cold water ammonia distilled from liquor first deprived of sulphureited
hydrogen by revivifiable metallic substances, and also of carbonic acid, if
present, by lime, with or without an intermediate purification of the ammonia
during the distillatory process. Also the use of caustic solutions of soda or
potash and of fixed oil for the purification of ammonia gas on its way to
cold water, by which it is to be absorbed.
Distilling muriate of ammonia from mixtures of sulphate of ammonia and
common salt from earthen retoris into chambers for condensing the vapours
in detached crystals or flowers, and the consolidation into cakes of flowery
crystals of muriate of ammonia by mechanical pressure.
Obtaining as a precipitate hydrated sulphuret of manganese for oxidation by
atmospheric air by decomposing solutions of the mixed sulphates of manganese
and soda by sulphuret of sodium with the simultaneous production of sulphate
of soda in solution.
In witness whereof, I, the said Richard Laming, have hereunto set my
hand and seal, this Thirty-first day of May, in the year of our Lord
One thousand eight hundred and fifty-nine.
RICHARD LAMING. (L.S.)