IMPROVE- MENTS IN OBTAINING ALKALIES AND ALKALINE COMPOUNDS
Year: 1859

page_text: LETTERS PATENT to Richard Laming, of Clifton Villas, Maida Hill,
West, in the County of Middlesex, for the Invention of "IMPROVE-
MENTS IN OBTAINING ALKALIES AND ALKALINE COMPOUNDS."
Sealed the 15th May 1860, and dated the 17th November 1859.
PROVISIONAL SPECIFICATION left by the said Richard Laming at the
Office of the Commissioners of Patents, with his Petition, on the 17th
November 1859.
I, RICHARD LANING, of Clifton Villas, Maida Hill, West, in the County of
Middlesex, do hereby declare the nature of the said Invention for "IMPROVE.
MENTS IN OBTAINING ALKALIES AND ALKALINE COMPOUNDS," to be as follows:-
A current of gaseous matter, composed, at least in part, of carbonate of
ammonia, or its acid and alkaline constituents, is forced through a close vessel
containing a porous mixture of sulphuret of sodium, water or its vapour in
small quantity being also present. From an opening in the vessel hydro-
sulphate of ammonia passes out in an elastic form, while solid carbonate
of soda remains behind in it to be obtained in a separate state by lixiviation
and evaporation. This part of the Invention may be modified by forcing a
current of air or other elastic medium through a porous mixture of sulphuret
of sodium and a carbonate of ammonia, in which case also the presence of
humidity favors the chemical action. The ammonia, which escapes as hydro-
sulphate, is next changed back again iuto carbonate, by being made to pass
[Price Sd.]

page_text: through a mass of red-hot carbonate of lime, and, when thus reproduced, the
volatile alkaline carbonate may be used for decomposing a fresh portion of
the sulphuret of sodium, or applied to other purposes. Or, the hydrosulphate
of ammonia from the close vessel may be received into impure coal gas, where
it will render soluble, in a little water judiciously applied, the impure acids of
the gas, at the same time that the carbonic acid with which it becomes in
part combined fits it for repeating, after its abstraction from the gas, the
decomposition of alkaline sulphuret, this reproduction of usefulness being due
to the property which N H3, H S has, under the circumstances, of becoming a
mixture of NH3, 2 HS, and 2 N H,, 3 CO₂, 2 HO. Lustead of discharging
the hydrosulphate of ammonia into foul gas in the form of vapour, it may be
condensed in water, and kept in stock as a liquid, to be applied to the gas in
scrubbers, as wanted. Or, its vapour, with or without atmospheric air, may
be forced through a porous mass of revivifiable oxide, which will keep back
its sulphretted hydrogen, and liberate its ammonia, in both which cases the
free ammonia may be obtained and applied to the gas in solution, or, when
unaccompanied by atmospheric air, let at once into the gas, to be afterwards
recovered by a skilful employment of a little water. For decomposing sul-
phuret of sodium in the presence of humidity, it is not necessary that the
ammonia and the carbonic acid be in particular proportions; the former may
be even altogether wanting, but the action will then be less energetic, and the
Invention, of course, stop short in its career of usefulness. Nor need the
carbonic acid so used be free from admixtures of carbonic oxide, atmospheric
air, or other gases with which it sometimes becomes diluted in economical
processes for its manufacture.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Laming in the Great Seal Patent Office on the
17th May 1860.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RICHARD
LAMING, of Clifton Villas, Maida Hill, West, in the County of Middlesex,
send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Seventeenth day of November, in the year of our
Lord One thousand eight hundred and fifty-nine, in the twenty-third year of
Her reign, did, for Herself, Her heirs and successors, give and graut unto
me, the said Richard Laming, Her special licence that I, the said Richard

