IMPROVEMENTS IN OBTAIN- ING AND COMBINING AMMONIA
Year: 1855

page_text: LETTERS PATENT to Richard Laming, of Carlton Villas, Maida Vale, in
the County of Middlesex, for the Invention of "IMPROVEMENTS IN OBTAIN-
ING AND COMBINING AMMONIA,"
Sealed the 6th July 1855, and.dated the 24th January 1855.
PROVISIONAL SPECIFICATION left by the said Richard Laming at the
Office of the Commissioners of Patents, with his Petition, on the
24th January 1855.
I, RICHARD LAMING, of 36, Carlton Villas, Maida Vale, in the County of
Middlesex, do hereby declare the nature of the said Invention for "IMPROVE-
MENTS IN OBTAINING AND COMBINING AMMONIA" to be as follows:-
When the acid in sulphate of lime is used for extracting ammonia from gas,
I at once levigate gypsum in its native state, instead of first roasting it, or
substituting for it an artificial sulphate of lime. When a rotating sieve is.
used for intr :ducing into a gas purifier an acid or other liquid to extract
ammonia from gas, I keep the sieve in motion by causing the liquid to be
projected against a horizontal set of floats or vanes connected with it; and I
cause any liquid used for extracting ammonia from gas to flow over the surfaces
of successive shelves in gas purifiers, while the gas is made to flow over the
surfaces of the liquid in an opposite direction; or, which is better, I cause the.
liquid to be supported by the upward pressure of the gas on one or more
pierced diaphragms, and to overflow from them by hydraulic traps, the gas
being made to pass upward through the liquid by means of the perforations in
the diaphragms.

page_text: In using a continuous process for extracting ammonia from gas liquor or
other ammoniacal liquor, I heat one portion of the liquor before it enters the
extracting vessel by means of the vapours raised from a previous portion, and
having first extracted from the liquor its carbonate and other volatile salts of
ammonia, I then set free (by means of lime or magnesia, in a separate vessel
connected with the extracting apparatus,) the ammonia from such of its salts
as are not volatile. I combine ammonia by distilling it from gas liquor or
other ammoniacal material into an acid mixture of phosphate, by which it
becomes fixed.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Richard Laming in the Great Seal Patent Office on the
20th July 1855.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RICHARD
LAMING, of Carlton Villas, Maida Vale, in the County of Middlesex, send
greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twenty-fourth day of January, in the year of our Lord
One thousand eight hundred and fifty-five, in the eighteenth year of Her
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, 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
Islauds, and Isle of Man, an Invention for "IMPROVEMENTS IN OBTAINING
AND COMBINING AMMONIA," upon the condition (amongst others) that I, the said
Richard Laming, by an instrument in writing under my hand and seal,
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 1, 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 :-

page_text: One part of this Invention consists in extracting ammonia from coal gas bý
means of liquids in an improved apparatus, for the use of the original of which
in the purification of gas Alfred Vincent Newton obtained a Patent, dated the
Tenth of March, One thousand eight hundred and fifty-four. That apparatus
and the present improvement are constructed on the principle of Coffey's
still," well known for distilling alcohol,and for the application of which to the
distillation of ammonia William Edward Newton obtained a Patent, now in
my possession:
21
"
In order that the nature and extent of my improvement may be better
understood, I will before describing it first reproduce Alfred Vincent Newton's
description of his original gas purifier. "It consists of one or more horizontál
"shelves wholly occupying the area of a close vessel of any convenient form;
diameter, and material, and of suitable height. If there be more than one
shelf they should be placed a few inches apart. Each shelf should be pierced
with small holes for the passage of the gas upwards, and fitted with a pipe
projecting half an inch or so above its upper surface, and sealed at its lower
end by dipping into a cup of liquid. This pipe serves for the descent of all
the washing liquid which accumulates on the shelf to a depth greater than
necessary without allowing the gas to ascend by the same channel.
preferred to have as many shelves and layers of washing liquid as the gas can
overcome the resistance of, so that it may pass upward through the small
perforations without allowing the liquid to descend thereby. In using this
apparatus, the liquid enters in a small continuous stream at the upper part of
the vessel, distributes itself on the shelves; overflows into the pipes, and
descends by them to escape from the vessel through an inverted syphon at
its lower part. On the other hand, the gas enters foul below the undermost
shelf, ascends by the small holes through the washing liquid, and leaves the
"vessel near its top, being impelled by the expansion within the retorts or by
mechanical means.'
6:
"
It is
Now, my improvement consists in adding to each. of the shelves or.
diaphragms,above described, a somewhat smaller diaphragm, uupierced with
small holes, which I fix horizontally about an inch above it, to make tlie gas,
after it has ascended through the holes in the under diaphragms, pass horizon-
tally along the under surfaces of the blank diaphragms before it can emerge
from the liquid used to purify the gas, that liquid being maintained at a proper
depth by elevating the upper orifices of the pipes, by which it has to descend
about half an inch above the level of the unpierced diaphragms. The g is may.
be allowed to escape from between each two associated diapliragms at every
part of the edge of the upper one, or at certain parts only; for example, when

