IMPROVEMENTS IN THE UTILIZATION OF THE ALKALINE, NEUTRAL, AND SALINE SALTS CONTAINED IN THE MOTHER LIQUORS, OR WEAK ALKALI RESULTING FROM THE MANUFACTURE OF CRYSTALS OF SODA OR OTHER ALKALINE SALTS
Year: 1868

page_text: LETTERS PATENT to John Oliver, Chemist, and Charles Octavius
M Allum, Merchant, both of the Town and County of Newcastle-
upon-Tyne, for the Invention of "IMPROVEMENTS IN THE UTILIZATION
OF THE ALKALINE, NEUTRAL, AND SALINE SALTS CONTAINED IN THE MOTHER
LIQUORS, OR WEAK ALKALI RESULTING FROM THE MANUFACTURE OF CRYSTALS
OF SODA OR OTHER ALKALINE SALTS."
Sealed the 2nd March 1869, and dated the 10th September 1868.
PROVISIONAL SPECIFICATION left by the said John Oliver and Charles
Octavius M'Allum at the Office of the Commissioners of Patents,
with their Petition, on the 10th September 1868.
We, JOHN OLIVER, Chemist, and CHARLES OCTAVIUS M'ALLUM,
Merchant, both of the Town and County of Newcastle-upon-Tyne, do
hereby declare the nature of the said Invention for "IMPROVEMENTS IN
THE UTILIZATION OF THE ALKALINE, NEUTRAL, AND SALINE SALTS CONTAINED IN
THE MOTHER LIQUORS OR WEAK ALKALI RESULTING FROM THE MANUFACTURE OF
CRYSTALS OF SODA OR OTHER ALKALINE SALTS," to be as follows:-

page_text: "The Invention consists in the utilization of such alkaline, neutral, and
saline salts in the manner following, that is to say :-
Firstly. We make use of the said salts for the preparation of " esparto
grass " and other vegetable substances to obtain therefrom fibrous
inaterial applicable for paper making and for toxtile manufactures.
Hitherto the strong alkalies of commerce have been used for this
purpose, being previously converted into caustic alkali by the addition
of lime, or the caustic soda of commerce has been employed, both of
wwhich are much more costly than our improved process. In utilizing
the said salts for this purpose we either take the mother liquor as it
results from the manufacture of the crystals and render it caustic by
the addition of lime and then boil the vegetable substance therewith, or
if the preparation of the vegetable substance is not carried on in the
same works as the manufacture of the crystals we evaporate the mother
liquor to dryness, and use the residuum with the addition of lime and
water to make the caustic solution on the premises where the manu-
facture of the fibre is effected.
Secondly. After boiling the vegetable substanee with the caustic ley
as above described, we recover from the latter by ordinary well-known
chemical processes carbonate or other commercial salts of soda.
Thirdly. By the addition to such mother liquor or weak alkali of
sulphate of magnesia, or other compound or preparation of magnesia or
of lime, (or both lime and magnesia,) we obtain therefrom various
chemical compounds, such as carbonate and hydrate of magnesia, sul-
phate and phosphate of soda, and other more valuable salts or products
.not hitherto obtained 'from such mother liquor or weak alkali.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said John Oliver and Charles Octavius McAllum in the
Great Seal Patent 'Office on the 10th March 1869.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, JOHN 30
OLIVER, Chemist, and CHARLES OCTAVIUS MCALLUM, Merchant, both of
the Town and County of Newcastle-upon-Tyne, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Tenth day of September, in the year

page_text: of our Lord One thousand eight hundred and sixty-eight, in the thirty-
second year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto us, the said John Oliver and Charles Octavius M*Allum,
Her special licence that we, the said John Oliver and Charles Octavius
McAllum, our executors, administrators, and assigns, or such others as
we, the said John Oliver and Charles Octavius M'Allum, our executors,
administrators, and assigns, should at any time agipe with, and no atliers,
from time to time and at all times thereafter during the term thercini
expressed, should and lawfully might make, uso, 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 UTILI-
BATION OF THE ALKALINE, NEUTRAL, AND SALINE SALTS CONTAINED IN THE MOTHER:
LIQUORS OR WEAK ALKALI RESULTING FROM THE MANUFACTURE OF CRYSTALS OF
SODA OR OTHER ALKALINE SALTS," upon the condition (amongst others) that
we, the said John Oliver and Charles Octavius McAllum, our executors.
or administrators, by an instrument in writing under our, or one of our
or their, or one of their hands and scals, 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 we, the said John Oliver and Charles Octavius
McAllum, do hereby declare the nature of our said Invention, and in
what manner the same is to be performed, to be particularly described
and ascertained in and by the following statement in writing, that is to
Bay:
This Invention relates to the utilization of such alkaline, neutral, and
saline salts as may be present in the residual or mother liquors.resulting:
from the manufacture of soda crystals.
And in order that the said Invention may be fully understood. we will
now proceed more particularly to define the nature of our improvements
and in what manner the same is to be performed..
But before describing the nature of our said improvements we may
remark that it has heretofore been the practice in treating textile plants:
for obtaining fibrous material applicable to the manufacture of paper or
textile fabrics to operate upon the fibrous material under treatment with.
strong soda ash obtained from the black ash or tank liquors, andi