page_text: 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, exercise, and vend, within the United Kingdom of Great Bri-
tain and Ireland, the Cha nel Islands, and Isle of Man, an Invention for
"IMPROVEMENTS IN OBTAINING ALKALIES AND ALKALINE COMPOUNDS," upon the
condition (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:-
This invention is based in part on the influence which atmospheres of
elastic matter have in promoting, by what is called diffusion of gases, certain
results of chemical affinity. Sulphuret of sodium in a humid condition may
be decomposed by carbonic acid simply brought into contact with it. I
decompose, by carbonic acid that sulphuret contained in a solid state within
a close vessel, furnished with induction and eduction pipes, by adding to the
condition of contact that also of an atmosphere, either of the decomposing gas
itself, or of some other elastic medium, which I force into or through the
vessel in a current, thus supplying the sulphuretted hydrogen which is given
off with something to diffuse itself into, thereby facilitating the decomposition
at ordinary temperatures or thereabouts, of the sulphuret into a carbonate of
soda,from which may afterwards be prepared the alkali soda or its marketable
compounds. It is known, that in the presence of free oxygen, the sulphur
of sulphuret of sodium has a tendency to become oxidized, and that such
oxidation prevents the due effect of the carbonic acid, therefore I prefer to
have the carbonic acid uncontaminated with oxygen gas when first obtained,
or, at least, to render it free from that impurity before I use it; and, for the
same reason it is better that the heated vessels or furnaces in which the
sulphuret of sodium is, made, for the purposes of this Invention, exclude
the atmospheric air, in order that no part of its sulphur become re-oxidized
during the process of manufacture. For the conversion of solid sulphuret of

page_text: sodium into carbonate of soda, it is desirable that water or moisture be
present in sufficient quantity to oxidize the sodium and hydrogenize the
sulphur, a condition that may be established by causing enough vapour to
accompany the carbonic acid, or, in the absence of sufficient vapour, by
making the sulphuret damp, and which is always to be borne in mind
throughout this Specification, though it may not be expressed on each
recurring occasion. Forty parts of the sulphuret require nine parts of the
elements of water; but the latter may be present in larger proportion.
In those soda factories in which hydrochloric acid is a waste product, it
may, by its well-known action on carbonate of lime, be made to supply carboric
acid free from oxygen gas, for the purposes of this Invention; or it may be
obtained by exposing to a red heat in close vessels bitter spar or dolomite.
Carboric acid may also be made by the combustion of carbon in atmospheric
air, in which case the residue of oxygen gas which it will generally contain
should be removed. I effect that removal in the following manner, by means
of some known contrivance, such as a pumping or blowing machine, or a
chimney draught; I force the gaseous products of combustion from an ordinary
furnace or other place for burning in atmospheric air, carbonaceous matters,
with or without limestone, first through a long iron pipe exposed to the air or
otherrefrigeratory convenient for cooling them down to near the atmospheric
temperature,and then through a close vessel charged with a larger quantity of
artificial hydrated sulphuret of iron than they can oxidize, the said sulphuret
having been previously made pervious to the passing gases by a due admixture
of sawdust or other suitable material. The vessels used for containing the
metallic sulphuret may be like those known in gasworks under the name of
dry purifiers; within them the oxygen becomes arrested, and the metal of the
sulphuret changed into an hydrated oxide, provided only that the temperature
be not allowed to rise too high.
A current of elastic matters containing carbonic acid without admixture of
atmospheric oxygen may be obtained by and used during the combustion that
produces sulphuret of sodium. For this purpose, sulphate of soda and about
one-third or one-fourth of its weight of coal or coke, or other form of carbon,
both in fine powder,having been intimately blended together, may be submitted
to a red heat in a close retort, having its eduction pipe in direct communi-
cation with the vessel containing the sulphuret of sodium to be decomposed.
The products of combustion freed froin oxygen, as above described, or car-
bonicacid otherwise obtained, together with any unobjectionable matters that
may accompany it, I conduct into the vessel containing the sulphuret of
sodium, the mass of which it should freely penetrate; and to provide for its