page_text: the upper diaphragm is circular, the gas may conveniently be allowed to escape
all round it; and if it be square, it may be convenient to let the gas escape only
at two of its opposite sides, which may be done either by turning the edge
downward at the other sides, or by fixing the diaphragm to two of the sides of
the vessel, it being supposed in that case to be square.. As the gas in its
horizontal passage has a tendency to drive the liquid before it from between
each pair of diaphragms, the upper one of each pair may be made with several
large holes, of about an inch or more in diameter, fitted with short pipes
turned downwards, so as to admit of the liquid on a diaphragm descending
through it without allowing the gas to ascend by the same apertures. The
small holes in the under diaphragms should be neither so numerous nor so
large as to allow the gas to pass through them with less rapidity than will pre-
vent the liquid passing in the opposite direction, and yet numerous and large
enough to let all the gas pass upwards without driving the liquid before it up
the drop pipes or hydraulic traps. Instead of or in addition to the second un-
pierced diaphragms, Isometimes adapt to each hole of the pierced diaphragms
a light valve with a spreading head. This arrangement, beside contributing to
the perfect distribution ofthe gas throughout the purifying liquid, facilitatesmy
making in each pierced diaphragm the extreme number of holes consistent
with a proper speed of the gas under the maximum make of winter without
too much diminishing the speed during the minimum make of gas in summer.
Tuse in this improved apparatus water,gas liquor, or other ammoniacal liquor,
which I prefer to introduce in a small continuous stream; there are also
intermitting methods sometimes recommended for introducing liquids into
ordinary scrubbers, and which may be substituted, but I consider them less
desirable. Sometimes I use an ammoniacal liquor on the lower diaphragms,
and finish the washing of the gas in the vessel by water used on one or more
of the uppermost diaphragms,in which cise the pipe for introducing the water
opens into the vessel above the top diaphragm, and another pipe for the
ammoniacal liquor opens between two of the diaphragms lower down.
Whether ammonia be extracted from gas by any diaphragm apparatus, by
ordinary scrubbing,or by the systematic use of a small quantity of water, or of
water and ammonia, in conformity to my process for purifying gas by making
ammonia serviceable thereto, and which is the subject of a Patent bearing date
the Thirteenth September, One thousand eight hundred and fifty-three, I
next treat it in common with the gas liquors from the condensers and solutions
of the volatile compounds of ammonia, from the distillation of animal matters,
or from a
any other
source, by a continuous process of distillation, in which the
portion of liquor about to enter the distillator vessel may be heated by means

