IMPROVEMENTS IN THE TREATMENT OF KELP AND IN THE MANUFACTURE OF PRODUCTS THEREFROM
Year: 1862

page_text: LETTERS PATENT to James Walker, of Glasgow, in the County of
Lanark, North Britain, Manufacturing Chemist, for the Invention of
"IMPROVEMENTS IN THE TREATMENT OF KELP AND IN THE MANUFACTURE OF
PRODUCTS THEREFROM."
Sealed the 20th February 1863, and dated the 1st September 1862.
PROVISIONAL SPECIFICATION left by the said James Walker at the
Office of the Commissioners of Patents, with his Petition, on the 1st
September 1862.
I, JAMES WALKER, of Glasgow, in the County of Lanark, North Britain,
Manufacturing Chemist, do hereby declare the nature of the said Invention
of "IMPROVEMENTS IN THE TREATMENT OF KELP, AND IN THE MANUFACTURE OF
PRODUCTS THEREFROM," to be as follows, that is to say :—
This Invention comprises improved modes of treating kelp for the obtain-
ment or manufacture therefrom of various products, such as iodine, salts of
soda, salts of potash, and borax.
According to one plan a solution of the soluble portion of the kelp is
neutralised with sulphurous acid, and the resulting sulphites and hyposulphites
of soda are separated by evaporation and crystallisation. The residual mother
liquor is treated as herein-after described.
According to a second plan the kelp solution is neutralised with sulphurous
acid and then boiled with sulphur, or is first boiled with sulphur and then

page_text: neutralised with sulphurous acid and the resulting hyposulphite of soda is
separated by evaporation and crystallisation, leaving a residual mother liquor
to be treated as herein-after described.
According to a third plan the kelp solution is treated with a salt of iron,
magnanese or alumina, so long as a precipitate is formed, or it is neutralised
(avoiding excess) with sulphuric, muriatic, or nitric acid, or with mixtures of
such acids and salts, such for instance as that known to iodino manufacturers
as "sour lye" or "acid liquor," or that known to chlorine manufacturers as
"still liquor." The precipitate, if any, is separated by settling and decantation
and the clear solution is evaporated to about ninety degrees Twaddle, or even
higher, when the greater portion of the chlorides, sulphites, and sulphates of
soda and potash will be deposited as a salt during evaporation, the resulting
liquor yielding crystals of hyposulphite of soda. The residual mother liquor
is treated as herein-after described.
According to a fourth plan there is added to the kelp solution boracic acid
in the proportion to form borax (biborate of soda) with the free alkali, and the
borax is crystallised out and then the hyposulphite of soda, leaving a residual
mother liquor to be treated as herein-after described. The residual mother
liquor obtained by the herein-before described processes is evaporated to
dryness and fused at a dull red heat to decompose the remaining byposulphite.
The fused mass is then dissolved and evaporated until it deposits the sulphate
of soda and potash formed in fusing. The remaining liquor will consist chiefly
of iodide of sodium, which may be converted into iodide of potassium by
adding carbonate of potash or chloride of potassium in the proportions of their
chemical equivalents. The iodide of potassium is formed in either case by
double decomposition, and may be crystallised in the usual manner after
separating the soda salt. Or the residual mother liquor may have added to
it hydrochloric acid in sufficient quantity to decompose the remaining
byposulphite, the sulphurous acid being then driven off by boiling. The liquor
is afterwards filtered and allowed to settle in order to separate sulphur and
other insoluble matter. The clear liquor is then evaporated to dryness and
fused at a gentle heat, and the fused mass, consisting chiefly of iodide of
potassium and chloride of sodium is dissolved, and the iodide of potassium
crystallised in the usual manner after separating the soda salt.
According to a fifth plan the kelp solution is ovaporated to dryness and
fused at a dull red heat, and the fused mass is mixed with boracic acid (in the
proportion to form borax) along with an oxidising substance such as nitrate of
soda, or potash, chlorate of potash, chromate of potash, peroxide of iron, or
binoxide of managnese, preference being given to the last. The mixture

page_text: is heated in a retort, when iodine will be distilled over and may be collected in
receivers. The residue is then dissolved and crystals of borax obtained in the
ordinary manner.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said James Walker in the Great Seal Patent Office on the 27th
February 1863.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JAMES
WALKER, of Glasgow, in the County of Lanark, North Britain, Manufacturing
Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the First day of September, in the year of our Lord
One thousand eight hundred and sixty-two, in the twenty-sixth year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto me, the
said James Walker, Her special licence, that I, the said James Walker, my
executors, administrators, and assigns, or such others as I, the said James
Walker, 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 Britain and Ireland, the Channel
Islands, and Isle of Man, an Invention for "IMPROVEMENTS IN THE TREAT-
MENT OF KELP, AND IN THE MANUFACTURE OF PRODUCTS THEREFROM," upon the
condition (amongst others) that I, the said James Walker, my exccutors 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 Offico within
six calendar months next and immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said James Walker, do hereby declare the
nature of my said Invention, and in what manner the same is to be performed,
to be particularly described and ascertained in and by the following state-
ment, in writing, that is to say :-
My said Invention comprises improved modes of treating kelp for the
obtainment or manufacture therefrom or thereby of various products, such as
iodine, salts of soda, salts of potash, and borax. And in carrying out my
Invention I employ solutions containing the soluble portions of the kelp,