page_text: doing so, I use the alkaline sulphuret diffused through a sufficient proportion
of carbonaceous or other suitable matter. I prefer to use it as it presents
itself when made into a porous mass, by calcining in a close vessel sulphate of
soda intimately mixed with about halfits weight of coal or coke. The carbonic
acid of the current converts in a rapid and satisfactory manner the solid sul-
phuretofsodium into a compound of soda and carbonic acid, with the liberation
of sulphuretted hydrogen, which I either arrest by receiving it into a gas dry.
purifier, or other convenient vessel. charged with revivifiable oxide of iron,
made pervious by sawdust or other suitable matter, or burn in the way well
known for making sulphurous or sulphuric acid, or use or get rid of by other
means. When the conversion of the sulphuret of sodium is complete, a fact
indicated by the porous mass ceasing to give off sulphuretted hydrogen, I
remove it from the vessel and obtain from it,by lixiviation with hot or cold
water, a solution that affords by evaporation and c: ystallization salts of soda
of good quality, or by evaporation to dryness excellent soda ash, alkali, or
carbonate of soda, or by treatment with lime a nearly pure solution of caustic
soda.
The elimination of sulphuretted hydrogen from sulphuret of sodium, by the
agency of carbonic acid, may be made conducive to a supply of the latter sub-
stance for repeating the elimination, by conducting the former; gas into a mass
of red hot carbonate of lime contained in a close retort heated from the
outside. The sulphuretted hydrogen as it arrives changes the carbonate of
lime into sulphuret of calcium, carbonic acid gas being given off to be
conducted by the eduction pipe into the sulphuret of sodium.
But as a source for the current of carbonic acid and other elastic matters
to be used for decomposing sulphuret of sodium I prefer the ordinary con-
densed liquoriof gasworks and the ammoniacal washings of coal gas and other
cheap liquors containing carbonate of ammonia; because, while the current
they furnish is eminently effective in causing the decomposition, it at the same
time, yields the volatile alkali or some of its compounds in addition to the alkali
which is fixed. To obtain from them the elastic current I submit the liquors
to a continuous process of distillation in some efficient form of apparatus,
such, for example, as the square tower or column, known as the Invention of
Eneas Coffey, for the distillation and rectification of alcohol, and which, when
made of iron and somewhat modified to adapt it to ammoniacal liquors, I use
in preference to all others. To modify Coffey's distillatory apparatus for the
purposes of this Invention, the small holes in its diaphragms should be sup-
pressed, and one edge of each of them cut away to the extent of several
inches at two opposite sides of the tower alternately, so as to open up a long

page_text: serpentine or zig-zag passage for the fluid matters throughout the whoe of
theapparatus, instead of leaving one part of it divided into separate chambers.
The edge of each diaphragm or plate where cut away may be turned up a
little to keep back a shallow head of liquor, which by this arrangement is
made to cascade from one plate to another until it flows out at the lower end
of the series. The ammoniacal liquor distilled in such an apparatus, as it
flows and falls in contact with steam passing in an opposite direction, gives
out a constant supply of carbonic acid of ammonia, and generally also of
suphuretted hydrogen mixed with aqueous vapour; while the steam which is
perpetually entering below to effect the distillation may be so regulated in
quantity, as to become almost wholly condensed and thrown back by its
contact with the worm through which the cold liquor to be distilled continually
enters the apparatus at its upper part, so that very little of it shall pass out
with the volatilized ammonia by the eduction pipe. The steam is in proper
quantity when the pipe just named has somewhat more than the lowest degree
of heat that suffices to prevent the ammoniacal compounds from con lensing
within it, the rule being to maintain it at a temperature so high that the
unprotected hand will hardly bear to remain upon it As the elastic matters
make their exit in a continuous stream, from either this or any other suitable
distilling apparatus, without too much accompanying vapour,1 receive them
into the vessel charged with sulphuret of sodium, where the carbonic acid
produces carbonate of soda, the sulphuretted hydrogen as it arrives adds itself
to that portion of the same gas which the carbonic acid liberates, and the
introduced ammonia serves the good purpose of promoting the liberation by
giving the sulphuretted hydrogen something to expand into and chemically
combine with. On this last account when ammonia gas can be cheaply ob
tained, it may be desirable to use it generally as one of the ingredients of
the decomposing current, even when the above named liquors are not the
source of the necessary carbonic acid; but in all such cases care must be
taken to have in the passages through which the ammoniacal compounds
pass a sufficient quantity of watery vapour, together with an adequate
temperature to maintain them in an elastic state. The ammonia being
commercially valuable needs to be afterwards recovered, which may be
done in various ways, as, for example, by receiving it as it leaves the soda
vessel into diluted sulphuric acid, or when it is combined with only a
single chemical equivalent of sulphuretted hydrogen into foul coal gas, or
into cold water that may afterwards be used to wash or scrub such
gas, the
acid impurities of which it will combine with, or in other ways, some of
which will be herein-after mentioned.

