Year: 1887

page_text: Date of Application, 19th Sept., 1887
Complete Specification Left, 16th June, 1888
Complete Specification Accepted, 3rd Aug., 1888
I, CHARLES SAMUEL BEDFORD of Sycamore Lodge, Leeds in the County of York,
Chemist, do hereby declare the nature of this invention to be as follows:-
This invention has for its object the manufacture of colouring matters from the
combination of certain diazo compounds with the active principles of certain woods,
more especially of those contained in fustic (old fustic yellow wood), young fustic and
mahogany. The diazo compounds especially preferred for this purpose are the
chloride, sulphate, nitrate, or sulphonic acid of diazo-benzene or of diazo-toluene, of
diazo naphthalene or of diazo xylene.
The following is an illustration of the working of the process:-
In the preparation of the colour 1,000 lbs. of rasped fustic are stripped by successive
boils with water, with or without the addition of alkali or acid, preferably with about
3 per cent. of sodium carbonate (soda crystals) divided in the first two liquors; if
more be used, the colouring matter dyes a flatter shade. It generally requires four
boils to strip the wood and the successive liquors are mixed together, strained, passed
through a cooling worm, and run into a large open vat. If the fustic has been stripped
by water or acidified water the liquor must be rendered slightly alkaline before the
addition of the diazo compound.
38 lbs. of aniline are poured into an open tub containing about 1,000 lbs. water and
100 lbs. hydrochloric acid, and the whole stirred. A solution of 38 lbs. sodium
nitrite is then run in with constant stirring to form the diazo-chloride. After standing
a little while this liquor is then gradually run by means of a spigot or other suitable
apparatus into the fustic liquor, which is now kept constantly stirred while the
colouring matter forms.

page_text: After the whole has been run in, a small quantity of sulphuric acid is added, when
the whole of the colour is at once precipitated and may be collected on a filter and
dried with the addition of a little alkali to make it soluble, or it may be used as
a paste.
To prepare the brown naphthaline colour; 50 lbs. of naphthylamine are dissolved
by boiling in about 2000 lbs. water acidified with 160 lbs. of hydrochloric acid, then
cooled, and the liquor made up to 400 lbs., it is then diazotised with 40 lbs. sodium
nitrite.
The fustic liquor is then treated with this solution, as above described.
In place of extracting the colouring matter from the fustic by successive boilings,
the extraction can be accomplished on the methodical principle, in which the fresh
-boiling water is caused to act on the nearly exhausted wood, and then on less nearly
exhausted material, till it leaves the series or apparatus, after acting on the hitherto
untreated material; in such case also the material as it gets more and more exhausted
meets with water less and less saturated with colour, till it is drawn out of the series
through the newly applied fresh boiling water. In this case the alkali is preferably
added near the middle of the series.
1000
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool,
Agents for the Applicant.

page_text: COMPLETE SPECIFICATION..
New or Improved Colouring Matters and Process of Manufacturing
the same.
I, CHARLES SAMUEL BEDFORD, of Sycamore Lodge, Leeds, in the County of York,
Chemist, 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:-
This invention has for its object, the manufacture of yellow-orange, or brown
colouring matters, from the combination of certain diazo compounds, with the active
principles of fustic (yellow wood), the chief varieties being known as Cuba, Tampico,
Corinto, Maracaibo, Vera Cruz, and Jamaica fustic, also with those contained in
mahogany. The diazo compounds used in the manufacture of these colouring matters
are the salts (that is the chloride, sulphate, nitrate or sulphonic acids) of diazo-benzene,
of diazo-toluene, of diazo-xylene, or of diazo-naphthalene.
The following is an illustration of the working of the process.
In the preparation of the colour from Jamaica fustic:-500 lbs. of the chipped or
rasped wood are placed in a vat provided with a false bottom, and stripped by succes-
sive boilings with water of an hour's duration, with or without the addition of alkali
or acid, preferably with about 3 per cent. of sodium carbonate (soda crystals) divided
in the first two liquors, if more be used, the colouring matter dyes a flatter shade.
It generally requires six boils to strip the wood, and the successive liquors, after
being strained by means of the false bottom, are pumped into a vat at a higher
elevation, provided with a cooling worm and agitator. When the temperature is
reduced sufficiently low, say to 60 degrees Fahrenheit, they are run together in a
large open vat, provided with stirrers. By this method of stripping, the combined
fustic liquors should measure about 860 gallons. About 25 lbs. of aniline, and about
26 lbs. of concentrated sulphuric acid (in the form of aniline sulphate), are placed in
an open tub containing 120 gallons of cold water standing above the fustic liquor.
A solution of about 20 lbs. sodium nitrite (98 per cent.) is then gradually run in with
constant stirring till the sulphate is dissolved, and the diazo-sulphate formed.
This liquor is then run by a perforated pipe or other suitable means into the fustic
liquor, which is kept constantly stirred while the colouring matter forms. Whilst the
diazo liquor is being run in, alkali, preferably sodium carbonate, must be added to
the fustic liquor in order to bring about the required reaction. If the wood has been
stripped with 3 per cent. of soda crystals, a gradual addition of about 5 lbs.
will be sufficient, but if plain water or acidified water has been used, more will be
required.
If the colouring matter does not entirely separate, a few pounds of sulphuric acid
are added, and the precipitate collected in a filter press. The yield is 625 lbs. of a
stiff paste, which may be used for dyeing in paste form, or it may be dried with the
addition of a little alkali to make it soluble, and afterwards ground. The toluene and
xylene colouring matters are produced in a similar manner.
To prepare the brown naphthalene colour-About 33 lbs. of naphthylamine are
dissolved by boiling in about 100 gallons of water, acidified with about 96 lbs. of
hydrochloric acid, then cooled, and the liquor made up to 200 gallons, it is then
diazotisod with about 25 lbs. sodium nitrite.

