Production of Compounds of Antimonic Fluoride with Alkaline Fluorides and the Application thereof and of known Com- ninations of these Substances to Dyeing and Printing.
Year: 1887

page_text: Date of Application, 1st Sept., 1887
Complete Left, 30th May, 1888
Complete Accepted, 20th July, 1888
[Communicated from abroad by CARL WACHENDORFF, of Oestrich on the Rhine,
Germany, Doctor of Philosophy, and Partner in the firm of Rudolph Koepp
& Co.. Manufacturers.]
Production of Compounds of Antimonic Fluoride with Alkaline
Fluorides and the Application thereof and of known Com-
ninations of these Substances to Dyeing and Printing.
ninations of these substances to Dyeing ana
I, CHARLES DENTON ABEL of No. 28 Southampton Buildings, Chancery Lane in the
County of Middlesex, Consulting Engineer and Patent Agent do hereby declare the
nature of this invention to be as follows:-
It has been, for some time since, attempted to find a cheaper substitute for the
costly tartar emetic in printing fabrics, but the substitutes proposed have not proved
efficaceous.
Antimonic tri chloride decomposes with water and of the antimonic oxide separated
only a small portion is taken up by the fibre.
The alkaline glycerine Antimony solution has the disadvantage of alkaline reaction.
Antimonic oxalate is only used with soft water on account of the separation of
oxalate of lime if hard water be used.
Antimonic fluoride is very unstable in the solid form; it gives off hydrofluoric acid
and it can therefore only be used commercially as an aqueous solution. For transport
however receptacles of metal glass porcelain or earthenware cannot be used as they
are all attacked by the Antimonic fluoride.
This alone would cause an insurmountable difficulty in its technical application.

page_text: According to the present invention the above difficulties are avoided by forming
combinations of Antimonic fluoride with some of the alkaline fluorides and alkaline
chlorides.
These compounds are of a constant nature and have therefore no detrimental effect
upon the usual means of packing; they crystallize and dissolve readily in water,
they do not injure animal or vegetable fibre, and form with tannin and dye stuffs just
as pure and fine colours as tartarised antimony, which they closely resemble both in
their properties and mode of application.
As, furthermore, they contain partly just as much, partly more oxide of antimony
than the tartar emetic and are prepared at less cost they should be employed in
preference to this.
The preparation of the said antimonie Anoride with the alkaline Anorides is ас
NH. Fl. Sb Fl, and 3 NH. Fl. Sb Fl.
For preparing the first compound 150 Kilos of antimonic oxide are dissolved in
200 Kilos of hydrofluoric acid of 30 per cent., to which is added an aqueous solution a
of 37 Kilos of ammonium fluoride; or the antimonic oxide is dissolved in 270 Kilos
of hydrofluoric acid of 30 per cent., to which is added 57 Kilos of ammonia of 30 per cent.
After evaporation the compound NH, Fl. Sb F, separates in small scales readily
soluble in water.
Tri-ammonium antimonic fluoride 3 NH, Fl. Sb Fl, is only formed if an excess of 4
ammonium fluoride is present, otherwise it is formed with the obvious alterations, in
the same manner as the tri-potassic antimonic fluoride 3 K Fl Sb Fl..
APPLICATION OF THE SAID COMBINATIONS OF ANTIMONIO FLUORIDE WITH ALKALINE
FLUORIDES TO DYEING AND PRINTING.
The fabrics, yarns &c. to be dyed or printed in colors are first impregnated or 4
printed upon with tannin or tanning materials, or with colors containing the same, and
are then, either before or after dyeing or printing them, passed through an aqueous
solution of one of the above named antimony compounds, or they may be first passed
through the antimony bath and then be treated with coloring matters containing
tannin or tanning substances.
E

page_text: Generally speaking therefore the application of these antimony compounds is the
same as that of the tartar emetic.
The quantity of the antimony compounds employed for the solution depends upon
the proportion of antimonic oxide contained in them. No antimonic oxide separates
on dissolving the bath remaining clear. On the other hand the antimonic oxide is
taken up very rapidly and perfectly by the fibre so that the bath can always be
renewed without loss of antimonic mordant.
In addition to the above described new compounds of antimonic fluoride with
alkaline fluorides and chlorides it has been found by my foreign correspondent
that the compounds of antimonic fluoride. with alkaline fluorides prepared by
F. A. Fluckinger in 1852 (see Paggendorfs Annalen 87 p. 245) are also applicable
as mordants for dyeing and printing. These are the combinations of antimonic
fluoride with potassic fluoride, K Fl. Sb Fl and 3 K Fl. Sb Fl,; with sodic fluoride
3 Na Fl. Sb Fl,; and with Ammonium Fluoride 3 NH, Fl. Sb Fl.
It is only as regards their physical properties, in particular their powers of
crystallisation, that these are inferior to those above described.
Dated this 1st dose of Santember 1887
ABEL & IMRAY,
Agents for the Applicant.