page_text: perferring to operate upon such solutions after they have attained the stage
known to manufacturers of ioline as "finish liquor."
In the first of my improved modes of treating kelp the finish liquor or kelp
solution is diluted with water until its specific gravity is reduced to 1.25 or 50
degrees Twaddle. It is then neutralised with sulphurous acid and allowed to
settle. The clear solution is drawn off and evaporated until it retains a specific
gravity of 1-55 to 1.60, or 110 to 120 degrees Twaddle. During evaporation
a quantity of soda and potash salts are deposited, which are set asido to be
treated separately. The concentrated solution yields crystals of hyposulphite
of soda on cooling, and these crystals are purified by redissolving and re-
crystallising. The fixed salts obtained during evaporation I prefer to put
into the keaves or lixiviating vats to be treated along with fresh kelp. The
mother liquid obtained from the first crystals of hyposulphite of soda is treated
as herein-after described.
According to a second plan the finish liquor or kelp solution is neutralised
with sulphurous acid and then boiled with sulphur, or is first boiled with
sulphur and then neutralized with sulphurous acid. Instead of neutralising
with sulphurous acid, the liquor, either before or after boiling with sulphur,
may be oxidised by exposure to atmospheric air in a tower filled with coke, or
by other known means. The neutralised or oxidised liquor being treated
as in the first plan, the residual mother liquor is treated as heroin-after
described.
According to a third plan there is added to the finish liquor or kelp solution
a soluble salt of iron, manganese, or alumina, so long as a precipitate is
formed; or it is neutralised with sulphuric, muriatic, or nitric acid, or with
mixtures of such acids and salts, such, for instance, as that known to manu-
facturers of iodine as "sour lye" or "acid liquor," or that known to manu-
facturers of chlorine as "still liquor." I prefer to have the mixture slightly
alkaline in order to prevent the already existing byposulphite of soda from
being decomposed. After settling the clear liquor is drawn off to be treated
as in the first plan, the residual mother liquor being treated as herein-after
described.
According to a fourth plan there is added to the finish liquor or kelp
solution boracic acid in sufficient quantity to form borax (biborate of soda)
with the soda existing in the solution as carbonate of soda, caustic soda, and
sulphido of sodium. The borax is then crystallised in the usual manner, and
from the remaining mother liquor hyposulphite of soda is obtained by further
concentration; this salt being separated the residual mother liquor is treated
as immediately herein-after described. The treatment of the neutralised.

page_text: oxidised, or residual mother liquors herein-before referred to is as follows, that
is to say, by one plan the liquor is evaporated to dryness and fused at a
moderate red heat to decompose the remaining hyposulphite. The fused
product consists chiefly of iodide of sodium with sulphates of soda and potash
and traces of other salts. The said product is dissolved in water and evaporated
to a specific gravity of about 1.65 or 130 degrees Twaddle. The sulphates of
soda and potash are deposited during evaporation and may be fished out, and
after washing be put into the keaves to be treated along with fresh kelp. To
the solution of iodide of sodium obtained, as herein-before described, there are
added seventy parts of carbonate of potash for every one hundred and fifty
parts of iodide of sodium contained in the solution; or, for the seventy parts of
carbonate of potash there are substituted seventy-five parts of chloride of
potassium. In either case iodide of potassium is formed and the corresponding
salt of soda. The iodide of potassium is crystallised in the usual manner after
separating the carbonate of soda or chloride of sodium, as the case may be.
By another plan the neutralised, oxidised, or residual mother liquor has added
to it hydrochloric acid in quantity sufficient to decompose the remaining
hyposulphite (avoiding excess); the matters are then evaporated to dryness
and fused at a moderate red heat. The fused mass, consisting chiefly of iodide
of potassium and chloride of sodium, is dissolved, and the iodide of potassiumi
is crystallised in the usual manner after separating the soda salt. Should
there be too little potassium present to combine with all the iodine, the
deficiency is made up by adding the requisite quantity of chloride of potassium
or carbonate of potash.
According to a fifth mode of treating the finish liquor or kelp solution it is
evaporated to dryness and fused at a moderate red heat; there is then mixed
with the fused mass as much boracic acid along with an oxidised substance as
will decompose the iodide of sodium and take up the soda from the other
decomposable salts, and at the same time form borax (biborate of soda). The
oxidising substance preferred is binoxide of manganese, but others may be
used with advantage, such as nitrate of soda, nitrate of potash, chlorate of
potash, chromate of potash, or peroxide of iron. The described mixture is
Leated to redness in a retort of iron or fire-clay, and the iodine which distils
over is collected in receivers in the usual manner. This process may also be
adopted for separating iodine from the fused iodide of sodium or iodide of
potassium obtained under my first, second, third, and fourth modifications of
processes herein-before described. After separating the iodine the residue is
taken from the retort, and yields crystals of borax by dissolving and crystal-
lising in the usual manner.

page_text: Having thus particularly described my said Invention and the manner in
which the same is or may be performed, I have to state that I do not restrict
myself to the precise details herein-beforo described, but that what I believe
to be novel and original, and claim as the Invention secured to me by the
herein-before in part recited Letters Patent is, the preparing of byposulphite
of soda, borax, iodide of sodium, iodide of potassium, and iodine, from or by
means of kelp liquors or products, substantially in the manner herein-before
described.
In witness whereof, 1, the said James Walker, have hereunto set my
hand and seal, this Twenty-sixth day of February, in the year of our
Lord One thousand eight hundred and sixty-three.
Witness,
EDMUND ПUNT,
Patent Agent,
28, St. Enoch Square, Glasgow.
JAS. WALKER. (L.S.)