IMPROVEMENTS IN THE MODE OF OBTAINING CERTAIN CHEMICAL SUBSTANCES, AND IN THE TREATMENT! OP VEGETABLE FIBRE, AND IN OBTAINING MANURIAL AND OTHER PRODUCTS THEREFROM." PROVISIONAL SPECIFICATION
Year: 1861

page_text: ETTERS PATENT to John Oliver, of Colchester, in the County of Essex,
Manufacturing Chemist, John Grantham, of No. 81, Nicholas Lane, in
the City of London, Engineer, William Sinnock, of Sylvan Cottage,
Woodford, in the County of Essex, Ropery Engineer, and Montague
Richard Leverson, of No. 12, Saint Helen's Place, in the City of London,
Solicitor and Patent Agent, for the Invention of "IMPROVEMENTS IN THE
MODE OF OBTAINING CERTAIN CHEMICAL SUBSTANCES, AND IN THE TREATMENT!
OP VEGETABLE FIBRE, AND IN OBTAINING MANURIAL AND OTHER PRODUCTS
THEREFROM."
PROVISIONAL SPECIFICATION left by the said John Oliver, John'
Granthain, William Sinnock, and Montague Richard Leverson, at the
Office of the Commissioners of Patents, with their Petition, on the
20th September 1861.
5 We, JOHN OLIVER, of Colchester, in the County of Essex, Manufacturing
Chemist, JOHN GRANTHAM, of Number 31, Nicholas Lanc, in the City of.
London, Engineer, WILLIAM SINNOCK, of Sylvan Cottage, Woodford, in the

page_text: County of Essex, Ropery Engineer, and MONTAGUE RICHARD LEVERSON,
Number 12, Saint Helen's Place, in the City of London, Solicitor and Pater
Agent, do hereby declare the nature of the said Invention for "IMPROVEMENT
IN THE MODE OF OBTAINING CERTAIN CHEMICAL SUBSTANCES, AND IN THE TREATMEN
OF VEGETABLE FIBRE, AND IN OBTAINING MANURIAL AND OTHER PRODUCTS THERI
FROE,"
," to be as follows:-
The Invention consists of certain improvements in the manufacture of pul
from vegetable fibrous materials suitable for the manufacture of various classe
of paper articles, of furniture, and other works of art, and of obtaining
several commercial products as bi-products of the manufacture.
Our mode of treatment consists in macerating or boiling the vegetable
fibrous material in water or a solution of mixed alkaline salts, after which we
subject it to mechanical treatment to abrade the corticous structure of the
plant, by which means it is brought into the most favorable state to be acted
upon by sundry alkaline salts in solution, by which a considerable quantity of
organic matter and inorganic constituents are removed in combination with
the alkaline salts used in the operation. The said solutions are run into
convenient vessels, and treated with nitric acid or nitrous acid and various
oxides of nitrogen and atmospheric air; by this means the neutral and alkalino
compounds present are decomposed or partly so, and valuable manurial sub-
stances obtained. For the manufacture of the manurial substances we appro-
priate the oxides of nitrogen generated as bi-products in the manufacture of
oxalic acid, sulphuric acid, and various other processes of chemical manufacture.
The said vegetable fibrous material, subjected to the foregoing manipulations,
is transferred to a bath of diluted nitric, nitro-hydrochloric, hydrochloric, or
sulphuric acid to remove any metallic, earthy, or phosphalic compounds
remaining in combination with the fibrous material. The vegetable fibrous
material thus treated is removed from the acid bath, and submitted to the
action of bleaching agents, the respective characters of which are comportable
to the physical character and commercial value of the article operated upon,
and are regulated according to the degree of whiteness to be imparted to it,
and amount of fibre required in the pulp produced. The class of bleaching
agents brought into requisition comprises certain combinations of sulphur &
oxygen, oxygen and hydrogen, chlorine free and in solution, obtained either
from ordinary chloride of line, or from such chlorides as are decomposed by
heat, from which, with the aid of an oxydizing agent, I obtain chlorine and
bi-products of commercial value. The bleached fibrous material is now

