IMPROVEMENTS IN THE MODES OF OBTAINING OR MANUFACTURING SULPHUR AND SULPHURIC ACID
Year: 1848

page_text: TO ALL TO WHOM THESE PRESENTS SHALL COME, I, RICHARD
LAMING, of Chichy la Garenne, near Paris, in the Republic of France,
Chemist, send greeting.
WHEREAS Her present most Excellent Majesty Queen Victoria, by
Her Royal Letters under the Great Seal of Great Britain, bearing date
at Westminster, the Fourth day of September, in the twelfth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me,
the said Richard Laming, Her especial license, full power, sole privilege
and authority, that I, the said Richard Laming, my exors, adññiors, and
assigns, and such others as I, the said Richard Laming, my exors, adiñors,
or assigns, should at any time agree with, and no others, from time to
time and at all times during the term of years therein mentioned, should
and lawfully might make, use, exercise, and vend, within England, Wales,
and the Town of Berwick-upon-Tweed, and in all Her Majesty's Colonies
and Plantations abroad, and in the Islands of Jersey, Guernsey, Alderney,
Sark, and Man, my Invention of "IMPROVEMENTS IN THE MODES OF OBTAINING
OR MANUFACTURING SULPHUR AND SULPHURIC ACID;" in which said Letters
Patent is contained a proviso, obliging me, the said Richard Laming, by an
instrument in writing under my hand and seal, particularly to describe and
ascertain the nature of my said Invention, and in what manner the same
is to be performed, and to cause the same to be enrolled in Her Majesty's
High Court of Chancery within six calendar months next and immediately
after the date of the said in part recited Letters Patent, as in and by the same,
reference being thereunto had, will more fully and at large appear.

page_text: NOW KNOW YE, that in compliance with the said proviso, I, the said
Richard Laming, do hereby declare that the nature of my said Invention, and
the manner in which the same is to be performed, is particularly described
and ascertained in and by the following description thereof, reference being
had to the Drawings hereunto annexed, and to the letters and figures marked
thereon (that is to say):-
The part of this Invention which relates to improvements in the manufac
ture of sulphuric acid is as follows:-I take pumice stone (other porous
bodies which will not be destroyed by the processes to which they have to be
submitted may be substituted, with more or less effect) and I boil it in con-
centrated sulphuric acid; having drained off the acid, I next immerse the
pumice stone in a little water containing ammonia, which may be in the
proportion of about twenty per cent. I next dry the pumice stone and put it
into a retort with about one per cent. of peroxide of manganese; the retort
being now closed, I gradually raise its temperature to near 600 degrees
Fahrenheit, and when this is attained I withdraw the fire by which I heated
the retort, and leave it to cool without admitting the atmospheric air to the
prepared pumico stone. Other modes of preparing pumice stone or other
suitable porous bodies may be substituted with a certain amount of effect for
that which I have described; for example, it may be boiled in sulphuric acid,
and then immersed either in nitric acid or a solution of an alkaline nitrate, or
it may be boiled, or simply immersed in a mixture of sulphuric and nitric
acids; but according to my observations the mode I have first described is the
preferable one.
I do not claim as my Invention the application of porous bodies generally
for making sulphuric acid by means of their catalytic energy, as platinum has
been already used for such a purpose; but what I do claim is, the invention of
the use of pumice stone and other cheap porous bodies in conjunction with
ammonia, as herein-after explained, and also the modes which I have de-
scribed, however they may be combined, for endowing such bodies with
increased catalytic energy.
In order to make sulphuric acid by the catalytic agency of porous bodies
prepared as I have described, I prefer to expose them in long narrow
passages to a current of sulphurous acid gas mixed with a due proportion
of atmospheric air and a minute quantity of ammonia gas, the said passages
for the most part containing also water, or the vapor of water, with which
the sulphuric acid may combine.
I will now describe an apparatus which I have devised for carrying out the
principles of my Invention, and which I claim, not only for the more imme-