page_text: By a Patent bearing date the 1st of December 1853 I made knowa a
process for decomposing a porous mixture of sulphuret of sodium and car-
bonate of ammonia by the elasticity conferred by slightly heating the mass; I
now improve upon that process by putting such a mass into a close vessel, and
forcing in by an induction pipe a current either of vapourorothernnobjection-
able matter in an elastic form, such, for example, as carbonic oxide or atmo-
sphericnitrogen, or even carbonic acid or ammonia, whatever is not condensed
passing out of the vessel by an eduction pipe. When vapour is abundantly
used to establish a current for the purposes of this Invention, the temperature
of the decomposing mixture should, by means externally applied, be main-
tained high enough for the vapour not to condense in the soda vessel; and
when nitrogen for the current is obtained from the atmosphere, it should be
deprived of oxygen by being made to traverse through an adequate quantity
of artificial hydrated sulphuret of iron or manganese.
I sometimes recover the used ammonia in combination with carbonic acid
derived from a heated earthy carbonate. For this purpose I prefer that it
leave the soda vessel accompanied by not less than one and a half equivalents
of sulphuretted hydrogen, which will generally be the case when the current is
originated by the distillation of liquors containing hydro-sulphate of ammonia.
I conduct the mixed gases by an eduction pipe into a close retort charged
with pieces of magnesian, or ordinary limestone, or chalk, exposed to a full
red heat, by which means I set carbonic acid free, and cause it to pass, along
with the ammonia, through an eduction pipe into an ordinary lead chamber,
in which the two gases condense together as carbonate of ammonia. When
the proportion of ammonia would otherwise be unduly large, the chamber in
which the condensation takes place may advantageously be maintained full of
carbonic acid obtained from some additional source. Or the carbonate of
ammonia as it leaves the retort may be dissolved in water by what is known
in gasworks as a water scrubber, or by other apparatus..
At other times I recover the ammonia in an uncombined state, by receiving
the gases from the soda vessel into a gas dry purifier or other appropriate
vessel, charged with a revivifiable oxide of iron or manganese, made pervious
by sawdust or other suitable matter, by which the sulphuretted hydrogen.
which is present is absorbed, and the ammonia set free. In this case it is
desirable whenever the elastic matters leave the soda vessel hot to cool them
down to near the atmospheric temperature by causing them to pass on their
way to the metallic oxide through an air or a water refrigoratory. The used
oxide may be recovered for a repetition of this service by employing it to
deprive of accompanying oxygen either carbonic acid or atmospheric nitrogen.