page_text: washed, treated with sesqui-carbonate of soda, immersed in a diluted solution
of mineral acid, and finally washed in water to remove all trace of salino
matter. The superfluous water mechanically retained by the pulp is removed
by expression to expedite transit.
In preparing the alkaline salts required for the treatment of vegetable fibre,
ns set forth in the foregoing manipulations, we prefer using sulphate of soda,
obtained as a bi-product in the manufacture of oxalic, nitric, sulphuric, and
hydrochloric acids, or from sulphate of soda obtained from the residual product
resulting from the manufacture of chlorine, from chloride of sodium, peroxide
of manganese, and sulphuric acid.
We decompose the sulphate of soda, obtained from whatever source, by
fusing it with carbonaceous matter, and the sulphurets thus formed we decom.
poso with carbonic acid, caustic or carbonate of lime, and magnesian limestone.
The sulphurets of calcium and magnesium obtained we treat with acids, and
obtain valuable salts of lime and magnesia.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said John Oliver, John Grantham, William Sinnock, and Mon-
taguo Richard Leverson in the Great Seal Patent Office on the 20th
March 1862.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, Joun
OLIVER, of Colchester, in the County of Essex, Manufacturing Chemist,
JOHN GRANTHAM, of No. 31, Nicholas Lane, in the City of London, Engineer,
WILLIAM SINNOCK, of Sylvan Cottage, Woodford, in the County of Essex,
Ropery Engineer, and MONTAGUE RICHARD LEVERSON, of No. 12, Saint
Helen's Place, in the City of London, Solicit and Patent Agent, send
greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twentieth day of September, in the year of our
Lord One thousand eight hundred and sixty-one, in the twenty-fourth year
of Her reign, did, for Herself, Her heirs and successors, give and grant unto
us, the said John Oliver, John Grantham, William Sinnock, and Montague
Richard Leverson, Her special licence that we, the said John Oliver, John
Grantham, William Sinnock, and Montague Richard Leverson, our executors,
administrators, and assigns, or such others as we, the said John Oliver, John

page_text: Grantham, William Sinnock, and Montague Richard Leverson, our 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 Islands
and Isle of Man, an Invention for "IMPROVEMENTS IN THE MODE OF OBTAINING
CERTAIN CHEMICAL SUBSTANCES, AND IN THE TREATMENT OF VEGETABLE FIBRE, AND
IN OBTAINING MANURIAL AND OTHER PRODUCTS THEREFROM," upon the condition
(amongst others) that we, the said John Oliver, John Grantham, William
Sinnock, and Montague Richard Leverson, our executors or administrators,
by an instrument in writing under our, or their; or one of their hands and
seals, should particularly describo and ascertain the nature of the said Inven
tion, and in what manner the same was to, be performed; and cause the
same to be filed in the Grent Scal. Patent Office within six calendar months
next and immediately after the date of the said Letters l'atent.
NOW KNOW YE, that we, the said John Oliver, John Grantham,
William Sinnock, and Montaguo Richard Loverson, do hereby declare tho
nature of our 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:-
Our Invention consists of improvements in the mode of obtaining certain
chemical substances, and in the treatment of vegetable fibre, and in obtaining
manurial and other products, therefrom, which may be more particularly
described :-
Firstly, as improvements in the mode of obtaining certain alkaline salts and
cartby chlorides.
Secondly, the application of the same to the treatment of vegetable fibrous
material for the manufacture of pulp, suitable for making tho various
descriptions of paper, articles of furniture, and other works of art.
And, thirdly, the application of the organic matter, mineral and saline
substances, extracted from the vegetable fibrous material operated upon,
combined with phosphatic and nitrogenous compounds, imparting a high
commercial value to them as manurial compounds.
We will now proceed to describe our improved method of making certain
salts of soda and chlorides (such as chloride of lime and chloride of magnesia),
which are intended to be used in the manufacture of pulp from vegetable
fibrous material. In manufacturing these salts of soda we prefer using.