page_text: diate purposes of the said Invention, but also as offering advantages under
the ordinary process for making sulphuric acid, which are not afforded by
lead chambers. Among these advantages are economy in space, in original
cost of apparatus, and in wear and tear.
In the accompanying Drawings Fig. 1 is a vertical tubular magazine of
sheet iron for containing the catalytic substance, the portion between A and B
forming part of the main conduit for the gases. A is an iron pipe, bringing
the mixture of sulphurous acid and atmospheric air from the sulphur furnace,
which may be of an ordinary kind, and B is a pipe also of iron, leading to the
subsequent parts of the apparatus. The ends of A and B are formed into
jackets which surround the tubular magazine and communicate with it by
incans of a great number of holes made in the vertical magazine, so small as
to prevent the catalytic substance from passing through them, at the same
time that they freely allow the passage of the gases. The top of the magazine
is closed by a moveable plate or door, and to its lower end is adjusted a
register, by which the magazine may be emptied of its contents. The maga
zine is divided by three other registers D, D', and D³, into four compartments,
the two middle compartments being always in communication with one another,
so far as the gases are concerned, by means of apertures made in the inter-
vening register D'. This contrivance enables a workman, by withdrawing the
registers in succession, beginning below, to remove at any time a determinate
quantity of the catalytic substance when its energy shall be expended, and
to supply its place by fresh catalytic substance contained in the magazine,
without either arresting the work or admitting a current of cold air to the
apparatus. The syphon pipe and stopcock E serve to introduce gradually
into the pipe A from an elevated vessel a small quantity of ammonia dissolved
in water. The ammonia should amount in a given time to about one part to
every thousand parts of concentrated sulphuric acid made during the same
period. I prefer to use the ammonia in a caustic state, but it may be used
combined with either sulphuric or carbonic acid. That portion of the tubular
magazine which makes part of the main conduit should be inclosed in a flue
or a furnace, so as to admit of being thereby heated at the commencement of
the operation to 550 or 600 degrees Fahrenheit, such a temperature being
found conducive to the catalytic action.
5 Fig. 2 is a view of one of four rows of columns F, shewn in elevation and
partly in section, with a cistern G, also in section, upon the cover of which
two rows of columns are supported, which columns are each brought into
connection with their cistern by means of short tubes in the cover thereof.
Fig. 3 is a plan of two similar cisterns, with their four rows of columns

page_text: standing in hydraulic joints. The longitudinal division a, represented by
dotted lines running along the middle of each cistern, has the effect of sepa-
rating it into two parts which communicate with each other at one end of the
cistern. b, b, Fig. 2, are transverse divisions fixed to the cover and sides of
the cistern, and reaching nearly to the bottom thereof, so that when the
cistern is supplied with liquid they will, by forming water-tight joints, so
intercept the passage over the surface of the liquid contents of the cistern that
the gases which arrive by the pipe B, and descend the column F¹, will, instead
of passing along the cistern from one end to the other, ascend the column F³,
pass along the connecting pipe at the top thereof, down the colunin F³, and
up the column F', and so on through the whole series. From F the gases
pass by the cistern into F¹ (Figure 3), and arriving at the end of the second
row of columns, they quit F 22 by the pipe at its upper end, and enter the third
row of columns F 23, proceeding in like manner through the two rows of
columns of the second cistern. Those of the gases which are incondensible
finally quit the fourth row at F 44, passing out at its top to enter a curved
pipe which conducts them into a leaden chest H for condensing the vapor, and
which chest, in its turn, communicates by an asceuding pipe fitted to one of
the two openings in its cover with a chimney, the draft of which is sufficiently
powerful to maintain a current throughout the whole conduit, of which each
column forms a part.
Figures 4 and 5 shew on an enlarged scale the internal arrangement of the
columns, in which I, I, I, I, I, I, represent the flat basins destined to be filled
with the catalytic substances, and serving also to keep back part of the water,
which enters each column in a slender stream by overflowing the hydraulic
joint at its summit, and which becomes a solution of sulphuric acid, more or
less strong as it is nearer to or farther from the pipe B. The water is brought
to the hydraulic joints by small pipes and stopcocks, not shewn in the Figure,
and it falls in each of the columns from basin to basin, thus successively
washing the porous bodies contained in them, and thereby acquiring sulphuric
acid, until, arriving at the base of the column, it overflows the hydraulic joint
at that place, and falls into the cistern below. As the columns of the lowest
numbers condense the largest quantities of sulphuric acid, it follows that the
liquid in the cistern at the base of the columns is more concentrated
as it is nearer to the cock k, by which it runs off into a common reser-
voir constructed as near as possible to the said cock, but not shewn in
the Figure. The weaker acid furnished by the columns of the higher
numbers becomes progressively stronger as it flows towards the cock K,
where it requires its. maximum of strength. To keep back the weak