page_text: Production of Compounds of Antimonic Fluoride with Alkaline
Fluorides and the Application thereof and of known Com-
binations of these Substances to Dyeing and Printing.
I, CHARLES DENTON ABEL of No. 28 Southampton Buildings, Chancery Lane in
the County of Middlesex, Consulting Engineer and l'atent Agent 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 :-
It has been, for some time since, attempted to find a cheaper substitute for the costly
tartar-emetic in printing fabrics, but the substitutes proposed have not proved
efficaceous.
Antimonic trichloride decomposes with water and of the antimonic oxide separated,
only a small portion is taken up by the fibre.
The alkaline glycerine Antimony solution has the disadvantage of alkaline
reaction.
Antimonic oxalate is only used with soft water on account of the separation of
oxalate of lime if hard water be used.
Antimonic fluoride is very unstable in the solid form; it gives off hydrofluoric
acid and it can therefore only be used commercially as an aqueous solution. For
transport however receptacles of metal, glass, porcelain, or earthenware cannot be used
as they are all attacked by the Antimonic fluoride.
This alone would cause an insurmountable difficulty in its technical application.
According to the present invention the above difficulties are avoided by forming
combinations of Antimonic fluoride with some of the alkaline fluorides.
These compounds are of a constant nature and have therefore no detrimental effect
upon the usual means of packing; they crystallize and dissolve readily in water, they
do not injure animal or vegetable fibre, and form with tannin and dye stuffs just as
pure and fine colours as tartarised antimony, which they closely resemble both in their
properties and mode of application.
As furthermore, they contain partly just as much, partly more oxide of antimony
than the tartar emetic and are prepared at less cost, they should be employed in
preference to this.
The preparation of the said antimony fluoride with the alkaline fluorides is as
follows:-
Z

page_text: For preparing this compound, 50 kilos oxide of antimony are dissolved in
200 Kilo of hydrofluoric acid of 30 per cent. and 232 Kilos of carbonate of potash
are added.
Or 150 Kilos Antimonic oxide are treated with 470 Kilos of hydrofluoric acid of
30 per cent. to which are added 276 Kilos of carbonate of potash.
In both cases there is a considerable excess of potassic fluoride over and above the
quantity theoretically required.
The solution obtained by the one or other of those methods is evaporated to
crystallisation, and after the crystals have been separated from the mother lye and
dried, they are treated in the known manner.
(h) Prenaration of sodic-antimionic fluoride
soluble in water.
Triammonium antimonic fluoride 3 NH, Fl Sb Fl,, is only formed if an excess of
antimonic fluoride is present, otherwise it is formed with the obvious alterations in
the same manner as the tripotassic antimonic fluoride 3 K FI Sb Fl.
APPLICATION OF THE SAID COMBINATIONS OF ANTIMONIO FLUORIDE WITH ALKALINE
FLUORIDES TO DYEING AND PRINTING.
The fabrics, yarns &c. to be dyed or printed in colors are first impregnated or
printed upon with tannin or tanning materials, or with colors containing the same,
and are then, either before or after dyeing or printing them, passed through an aqueous
solution of one of the above named antimony compounds, or they may be first passed
through the antimony bath and then be treated with coloring matters containing
tannin or tanning substances.
Generally speaking therefore, the application of these antimony compounds is the
same as that of the tartar emetic.
The quantity of the antimony compounds employed for the solution depends upon
the proportion of antimonic oxide contained in them. No antimonic oxide separates
on dissolving the bath remaining clear. On the other hand the antimonic oxide is
taken up very rapidly and perfectly by the fibre so that the bath can always be
renewed without loss of antimonic mordant.
In addition to the above described new compounds of antimonic fluoride with
alkaline fluorides it has been found by my foreign correspondent that the compounds
of antimonic fluoride with alkaline fluorides prepared by F. A. Fluckinger in 1852
(see Poggendorfs Annalen 87 p. 245) are also applicable as mordants for dyeing and
printing. These are the combinations of antimonic fluoride with potassic fluoride:
K Fl. Sb Fl, and 3 K Fl. Sb F), with sodic fluoride 3 Na Fl. Sb Fl, and with
Ammonium fluoride 2 NH, FI Sb Fl..
4
It is only as regards their physical properties, in particular their powers of
crystallisation, that these are inferior to those above described.

page_text: They are applied in the same manner as described with reference to the new
compounds.
Having now particularly described and ascertained the nature of this invention
and in what manner the same is to be performed I declare that what I claim is :-
1. The production of the herein described new compounds of antimonic fluoride
with alkaline fluorides.
2. The application of the herein described new compounds of antimonic fluoride
with alkaline fluorides, as also of the hereinbefore mentioned compounds of antimnonic
fluoride and alkaline fluorides prepared by F. A. Fluckinger, to dyeing and printing,
substantially as herein described.