page_text: of the vapours which have issued from a previous portion. The extracting
vessel is the same in form, and partly in arrangement, as that known as a
scrubber in coal gas works; but instead of receiving gas to be purified by a
liquid, my distilling scrubber is fitted up for receiving a liquid to be worked by
steam. For a large gas works it may be an upright cylinder, from 3 to 6 feet
in diameter, and about three or four of its diameters in height; its subordinate
parts are similar to those of Coffey's alcohol still, as patented by William
Edward Newton, for the distillation of ammonia; only that instead of numerous
diaphragms for distributing the steam and liquor,as that still has, this distilling
scrubber has but one diaphragm,and that one grated or pierced with large holes,
and used simply for supporting coke or other material used in scrubbers, and
to which the functions of the diaphragms are transferred. In using this still,I
distribute ammoniacal liquor over the upper surface of its charge of coke or
other material by means of a Barker's mill,a revolving sieve, or other suitable
contrivance, and I admit steam under the grated diaphragm in sufficient force
and quantity to strip the liquorofits volatile constituents on its way down to the
bottom of the still, the steam meanwhile ascending to escape,charged with the
volatile compounds of ammonia, by a pipe at its upper part, and by which they
are all conducted into a leaden apparatus, which may be formed by inserting
one vessel in another, filled to the depth of several inches with water,or acon-
centrated solution of sulphate of ammonia. Apipe, having its end closed, and
its inner portion pierced with small holes, distributes all the elastic products of.
the distillation below the surface of the liquid in the inner inverted vessel,
where they become deprived of ammonia by sulphuric acid, which is to be
admitted in a regulated stream by an invertedsy phon, for the purpose of con-
verting it into sulphate of ammonia as it arrives. The outer vessel is so much
larger than the inverted one as to leave room at one place for the solid
sulphate of ammonia to be ladled out from time to time, and to facilitate this.
the outer vessel is inclined downward at one end. The ammonia being this "
removed from the products of the distillation, then the steam and incondensible
gases may be allowed to e
escape out of the top of the inverted vessel, by a pipe
provided for that purpose,and which may be incased in another larger pipe,or
contained in a cistern, and immediately surrounded by the liquor destined to
enter the distillatory scrubber, which the steam will heat, becomingitselfinore
or less condensed, without any danger of obliterating the passages by the con-
cretion of ammoniacal compounds coudensible by cold. The noxious gases,
together with the condensed steam, may then be conducted to the furnaces to
be burned,or to oxide ofiron,for neutralizing their odour. Instead of sulphuric
acid, other suitable acids may be used for holding back the ammonia, due

page_text: provision being made for the preservation of the apparatus, in the case of any
particular acid, by a proper choice of materials used in its construction; and
instead of inverting one vessel within another,the apparatus may be made of
a close chest, on the principle of a common bird's fountain, only with a sloping
bottom, and with the sides of its trough reaching from the most depending
part of the bottom to near the top of the chest. For the distilling scrubber,
any of the continuous stills used with diaphragms for distilling ammonia, or,
indeed, any other form of continuous ammonia still, may be used with the
apparatus last described.
Ammoniacal liquor, as it accumulates at the bottom of the continuous still,,
whatever be its form or construction, often contains ammonia in a state o
volatile at the boiling temperature. When a sufficient quantity of such liquor
has accumulated, I let it out into a separate chamber incommunication both
with the still and with the boiler from whence the steam is derived, and
introduce to it as much lime or magnesia as will decompose the fixed
ammoniacal compounds, and then I turn the steam through the liquor on its
way from the boiler to the still. When a second sufficient quantity has
accumulated at the bottom of the still, I turn the steam direct into it from the
boiler by means of a bye-pass, and then, having discharged the separate vessel
of its expended contents, re-charge it and proceed to work.ás before.
Another part of this Invention relates to combining ammonia with acid
mixtures or compounds of phosphate of lime, and consists in fixing it, by
receiving it either alone or combined with other gases, immediately into contact
with the said mixtures or compounds as it becomes eliminated from ammoniacal
solutions or salts submitted to distillation. I use the phosphate of lime
dissolved or made sufficiently fluid by phosphoric, nitric, or hydrochloric acid,
and promote the chemical action by stirring whenever the nature of the mass
renders it necessary, and for so long a time as the ammonia continues to be
freely absorbed. When the ammonia is accompanied by noxious gases, and the
mixture with which it is to be combined is sufficiently fluid, the operation may
be conducted in a close vessel, fitted with an agitator, and with a pipe, for
carrying off the foul gases; but when odour is of no importance I prefer to
use an open vessel. When the absorption is complete the mixture may be
reduced to a solid state by evaporation and drying; or it may be mixed wet
with enough dry sawdust, breeze, boghead, ash, or other absorbent material to
facilitate its distribution as a manure. The latter mode of solidification is
particularly applicable when nitric acid has been used as the solvent, on
account of the peculiar properties of nitrate of ammonia at elevated tempera-
tures. What I prefer is, to dissolve bones, or other phosphate of lime, animal