page_text: for the purpose herein-before mentioned, · rby atmospheric revivification
practiced in any approved manner. Revivifiable oxide of iron is abundantly
supplied for purifying cool gas as made for that purpose by decomposing
copperas by lime; it is unavoidably diluted with about double its weight of
sulphate of lime, which not only itself occupies room in the purifiers, but also
renders necessary a greatly increased volume of sawdust for making the mass
porous. For my Invention I prefer hydrated and precipitated peroxide of iron
made without sulphate of lime by one or other of the following processes: -
1. By exposing borings, turnings, and other small pieces of iron until their
conversion into oxide is complete to the consecutive influencesofsulphuretted
hydrogen gas and atmospheric oxygen. The sulphuretted hydrogen used may
be that liberated by the decomposition. of sulphuret of sodium, or hydro-
sulphate of ammonia distilled from gas liquor or gas washings; and it may be
applied to the metal by enclosing the latter in vessels, through which the
sulphuretted hydrogen is made to pass. The oxidation of the resulting
sulphuret of iron may be done by establishing atmospheric contact in any
convenient manner.
2. By decomposing solutions of sulphate of iron, particularly those cheap
ones obtained in the pickling of iron for the manufacture of tinned plates, and
in the precipitation of copper by iron from its native combination with
sulphuric acid, by means of either sulphuret of sodium or magnesia, and by
afterwards exposing the washed precipitate to the air to oxidize. Calcined
magnesian limestone may be substituted for the last-named precipitating agent
but in that case the precipitate will not be so free as is desirable from sulphate
of lime; or by decomposing first the same iron sclutions by chloride of
calcium, and secondly, the resulting protochloride of iron by lime, with
subsequent oxzidation of the washed precipitate by exposure to the atmosphere.
In all these cases useful matters are recoverable for repeating the processes.
3. By calcining together at a red heat for two or three hours equivalent
proportions of an unrevivifiable oxide of iron and carbonate of soda, or by
keeping at a boiling point equivalents of the oxide and caustic soda in strong
solution until they chemically combine, and then in either case throwing down
the oxide in a revivifiable condition by dissolving out the alkaline base with
warm water. Sometimes a cheap unrevivifiable oxide for this purpose results
from the roasting of iron pyrites by manufacturers of oil of vitrol,and one may
be economically made from oxide of iron material which has become charged
with sulphur, by repeatedly absorbing sulphuretted hydrogen with alternate
exposure to the air, as in the ordinary practice for purifying coal gas by oxide
of iron. The charged oxide mixed with sawdust or breese being put into a

page_text: kiln, the carbonaceous matters may be ignited and fed with atmospheric
oxygen from below, as in the making of lime. Astheir combustion progresses
the sulphur above will be sublimed in a state of vapour,and may be condensed
in a cool chamber communicatingwith the dome of the kiln, leaving the oxide
behind in an unrevivifiable condition; or sulphur may be driven out from a
porous mass of the charged oxide into a chamber by forcing through it air or
other gases or vapour heated to 180 or 212 degrees of Fahrenheit, in which
case the oxide will be recovered in a condition more fit for absorbing
sulphuretted hydrogen, independently of its being combined with and pre-
cipitated from soda. Revivifiable oxide of iron undiluted with sulphate of lime -
may also be made more or less economically by other well known processes.
I sometimes absorb into cold water the free ammonia as it leaves the oxide
vessel in which it has been divested of sulphuretted hydrogen. For this
purpose I employ one, or, in preference, a set of close scrubbers, in the whole
of which the same water is used consecutively until it has become satisfactorily
rich in ammonia, beginning with that scrubber which is most distant from the
oxide vessel, and which I make to communicate with the atmosphere at its
upper part. Or I cause the water which is to absorb the free ammonia to pass
in a zig-zag direction over a number of horizontal trays or shelves, arranged
near to, and almost completely over, one another in a close vessel into which
they are fitted, so as to cause the water to fall from one tray or shelf to another
from the top of the apparatus to the bottom a sufficient number of times to
absorb all the ammonia gas, which entering below is constrained to pass
between the trays or shelves in the contrary direction in order to ascend. To
facilitate this absorption the ammonia gas should be cold, arriving through a
worm or other close refrigoratoryif necessary. The extent of absorbing surface
can hardly be too great, especially if a large quantity of ammonia be required
to be absorbed by a small quantity of water; and in case there should be
accompanying the ammonia any gas unsusceptible of absorption a vent is left
at the upper part of the apparatus for its escape. At other times I conduct
the free ammonia in an elastic state into impure gas, to combine it in great
part with the carbonic acid which the gas contains; and I afterwards by
washing or scrubbing the gas with water recover it in solution so combined for
further use in decomposing sulphuret of sodium, as herein-before described, or
for other purposes.
I obtain compounds of the volatile alkali in the following mauner:-I wash
a current of foul coal gas in three ordinary scrubbers, or sets of scrubbers used
consecutively, the middle scrubber, or middle set, serving to scrub the gas
with water containing ammonia uot fully saturated, for example N H,, or