page_text: acid from prematurely mixing with that which is stronger, transverse divi-
sions c, c, are provided in the cisterns G. These divisions are half the
height of the cisterns, and are fixed to its bottom and sides in such a way
as to form a compartment below each pair of columns. This arrangement
prevents the products of the columns of higher number from mixing with the
product of that of lower numbers, except by an overflow caused by the accu-
mulation of liquid. The cisterns G are constructed of wood lined with lead,
and the columns may (some or all of them) be made of this latter material,
but I prefer making nearly the whole of them of stone ware, as it is less
expensive and not subject to corrosion. On account of the high temperature
of the gases, as received by the column F' from the pipe B, and from the
consequent exposure of that column to atmospheric changes, it is desirable to
construct the said column F¹ of lead; and if the apparatus be intended to
work quickly, even one or more of the succeeding columns should also be
made of lead, or, what will answer the same purpose, F 1 may be of large
dimensions. The body of each column consists of several tubes put together
by hydraulic joints. The forty-four columns alluded to in the Figures, each
being two feet in diameter, by ten feet high, are competent to the daily pro-
duction of twenty-two hundredweights of concentrated sulphuric acid, and,
provided the sulphur furnace be properly constructed, the proportion of sulphur
necessary for this quantity will hardly exceed seven and a quarter hundred-
weights. It is convenient to erect the columns with the cisterns at their base
on the first floor of a building, and in that case the sulphuric acid may be
received from the cock K, into a reservoir close under the floor, which will
admit of its being concentrated during its descent to the ground.
Fig. 6 is a vertical section of one form of apparatus which I have invented
for concentrating sulphuric acid, and which enables me to supersede the ordi-
nary stills of platinum. It consists of a column made of stone ware or
porcelain tubes, cemented together with fire clay, and fitted interiorly with a:
number of horizontal diaphragms L, which each rest on ledges in the tubes,'
and have each a large hole in their centre. Between every two diaphragms
there is placed a table M, somewhat smaller in diameter than the diaphragms,
and supported horizontally thereon by feet, as shewn in the Figure. Both
the diaphragms and the tables are constructed with raised edges, which enables
each of them to retain on its upper surface a stratum of acid about an inch in
thickness. A syphon funnel N serves to introduce the weak acid through the
cover of the column, and to deliver it upon the uppermost diaphragm, whence
it falls from diaphragm to table, and from table to diaphragm, until, the
whole series being covered with it, the excess falls upon the hemispherical

page_text: guard O, and then into the bottom of the column, there rising to a level with
the highest part of the platinum syphon P, the end of which is inserted in the
column, and concentrated acid runs out; and having thus once filled the
syphon, it afterwards maintains its level within the column at the height of
the external orifice of the platinum tube. In the bottom of the column there
is an opening Q, destined to admit air heated in any ordinary manner to a
temperature sufficiently high to boil the weak acid on the diaphragms and
tables; and at the upper part of the column there is a corresponding
opening R, by which the vapours generated, together with the air which
generated them, pass out, the former to be condensed in any known manner,
or the whole to enter one of the columns F, which particular column should
be of lead, on account of the high temperature thus introduced into it.
Instead of heated atmospheric air, other heated gases, such, for example, as
the products of combustion, may be used in the concentrating column, but in
such a case the pipe R cannot be made conveniently to communicate with the
series of columns, F, as the gases might interfere with the sulphuric acid
process. When air is used, it need not be driven through the concentrating
apparatus, as the draft existing in the scries of columns F, with which it may
be in communication, will serve to draw into it the air from the pipes in
which it has been made hot. In order to protect the column from sudden
changes of temperature, and also to economize heat, it requires to be
surrounded by a jacket of masonry or other bad conductor of caloric. Instead
of passing heated air or gases through the concentrating apparatus, the orifice
at its bottom may be closed and the column packed in sand in a large cylinder
of iron, the whole apparatus may then be surrounded by a furnace or fluc.
In this way the heat necessary for the concentration would be supplied to the
acid from the outside through the iron, the sand, and the cylinder of earthen-
ware. Or, instead of a column, a long continuous pipe of stone ware or
porcelain, or a series of pipes of such materials and of any convenient form
and arrangement, may be used, and the heat applied in either of the two
ways I have just described, that is to say, either by heated air or other gases
ascending in the inside of the conduit and sweeping over the surface of the
acid, descending in a slender stream in an opposite direction, or by hot gases,
or sand, or other substance applied to the external surface of the conduit.
In either case the process would be virtually the same as that for which I
prefer to use the concentrating column.
What I claim as my Invention with regard to the concentration of sulphuric
acid is, the passing it in a slender stream, or the spreading it in a thin stratum,
having progressive motion over surfaces of earthenware, so arranged that the