page_text: or mineral, in hydrochloric acid, and then having used the compound to fix as
much ammonia as it well can to evaporate the product to dryness, which affords
highly concentrated manure, consisting of phosphate of lime of impalpable
fineness, combined with about an equal proportion of a powerful ammoniacal
salt.
a
Another partof this Invention relates to the extraction of ammonia from gas
by the agency of the sulphuric acid contained in sulphate of lime, and may be
put in operation in vessels known to coal gas manufacturers by the nanie of
dry lime purifiers. I will describe my mode of applying the Invention to coal
gas, and it may be applied in a similar mauner to gases generally at about the
ordinary temperatures, containing ammonia associated with carbonic acid.
Artificial sulphate of lime and burnt gypsum have already been applied for
extracting ammonia from gas: my Invention relates to improvements in the
way of using them, and also of advantageously using in their stead unburnt
gypsum. Any sulphate of lime used in a granular or minutely crystalline
condition acts either not at all, or chiefly by its surfaces, and hence incurs
waste of material. Any sulphate of lime used in a proper state offineness, and
mixed in small quantity with the inert material used with it to keep it
sufficiently pervious to the gas, produces only a weak ammoniacal mixture; and
if the fine gypsum be used in a proportion large enough to promise a mixture
rich in ammonia, then it is apt to form a hard cake in the purifying vessels,
and thus put a stop to the free passage of the gas. I begin by using finely
Levigated raw gypsum mixed with sufficient breeze, boghead, ash, or other
substance convenient for maintaining a passage for the gas through the
mixture, which I make damp, and put to work in the ordinary manner in dry
lime purifyers; I then take out the used material, levigate it, and replace it
lightly in the purifiers, to perform a second purifying operation; I repeat the
levigating and purifying. operations alternately with the same mixture a
further number of times, adding a fresh portion of gypsum whenever all that
has been previously added has become decomposed until I find by examination
that the used product is rich enough in ammoniacal salt to be satisfactory. At
the times when fresh additions of the fine gypsum are made to the mixture,
the levigating operations may be omitted. Instead of the usually cheap raw
gypsum, it may in some localities be economical to substitute for it the artificial
sulphate of lime, which is ocasionally to be obtained as a residue from chemical
manufacturies, or even burni gypsum may be substituted in this my improved
way of working. In certain districts mineral gypsum is so cheap that it may be
reduced raw to an impalpable powder by levigation, or elutriation, mixed with
a convenient proportion of some pervious and chemically inert material, and

page_text: submitted to a single operation on the gas with a satisfactory result, and in
this way I sometimes use raw gypsum as part of the present Invention.
I claim as new and useful, and as my Invention, first, the extraction of
ammonia from coal gas by the use of pierced and plain shelves or diaphragms,
so combined in pairs with a purifying vessel, that while the former serve by
their holes to distribute the gas through the mass of purifying liquid, the latter
serve by their resisting surfaces to prolong the submersion of the so-divided gas
without a corresponding increase in the depth of the purifying liquid; also
the extraction of ammonia from coal gas by the use of pierced shelves or
diaphragms in purifiers fitted with valves, in the manner described.
+
Secondly, the use of a scrubber,, as described, without diaphragms, for
extracting ammonia by a continuous process of distallation from solutions
containing it in a volatile state; also passing the volatile products emitted
from any continuous still working volatile compounds of ammonia into acid in
a fluid state, for combining the ammonia with the subsequent application of
the unabsorbed vapours to heat fresh portions of liquor about to enter thestill;
also the use of a separate vessel, connected by pipes with the distilling scrubber,
or any modification of Coffey's diaphragm still, for decomposing the fixed
compounds of ammonia contained in spent liquor by means of lime or
magnesia with the agency of steam on its way to the main apparatus.
Thirdly, combining ammonia-with acid mixtures, or compounds of phosphate
of lime, by bringing into immediate contact with them ammonia, as it or any of
its volatile compounds is eliminated from an ammoniacal solution or a salt
containing ammonia, and by which all intermediate operations are avoided.
Fourthly, the use of finely levigated raw gypsum for extracting ammonia
from gas containing it and carbonic acid, at any temperature low enough for
the
purpose; and also the repeated use, for the purpose last above mentioned,
of any mixture of sulphate of lime and inert matter, after either a new addi;
tion of the earthy'sulphate to the mixture or the application of a levigating
operation to break down in it the portion of sulphate of lime remaining
undecomposed.
In witness whereof, I, the said Richard Laming, have hereunto set my
hand and seal, this Twentieth day of July, in the year of our Lord
One thousand eight hundred and fifty-five.
RICHARD LAMING. (L.S.)