page_text: The fustic liquor is then treated with the above solution as previously described.
In place of stripping the fustic by successive boilings, the extraction can be accom-
plished on the methodical principle, in which the fresh boiling water is caused to act
on the nearly exhausted wood, and then on less nearly exhausted material, till it leaves
the series or apparatus after acting on the hitherto untreated material; in such case,
also, the material, as it gets more and more exhausted, meets with water less and less
saturated till it is drawn out of the series through the newly applied fresh boiling
water. In this case the alkali is preferably added near the middle of the series.
By this means, more concentrated liquors may be obtained, but it is not advisable to
use too strong extracts.
These colouring matters may also be produced within the fibre, and thus fixed upon
cotton by steeping the material alternately in the diazo solution, and then in the fustic
liquor, until the desired shade is produced.
The colouring matters may also be produced within the fustic wood. In this case, it
is advisable to use rasped wood instead of chipped; as the wood is then more finely
divided, and easier penetrated.
Example:-500 lbs. rasped wood are steeped in the diazo solution prepared with
25 lbs. aniline, 26 lbs. sulphuric acid, and 20 lbs. sodium nitrite, using only sufficient
water to thoroughly moisten the wood, which is repeatedly turned over.
After a short time, and when the diazo solution has thoroughly penetrated the
wood, a slight excess of sodium carbonate is added, and after being thoroughly
incorporated, the wood is drained from excess of moisture, when it is ready for use
in dyeing.
Fustic being a natural product occurring, as stated above, in several varieties, it
differs considerably in strength; the different kinds, therefore, require a slight modifi-
cation in the amount of diazo-compound added.
The above proportions, however, given for Jamaica fustic will enable a works'
chemist, by ascertaining the relative amount of colouring matter in a sample of the
wood used, and in average Jamaica fustic, to proportion the quantity of diazo-compound
with sufficient exactitude.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
:―
1. The herein described new or improved colouring matters formed of a combina-
tion of the active principle of Jamaica fustic, or other like wood, such as described,
with one or more of the chloride, sulphate, nitrate or sulphonic acids of diazo-benzene,
of diazo-toluene, diazo-xylene or diazo-naphthalene, substantially as described.
2. The process of forming the aforesaid colouring matters, substantially as herein
described.
3. The improvement in the process of making colouring matter, which consists in
forming a salt of a diazotised aromatic monamine, by treating the solution of a
slightly acid salt or sulphonic acid of the corresponding amine with sodium nitrite,
and then combining with extract of fustic or mahogany, substantially as described.
4. The improvement in the manufacture of colouring matter, which consists in
treating the comminuted fustic or mahogany wood with a solution of one or more of
the salts of the diazo-compounds of the series, diazo-benzene, diazo-toluene, diazo-
xylene, and diazo-naphthalene, until the wood is thoroughly permeated, and adding
the requisite quantity of alkali, substantially as described.
Dated this 15th day of June 1888
WM. P. THOMPSON & Co.,
Of 6, Lord Street, Liverpool,
Patent Agents for the Applicant..