An Improved Method of Fixing Tannate of Titanium on Vegetable Fibre.
Year: 1898

page_text: Date of Application, 13th Apr., 1898
Complete Specification Left, 13th Jan., 1899-Accepted, 11th Mar., 1899
PROVISIONAL SPECIFICATION.
An Improved Method of Fixing Tannate of Titanium on Vegetable
Fibre.
We, HENRY WARD KEARNS, Baxenden House, Baxenden, Accrington, Dyer,
and JOSEPH BARNES, Marl Bank, Accrington, Public Analyst, both in the County
of Lancaster, do hereby declare the nature of this invention to be as follows:-
When a soluble salt of titanium is mixed with a solution of tannin there is
formed a yellowish orange compound namely tannate of titanium. This compound
may or may not remain in solution according to circumstances. When, for
example, there is also present a soluble chloride or a soluble sulphate most or all
of the tannate of titanium will become precipitated, whereas on the other hand,
when the liquors are free from soluble chlorides and sulphates and there is at
the same time present an organic acid, such as oxalic acid, the tannate of titanium
remains in solution.
Hydrofluoric acid is also very effective in holding the tannate of titanium in
a soluble condition.
Now this invention consists in soaking or otherwise preparing the vegetable
fibre with a suitably prepared solution of tannate of titanium and afterwards
passing the vegetable fibre into a bath charged with a saline material such as
common salt, Glauber's salt, sal-ammoniac, chloride of calcium and the like. In
this manner the tannate of titanium may be fixed on the vegetable fibre easily
and expeditiously.
Dated this 12th day of April 1898.
HENRY WARD KEARNS,
JOSEPH BARNES.
COMPLETE SPECIFICATION.
An Improved Method of Fixing Tannate of Titanium on Vegetable
Fibre.
We, HENRY WARD KEARNS, of Baxenden House, Baxenden, near Accrington,
Turkey Red Dyer, and JOSEPH BARNES, of Marl Bank, Manchester Road, Accring-
ton, Public Analyst, both in the County of Lancaster, 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:-
When a soluble salt of titanium is mixed with a solution of tannin there is
formed a yellowish orange compound namely tannate of titanium. This compound
may, or may not remain in solution according to circumstances.

page_text: When, for example, there is also present a soluble chloride or a soluble sulphate
most or all of the tannate of titanium will become precipitated, whereas on the
other hand, when the liquors are free from soluble chlorides and sulphates, and
there is at the same time present an organic acid, such as oxalic acid, the tannate
of titanium remains in solution. Hydrofluoric acid is also very effective in
holding the tannate of titanium in a soluble condition.
The usual method employed for fixing tannate of titanium on vegetable fibre
consists shortly in first preparing the yarn or cloth in a bath of tannin such as a
solution of tannic acid, decoction of sumac or other bodies containing tannin,
and then squeezing the excess of liquor from the fibre and passing this same fibre
into a bath containing a soluble salt of titanium by which operation the tannate
of titanium is at once formed in an insoluble condition upon or within the fibre.
This process is more or less uncertain because the quantity of tannin taken up
cannot be determined with exactitude, it is also slow, as the fabric or fibre has to
remain in the solution for some hours and the process is therefore unnecessarily
expensive.
Now our invention consists principally in first treating the vegetable fibre with
a suitably prepared solution of tannate of titanium, and afterwards rendering
the tannate insoluble by passing the said fibre into a bath charged with a saline
material such as common salt, Glauber's salt, sal-ammoniac, chloride of calcium
or the like. In this manner the tannate of titanium may be fixed on the vegetable
fibre more easily and expeditiously.
We find this to be a more expeditious and economical mode of working than
the usual process.
First because it is not necessary to allow the fibre to remain
soaking for a long time, as is the case when the simple tannin bath is used, and
in the second place practically the whole of the tannin is utilized, and the final
result is more certain.
A suitably soluble form of tannate of titanium may be prepared by dissolving
the precipitated compound, which has been previously washed until it is free from
soluble chlorides or sulphates, in a warm solution of oxalic acid, or of tartaric
acid, but the method which we find convenient according to our invention is as
follows:-
A liquor of crude acid oxalate of titanium is made by dissolving crude acid
sodium titanate (obtained by fluxing ground rutile with caustic soda and washing
away the excess of caustic soda with water) in oxalic acid for which purpose we
take sufficient of the wet paste corresponding to 7 lbs. of air dried material (the
water in the paste being previously estimated by drying a weighed portion of
the paste and then weighing again when it has become dry by exposure to the air)
and dissolve it in a warm solution of 14 lbs. of oxalic acid in as little water as will
conveniently effect solution. The solution of the acid-sodium titanate in the
oxalic acid is hastened by occasional stirring. This liquor when cold is let down
with water to 38° Twaddel. We now dissolve 10 lbs. of commercial tannic acid
in about 8 gallons of water and then add 8th pints of the crude acid titanium
oxalate. Such a liquor we call tannin-titanium-oxalate. To dye yarn (or cloth)
a full yellowish orange shade we reduce the tannin-titanium oxalate to 20 Twaddel,
and steep the yarn (or cloth) therein for several minutes, then take out, wring up
or squeeze and at once plunge into a salt hath containing 4 lb. of common salt
(sodium chloride) per gallon of water and maintained at a temperature of 160°
Fahrenheit. A few turns (about five minutes) suffices to fix the tannate of
titanium on the fibre. For paler shades we use a weaker solution of tannin-
titanium-oxalate down to one sixteenth of a degree Twaddel for light creams.
For light shades it is as well to add from 7 to 10 grains of oxalic acid to each
gallon of salt bath in order to prevent any possible fixation on the fibre of tannate
of iron.
In the above described process a solution of fluoride of titanium may be used
in place of the acid oxalate of titanium.
Of course the yarn (or cloth) so dyed may be subsequently dyed (without any

page_text: further mordanting operation) by the basic colours for which purpose the bath
of tannin-titanium-oxalate at half a degree Twaddel will be found ample for
medium shades. When precipitated tannate of titanium is dissolved in tartaric
acid it may be printed on calico dried, and the tannate of titanium pattern fixed
in a hot salt bath.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed we declare that what
we claim is: :-
The improved method of fixing tannate of titanium on vegetable fibre con-
sisting in first treating the said fibre with tannate of titanium in a soluble
condition, and afterwards treating the same in a saline bath so as to change the
soluble tannate of titanium into an insoluble condition upon and within the fibres,
substantially as hereinbefore described.
GEO. DAVIES & SON
Agents for the Applicants,
4, St. Ann's Square, Manchester.