page_text: sulphate of soda, obtained as a bi-product in the manufacture of hydro-
chloric acid from decomposing chloride of sodium by means of sulphuric acid,
or from sulphate of soda obtained as a bi-product in the manufacture of nitric
or sulphuric acid, by decomposing nitrate of soda by means of sulphuric acid.
The sulphate of soda, obtained from 'whatever source, if sufficiently. pure,
we merely submit to a pulverizing process by grinding or any other convenient
method, but sulphate of soda obtained as a bi-product in the manufacture of
bydrochloric or nitric acid generally contains an excess of acid and moisture,
and in either case we prefer roasting the sulphate of soda in a reverberatory
furnace to expel any such excess of acid or moisture, and to obtain the
sulphate in a proper state to be converted into alkaline salts, such state being
well understood. The sulphate of soda thus obtained we mix with carbonate
of lime and coal or coke in about the following proportions, say, three hun-
dred weight of sulphate of soda, two and a half hundredweight of carbonate of
lime, and two hundredweight of coal; the two latter quantities may be varied.
according to quality, but it is desirable at all times to use a little in excess of
equivalent quantities. The mixture is next introduced into a reverberatory
furnace, and exposed to a heat sufficient to effect the decomposition of sulphate.
of soda, by which we obtain what is usually. called ball alkali or black ash,
and contains about fifty per cent. alkaline salts, and fifty per cent. of sulphuret:
of calcium, and other impurities. The ball alkali or black ash thus obtained.
is next broken into fragments, and introduced into suitable vats, where it is
treated with water, and the soluble alkaline salts are drawn off from the
insoluble residuum; the apparatus. used in these operations are well under-
stood. The alkaline salts thus obtained are preferred to the ordinary articles:
of commerce, in that they act moro energetically upon the resinous and:
albuminous portion of the vegetable fibrous material operated upon without:
affecting the tenacity of the fibre, and are obtained at from forty to fifty per
cent. less in cost than the ordinary articles of commerce. These soluble-
alkaline salts thus obtained we use in the first and second process to which
the vegetable fibrous materials operated upon are subjected, and also in pre-
paring caustic alkali for the subsequent treatment to which the vegetable
fibrous materials are subjected. We boil equivalent quantities of the above
alkaline solution and caustic hydrated lime together, and thus obtain caustic
soda in solution, and carbonate of lime precipitated; the former we use for
the treatment of fibrous material, as previously stated, and the precipitated
carbonate of lime, after well washing, we use to convert sulphate of soda into

page_text: the aforesaid alkalino salts, but ordinary carbonate of lime or dolomito may be
used in the same operation.
Second, in the treatment of vegetable fibrous material according to our
Invention, we prefer macerating or boiling the fibrous material in a solution
of alkaline salts, as obtained from the ball alkali or black ash, until the said
fibrous materials have been sufficiently acted upon by these mild salts, that
is to say, until the resinous, albuminous, and organic matters have been
sufficiently removed as to admit of the free disintegration of the fibres in tho
second operation to which we submit them. Sometimes it is desirable to
submit the alkaline solution to a current of carbonic acid gas to correct any
excess of caustic or corrosivo salts which may be present before macerating
the fibrous material therein. When tho material is coarse, and it is desired
to produce a fine pulp, the fibrous material, after undergoing the process of
maceration in the alkaline solution, is passed through a set of horizontal
cylindrical rollers fitted with a flexiblo cylindrical brush working upon the
material as it passes over the lower roller, after which wo boil the fibrous
material thus treated in a solution of mild alkalino salts, as obtained from tho
ball alkali or black asb, until sufficiently acted upon and saturated with the
said solution. We then remove the fibrous material from the alkaline solution,
and allow it to be exposed to the atmosphere until the alkali held in the
interstices of the fibrous material has crystalied throughout the entire mass,
or nearly so; we then immerse the said fibrous material into a diluted acid
bath (occasionally we transfer it to the bath without allowing it to crystalizo),
by which the alkaline salts in the intorstitial spaces of the fibrous material
are decomposed, and the rapid evolution of the carbonic acid separates the
fibres. The fibrous material thus treated is washed, and boiled in a solution
of caustic alkali of requisite density, to remove any traco of carthy or silicious
matter remaining in combination with it, but we prefer using a caustio
solution of about 1-025 specific gravity; after which it is washed, and, if,
necessary, immersed in a bath of dilute sulphuric, hydrochloric, or nitric acid
to remove any iron or phosphatic compounds that may remain in combination
with the fibre; after which it is washed, and submitted to a bleaching process.
But if it is necessary to produce a fine fibrous material, either for textile or
pulp purposes, we prefer taking the inaterial direct from the caustic alkaline
Folution, and exposing it to an atmosphere of carbonio acid gas in any con-
venient vessel until the caustic alkali adhering to or retained in the interstitial
spaces of the fibrous material is converted wholly or in part into carbonated