page_text: or contaminated with various neutral or saline salts, chiefly chloride
and sulphide of sodium, together with hyposulphite and sulphite of soda.
The sulphur present in the black ash or tank liquors is oxidised during
the subsequent processes of drying, carbonating, or refining, and reacts
upon the alkaline base re-forming sulphate of soda, hence the high-fired
ash appropriated to the manufacture of soda crystals contains a high
per-centage of neutral and saline. matter, chiefly consisting of chloride
of sodium and sulphate of soda, which are of no commercial value, and
in order to render these neutral compounds of commercial value we
proceed in manner as follows:-
Firstly. If we make use of the said salts for the purpose of
preparing esparto grass and other vegetable substances to obtain
therefrom fibrous material applicable for paper making and textile
manufactures we prefer taking the mother liquors as run from the
soda crystals and boiling them with hydrate of lime to form caustic
soda, either by appliping steam or furnace heat in any convenient vessel,
such apparatus being well understood. We prefer using about 40 parts
of hydrate of lime to every 50 parts of carbonate of soda present in the
alkaline solution operated upon. The caustic solution thus prepared we
prefer using of a density from 1.050 to, 1.060 specific gravity, and con-
taining from 5 to 10 parts of anhydrous soda to 100 parts of esparto
boiled. The process of boiling the fibre may be conducted in any
convenient vessel, but we prefer using close pans, of about 400 cubic
feet capacity, and fitted with the necessary means to introduce the
caustic solution and withdraw the black liquor from the boiled fibre,
which we pass through a set of horizontal cast-iron or other metal rollers.
to abrade the fibre and remove as much of the black liquor with which
it is saturated as possible; the fibrous material is now washed to remove
all colouring and extractive matter, and passed through a second set of
horizontal rollers under pressure to remove any excess of moisture, after
which it is transferred to a drying stove heated by the waste or other
heat and steam generated during the process of boiling the fibre and
concentrating the black liquors (by any convenient arrangement of flues
and heating apparatus) containing the neutral and saline salts; we
also cause a current of heated air to pass through the drying stoves to
carry off the steam generated and facilitate evaporating. The black
liquors in which the fibrous material has been boiled and containing

page_text: the extractive matter from the plant, together with the neutral and
saline salts present in the mother liquors resulting from soda crystals
is evaporated to dryness, or nearly so, and incorporated with carbonate
of lime and coal in about the following proportions, viz., 100 parts
of carbonate of lime and 70 parts of coal to every 100 parts of sulphate
of soda present in the black liquor operated upon. The incorporated mass
is next introduced into an ordinary black ash or ball furnace, and
exposed to a heat sufficient to decompose the sulphate of soda and
organic matter elaborated from the plant; the black ash thus obtained
is afterwards submitted to lixiviation, and the alkaline salts obtained by
the ordinary processes of manufacture, which are well understood. By
this mode of manipulation fully 75 per cent. of the neutral salts present
in the soda ash used in the treatment of fibrous material is recovered in
merchantable form.
Secondly. If the soda mother liquors contain a large excess of chloride
of sodium we prefer to utilize the alkaline and neutral salts present as
follows:-We decompose the carbonate of soda present in the ash with
sulphate of magnesia, by which means we obtain hydrated carbonate of
magnesia precipitated and sulphate of soda in solution; and in per-
forming this part of our improvements we prefer using a slight excess of
carbonate of soda to insure the complete decomposition of the sulphate
of magnesia, and to effect this we prefer to use hot solutions of carbonate
of soda and sulphate of magnesia at a temperature ranging from 160 to
180 Fahrenheit; the soluble salts are separated from the insoluble car-
bonate of magnesia by the ordinary process of filtration, well understood,
and the supernatent liquor containing the neutral saline salts evaporated
to dryness and treated with an equivalent quantity of sulphuric acid to
decompose the chloride of sodium present, and by this means we obtain
sulphate of soda of good quality applicable to the manufacture of 50 per
cent, ash by the ordinary process of manufacture.
Thirdly. Our improvements consist in decomposing solutions of
sulphate of soda by solutions of lime or other alkaline earths, by which
we obtain caustic soda and sulphates of the respective bases employed
(viz., lime, strontia, and baryta), which sulphates are applicable to
the manufacture of pigments and sulphate of ammonia.
Having thus described the nature of our said Invention, and in what
manner the same is to be performed, we would have it understood that
we do not confine our means or mode of operation to any particular form

page_text: of apparatus or mode of manipulation; but what we claim as our Inven-
tion is, the process or mode of utilizing the neutral saline salts contained'
in the soda salts employed, substantially as herein-before described and
set forth.
In witness whereof, I, the said John Oliver (on behalf of myself 5
and of the said Charles Octavius McAllum), have hereunto set my
hand and seal, this Sixth day of March, in the year of our Lord
One thousand eight hundred and sixty-nine.
Witness,
BRISTOW HUNT,
Solicitor and Patent Agent,
1, Serlo Street, Lincoln's Inn.
JNO.. OLIVER. (L.S.)