page_text: NH3, Co₂, or N H₂, H S, or a mixture of two or more of them; and the
first scrubber, or first set, being made to scrub the gas on its first arrival in
the series with water which has already been applied to the current in the
third scrubber, or third set, in such quantity as to prevent any of the ammo-
niacal compounds from-passing with the gas out of the series. If sets of
scrubbers are used instead of single ones, I cause the liquor used in each set
to enter each scrubber of its own set in consecutive order, beginning with that
through which the gas passes last. When the liquors used are in sufficient
quantities, all the carbonic acid of foul gas may be obtained from it as a
solution of ammoniacal carbonate, but to ensure that result it is desirable to
have as much unsaturated ammonia introduced by the middle scrubber, or set
of scrubbers, as will enable the water used in the third scrubber, or set, to
deprive the gas of all its sulphuretted hydrogen also in the form of a hydro-
sulphate of ammonia.
Having described the nature of my Invention, and how it maybe performed,
I proceed to state my claims in respect thereof; I claim,-
Firstly, making carbonate of soda by forcing into or through a solid mass
containing sulphuret of sodium a current of carbonic acid gas, with or without
other accompanying elastic matters that permit of the formation of the fixed
alkaline carbonate. I do not claim the condition of solidity without the simul-
taueous influence of the current, nor the latter without the former.
Secondly, making simultaneously hydrosulphate of ammonia and carbonate
of soda by forcing into or through a solid mass containing sulphuret of
sodium a current of elastic matters that permit of the formation of the two
alkaline compounds, carbonic acid and ammonia also being present, either in
the solid mass or in the current passing through it. I claim neither the con-
dition of solidity nor of the passing current when used separately; the claim is
for the combination of the two.
Thirdly, making free ammonia by the distillation of gas liquor or gas
washings, or similar liquors, and causing it with the carbonic acid and sulphu-
retted hydrogen, which the liquor gives off, to pass in an elastic current,
accompanied by a little vapour of water, through sulphuret of sodium, and
afterwards through a revivifiable oxide of iron or mangenese.
Fourthly, making solution of ammonia eliminated by distillation from gas
liquor or gaswashings or similar liquors, or by decomposing a mixed solid mass
containing sulphuret of sodium, ammonia and carbonic acid being present, by
absorbing it after it has been freed by any known means from accompanying
sulphuretted hydrogen and carbonic acid into a stream of water, flowing or
falling in contact with it and in an opposite direction.

page_text: Fifthly, the application in the decomposition of sulphuret of sodium into
carbonate of soda by a current of carbonic acid of artificial hydrated sulphuret
of iron to reinove accompanying oxygen gas from the carbonic acid itself, or
from any gaseous substance mixed or to be mixed with it for use.
Sixthly, making carbonate of ammonia, solid or in solution, by causing a
current of hydrosulphate of ammonia, or of mixed carbonic acid and am-
monia gases, to decompose red hot carbonate of lime, or carbonates of lime
and magnesia, and by receiving the volatile products of the decomposition
into suitable condensing apparatus.
Seventhly,obtaining impure solution of carbonate of ammonia by scrubbing
or washing impure coal gas lastly with pure water, firstly with the product of
that water washing, and intermediately with either the joint products of the
last and first water washings subsequently to their desulphuration either
wholly or in part, after being mixed with the raw ammoniacal or gas liquor
from the condensers and mains, or with water containing unsaturated
ammonia from other sources.
In witness whereof, I, the said Richard Laming, have hereunto set my
hand and seal, this Seventeenth day of May, in the year of our Lord
One thousand eight hundred and sixty.
Witness,
CHABLES SMITH,
8, Glos'ter Street,
Regents Park. N.W.
RICHARD LAMING. (Ls.)