page_text: alkali; we then immerse the article thus treated in a bath of dilute acid, by
which the carbonated alkali is decomposed, and the expansive power of the
carbonic acid gas generated in the centre of the sheaves or bundles of fibre,
effects their complete disintegration; after which the material is washed, and
submitted to a bleaching operation, the nature of which depends upon the
degree of whiteness to be imparted to and amount of fibre to be retained in
the article of pulp produced.
For bleaching half stuff of ordinary quality, we prefer using a solution of
chloride of lime at any convenient temperature, either with or without the
application of an acid, to liberate chlorine; but if we use an acid to liberate
chlorine from a solution of chloride of lime, or if we use free chlorine obtained
by decomposing peroxide of manganese by hydrochloric acid, we prefer per-
forming the bleaching operation in close vessels, and conveying the chlorine
generated in the operation into contact with hydrate of lime in close chambers
or compartments, similar to those used in the manufacture of chloride of
lime, such arrangement of apparatus being well understood. By this means
we obtain hypochlorite of lime and chloride of calcium, which we use in a
second operation, and thus accomplish a bleach at a small expenditure of
chlorine; but if we wish to produce a fine fibrous material, and to effect a
perfect bleach, we bleach with a solution of chlorine in water, the preparation
of which is well understood; but we prefer to bleach with a solution of hypo-
chlorite of magnesia, which we obtain in manner as follows:-In manu-
facturing bypochlorite of magnesia we prefer operating upon dolomite or
magnesian limestone with sulphuric acid, the respective proportions of which
we vary according to the composition of the dolomite used in the manufacture;
but as dolomite readily available for the purpose is to be found in great
abundance, containing about forty-eight per cent. carbonate of magnesia, fifty
per cent. carbonate of lime, and variable quantities of silica, iron, and other
impurities, and assuming limestone of this quality as the type of the article
operated upon, we proceed as follows:-We first expose the dolomite tò a
moderate heat to expel moisture, and then reduce it to powder by grinding
or any other convenient means. We then operate upon (say) one hundred
pounds of the pulverized dolomite with (say) one hundred pounds of oil of
vitriol. The above proportions give a little excess of dolomite, it being the
cheaper article. By decomposing the dolomite with sulphuric acid of any
convenient density we obtain soluble sulphate of magnesia and insoluble
sulphate of lime. We prefer performing the operation in close vessels, and