page_text: acid comes into contact with surfaces more highly heated as it becomes itself
more highly concentrated.
And I further claim the peculiar construction of concentrating apparatus,
as shewn and described with reference to Fig. 6 of the Drawings.
When the apparatus herein-before described is to be applied to the old
process for making sulphuric acid by aid of nitric acid, the tubular magazine,
Fig. 1, should be suppressed, and its place supplied by a column, such as is
represented in Fig. 6. The opening Q, Fig. 6, should be put in communi-
cation with the pipe A (Fig. 1) which brings the sulphurous acid gas and
atmospheric air from the sulphur furnace; and the pipe R, Fig. 6, should
be in correspondence with the column F1. The cock K, by which the acid
leaves the cisterns at the base of the columns, should be made to discharge
itself continually into the syphon funnel N, from whence it will find its way
down over the tables and diaphragms, to escape by the platinum syphon P
into the reservoir prepared to receive it. The nitric acid may be
introduced into the apparatus in the ordinary manner, or mixed with
the water which enters by the hydraulic joints at the summit of the columns P;
but it will be needed in less quantity than usual, on account of the difficulty
which this arrangement of apparatus opposes to the escape of the oxides of
nitrogen. I would remark that the pipe K, and also the concentrating
column (both of which are composed of earthenware), should be protected
from atmospheric changes, by enclosing them in some substance which is a
bad conductor of heat.
The part of this Invention which relates to improvements in making or
obtaining sulphur is as follows:-In saturating the ammoniacal liquor of
gas works by a mineral acid, as is practised for making sulphate and muriate
of ammonia, large quantities of sulphuretted hydrogen are set free, attempts
have been made to burn this sulphuretted hydrogen instead of sulphur in the
manufacture of sulphuric acid, but without success, on account of the large
proportion of incombustible carbonic acid which escapes from the gas liquor
mixed with the sulphuretted hydrogen. I succeed in utilizing this source of
sulphur by another means. I obtain the sulphur in a solid state, by introduc-
ing the mineral acid to the gas liquor in close wooden vessels, and, receiving
the mixed sulphuretted hydrogen and carbonic acid gases in a close wooden
vessel containing a solution of sulphurous acid, the two latter reagents recipro-
cally decompose one another, with the formation of sulphur, which may be
run out with the liquid, and which after a time precipitates. To prevent a
loss of the sulphurous acid in company with the escaping carbonic acid gas,
I cause the latter to pass up a wooden column, through several superposed

page_text: layers of sawdust, kept wet by a shower of water falling onto the uppermost
layer and descending through it to the other layers, this weak solution being
drawn off from the bottom sewers to dissolve a fresh dose of sulphurous acid
for a subsequent operation.
'I claim, as my Invention, the combination of the several steps in the opera-
tion which I have described for obtaining sulphur, and not any isolated portion
of the process.
In witness whereof, I, the said Richard Laming, have hereunto set my
hand and scal, this Third day of March, in the year of our Lord
One thousand eight hundred and forty-nine.
(L.S.) RICHARD LAMING.
AND BE IT REMEMBERED, that on the Third day of March, in the
year of our Lord 1849, the aforesaid Richard Laming came before our
said Lady the Queen in Her Chancery, and acknowledged the Specification
aforesaid, and all and every thing therein contained and specified, in form
above written. And also the Specification aforesaid was stamped according
to the tenor of the Statute made for that purpose.