A New or Improved Manufacture of Double Salts Containing Fluorine and an Always Constant Amount of Antimony.
Year: 1892

page_text: Date of Application, 27th Sept., 1892
Complete Specification Left, 5th June, 1893-Accepted, 15th July, 1893
PROVISIONAL SPECIFICATION.
A New or Improved Manufacture of Double Salts Containing
Fluorine and an Always Constant Amount of Antimony.
A communication by THEODOR MAYER, of Feuerbach, in the Empire of Germany,
Manufacturer.
I, WILLIAM PHILLIPS THOMPSON, F.C.S., M.I.M.E., of the Agency for Foreign
Patent Solicitors, 6 Lord Street, Liverpool and 6 Bank Street, Manchester both
in the County of Lancaster and 323 High Holborn in the County of Middlesex
Civil Engineer, do hereby declare the nature of this invention to be as follows:-
This process has for its object the manufacture of compounds of fluoride of
antimony with the sulphate or chloride salts of soda, potash or ammonia, which are
composed according to the formula Sb (FICI)' M'A', in which M¹ denotes the
(monatomic) base, and A¹ the monatomic equivalent of sulphuric or hydrochloric
acid. The process is characterised, as compared with the methods at present
employed for the manufacture of fluoride of antimony compounds, by the simul-
taneous use of hydrochloric acid, whereby compounds are obtained containing two
molecules of hydrochloric acid with one molecule of a sulphate salt. By the use of
hydrochloric acid, an always constant proportion of antimony equivalent to
55 per cent. oxide of antimony is obtained in the compounds, which, as analysis
shows, is the result of the partial replacement of fluorine by chlorine, and of
sulphate salt by chloride salt. The sulphate of potash salt, which consists mainly
of (Sb Fl K'SO', rields the finest crystals, whilst a small part of the sulphate
of potash is replaced by chloride of potassium."
The process is as follows:-
60 parts of oxide of antimony are dissolved in a mixture of hydro fluoric acid
and concentrated hydrochloric acid.
25 parts of sulphate of potash are then stirred into the gently warmed solution,
and as much hydro_fluoric acid is added until water added to a sample causes no
more separation. The crystallisation of the compound (Sb Fl³); K*SO* then takes
place after the cooling of the solution, during which the sulphate of potash is
partially replaced by chloride of potassium.
The same process is employed when sulphate of soda, or ammonia, or chloride of
potassium, sodium or ammonium is employed.
In the latter cases, a portion of the fluorine is replaced by chlorine, so that, in
this case also, as in the sulphate compounds, double salts are obtained which
contain a constant proportion of antimony equivalent to about 55 per cent. of oxide
of antimony.
Dated this 26th day of September 1892.
COMPLETE SPECIFICATION.
A New or Improved Manufacture of Double Salts Containing
Fluorine and an Always Constant Amount of Antimony.
A communication by THEODOR MAYER, of Feuerbach, in the Empire of Germany,
Manufacturer.
I, WILLIAM PHILLIPS THOMPSON, F.C.S., M.I.M.E., of the Agency for
Foreign Patent Solicitors, 6, Lord Street, Liverpool, and 6, Bank Street,
Manchester, both in the County of Lancaster and 323 High Holborn in the
Price 8d.1

page_text: County of Middlesex, Civil Engineer, do hereby declare the nature of this
invention and in what manner the same is to be performed, to be particularly
described and ascertained in and by the following statement :-
The processes hitherto employed for producing the double salts of fluoride of
antimony and alkaline sulphates are based on the formation of compounds which
contain molecule of the alkaline salt to 1 molecule of the fluoride of antimony.
As the sole exception, the salt of the formula 2 SbF, 1+Am,SO, may be named.
This process, on the contrary, has for its object the manufacture of compounds
which correspond to the formula 2 SbF, M,SO, (in which M represents potash,
soda or ammonia).
If, in fact, fluoride of antimony and alkaline sulphate be caused to act on one
another in such proportionate quantities that at the most 1 molecule of alkaline
sulphate is employed to 2 molecules SbF, there result sharply characterised
already crystallising compounds of the composition of 2 SbF, M,SO, compounds
which were hitherto entirely unknown and which represent a new class of double
antimony salts. The formation and crystallisation of these new salts are considerably
facilitated by a partial replacement of the fluoric acid in the process, with a certain
amount of hydrochloric acid. If a certain limit be exceeded in the addition of this
hydrochloric acid, the latter has a decomposing action on the sulphate, and
mixtures are formed of double sulphate salts with double alkaline chloride salts of
the formula SbF,MCI or the latter alone.
The technical value of the already crystallising compounds of 2 molecules of
SbF, with 1 molecule of alkaline sulphate lies in the fact that the amount of
antimony contained in it is higher than that of all the other like crystalline salts,
and that they are at least equal, if not superior, to the compounds SbF, M.SO.
and SbF, MCI in mildness, permanency and solubility, and, further, the price of
antimony is, of course, correspondingly lower in these new salts than in the other
competing products, as the amount of ballast materials is much smaller. For
technical manufacture only the double fluoride of antimony and potash and
ammonia sulphate is suitable.
The process for producing these salts is as follows
:-
A quantity of oxide of antimony, thoroughly corresponding to 1 molecule, is
stirred up in water, and fuming fluoric acid or 33 per cent. hydrochloric acid
and fuming fluoric acid is added thereto until the oxide is dissolved, and a
sample of the solution, when diluted with water, remains clear, and then the
quantity of alkaline sulphate suitable for 1 molecule is stirred into the warmed
solution. On the solution cooling, the double salts in question then crystallise out.
The double fluoride of antimony and sulphate of potash 2 SbF, K,SO, is
deposited, in the case of a solution free from hydrochloric acid, in crusts and dregs
of small prismatic, or lancet-shaped crystals, and, from a solution containing
hydrochloric acid, in sparkling crystals of predominating prismatic shape, it is
easily soluble in water, and is characterised by great mildness and permanency
(constancy).
The analysis of this salt shows-

page_text: crystallises very beautifully out of a solution containing hydrochloric acid in
octahedrons resembling alum. It is also very soluble in water, and of a mild
constitution. It is noteworthy that it does not appear to be isomorphic with the
corresponding potash salt. The analysis of this salt, which is easily reudered
impure by small quantities of the compound 2 SbF, Am,SO„, gave as a result-
The double fluoride of sulphate of soda and antimony 2 SbF¸ Na,SO could not
hitherto be obtained in a crystalline form.
As may be seen from the above explanation, these new double fluorides of
antimony and alkaline sulphates exceed the crystalline salts hitherto known with
one molecule of SbF, by about 11 per cent. of their antimony contents.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, as communicated to me by
my foreign correspondent, I declare that what I claim is :-
A process for making double antimony salts of fluoride of antimony and alkaline
sulphates, with or without the addition of hydrochloric acid, by using such pro-
portionate quantities that compounds result of the composition 2 SbF, M,SO, as
representatives of which the double fluoride of antimony and sulphate of
potash 2 SbF, K,SO, and the double fluoride of antimony and sulphate of ammonia
may be cited.
Don T 1902
WM. P. THOMPSON & Co.,
Agents for the Applicant.