page_text: using the carbonic acid gas generated in the decomposition of the dolomite to
carbonate the caustic alkali adhering to or retained in the interstitial. spaces
of the vegetablo fibrous material, when it is required to submit that article
to the carbonating process for the purpose of dividing the fibres, as previously
explained. The soluble sulphate of magnesia is then washed out from the
insoluble sulphate of lime in the ordinary way, the process being well under-
stood. The sulphate of lime thus obtained we use in the manufacture of
manure, which we will presently advert to. The solution of sulphate of
magnesia thus obtained we decompose by means of chloride of lime in solution,
producing bypochlorite of magnesia in solution, and precipitating the greater
portion of the sulphate of limo. In practical working we use equivalent
quantities of chloride of lime and sulphate of magnesia, or nearly so, pre-
ferring, however, to uso a slight excess of sulphate of magnesia to guard
against the injurious effect of the presence of chloride of lime upon the
delicate fibre. The hypochlorite of magnesia thus obtained is applied in the
bleaching bath in a very dilute form, producing a perfect bleach, without any
injurious effect upon the tenacity of the fibre, and effectually removed by ono
or two washings without injury to color. Vegetable fibrous material thus
treated may be prepared for transport by any convenient mode.
Thirdly, in carrying out that part of our Invention which has reference to
the application of organic matter, mineral and saline substances, extracted
from the vegetablo fibrous material operated upon, and mixing them with
phosphatic and nitrogenous compounds, so as to impart a high commercial
value to them as manurial compounds, we may observe, that recent
discoveries in the econoniy of vegetable physiology have pointed out the
potent effect of phosphatic and ntrogeneous compounds as artificial stimulants
when brought to bear on practical agriculture, and the commercial value of
all manurial agents generally depend upon the quantity of these respective
substances present. It is also well known that in manufacturing paper pulp
of fine quality from vegetable fibrous material, a loss of more than fifty per
cent. in the material operated upon is sustained, and the matter thus separated
from the fibre consists chiefly of organic, mineral, and saline substances,
which, mixed with proportionate quantities of phosphatic and nitrogenous
compounds, are possessed of high fertilizing powers. It is also well known
that in many processes of chemical manufacture vast quantities of nitrogenous
compounds are generated and. allowed to waste, and as one of such processes,
in which such waste occurs we select the manufacture of oxalic acid. The

page_text: following is the mode in which we carry this part of our iniprovements into
operation. After removing the fibrous material from the alkaline mixture, as
above described, organic, mineral, and saline, matters remain behind, and we
cause the nitrogenous gases and, compounds generated in the manufacture of
oxalic acid or other process of manufacture in which nitrous fumes aro
generated to pass together with atmospheric air through the alkaline solution
containing the organic matter, mineral and saline substances, extracted from
the vegetable fibrous material operated upon, by which the whole or nearly
the whole of the nitrogenous gases and compounds are taken up. We then
concentrate the solution thus treated, and add thereto a proper quantity of
soluble phosphates, and with sulphate of lime, obtained as a bi-product from
the manufacture of hypochlorite of magnesia, as above. described, from other
sources, to impart the fertilizing properties required in the case under treat-,
ment, on principles and by methods well understood.
.
J
Having now described the nature of our Invention of improvements in the
mode of obtaining certain chemical substances, and the application thereof to
the treatment of vegetable fibrous material, and the conversion and application
of the organic and other matters and substances extracted from the vegetable
fibrous material operated upon into a valuable manurial compound, we must
first observe we are aware that the operations or processes of manufacturing
the alkaline salts which we deem to be necessary for the treatment of vegetable
fibrous material for the purpose of obtaining half stuff or pulp, and which have
been herein described, are in practice well known, but the use and application
of such reagents as above described to the treatment of vegetable fibrous
materials in the form above specified has not hitherto been attempted; we
claim,-
First, improvements in the mode of obtaining certain earthy chlorides,
substantially as described.
Second, improvements in the application of certain alkaline salts, .under the
conditions and in the forms above set forth, to the treatment of vegetable
fibrous materials, substantially as described.
Third, the collecting, fixing, and utilization of the nitrogenous gases and
compounds generated in any of the processes or manufactures referred to in
the third portion of this our Specification (which nitrous gases and compounds
have heretofore been wasted), and mixing or combining them with the organic
matter, mineral and saline substances, extracted from the vegetable fibrous
material operated upon, which being combined with soluble phosphates

page_text: and sulphate of lime, by methods already known, and not included in our
claim, become fit for manurial purposes.
Fourth, the combination of these, manufactures in the manner described,
so that the products from the one are directly available for the other with but
little intermediate treatment.
JOHN OLIVER.
Signed, sealed, and delivered by the
within-named John Oliver, in the
presenco of
II. HARRON,
· Clerk to M. R. Leverson,
12, St. Helen's Place, EC.
MONTAGUE R. LEVERSON.
(L-8.)
Signed, sealed, and delivered by the
within-named Montague Richard
Leverson, in the presence of
H. HARRON,
Clerk to M. R. Leverson,
12, St. Helen's Place, E.C.