The Manufacture and Production of a Sulpho-acid suitable for Dyeing and Printing.
Year: 1890

page_text: Date of Application, 19th Sept., 1890
Complete Specification Left, 17th June, 1891-Accepted, 18th July, 1891
PROVISIONAL SPECIFICATION.
The Manufacture and Production of a Sulpho-acid suitable for
Dyeing and Printing.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
Middlesex, Gentleman do hereby declare the nature of this invention which has
been communicated to me from abroad by The Badische Anilin and Soda Fabrik of
Ludwigshafen-on-Rhine in the Empire of Germany to be as follows:-
In the Specification to Letters Patent No. 15,259 of the year 1888 granted to
me I have described three sulpho-acids of a red basic naphthalene colouring matter,
differing from one another in their degrees of solubility and other properties. Of
these, the disulpho acid and the "higher sulpho acid" which is readily soluble in
cold water dye wool from the acid bath a beautiful bluish-red colour, and the
former of them has a wide application in the dyeing industry, being known in
commerce under the name of "azo-carmine."
In their further investigations of these compounds, my foreign correspondents
have discovered a new dyestuff, of valuable properties, which fixes itself upon wool
from the acid bath giving yellowish-red shades and which results from the action
of diluted sulphuric acid or of certain other mineral acids upon the above named
"higher sulpho acid."
The production of the new dyestuff, from the said "higher sulpho acid " by
treatment with diluted sulphuric acid, appears to take place most readily at a
temperature of about from one hundred and seventy five to one hundred and eighty
degrees Centigrade and it is preferred to use sulphuric acid diluted to such an
extent that it boils at about this temperature, that is to say, an acid containing
about seventy five per cent. sulphuric acid (H,SO,) and the rest water.
If weaker
acid be used the production takes place more slowly, and if it be desired to work
at the above temperatures with such acids the apparatus must be closed and the
mixture must be heated under pressure.
As a convenient means of illustrating the nature of this invention I give the
following example for the production of the new sulpho acid, without binding
myself to details. The parts are by weight.
Mix about ten parts of the sodium salt of the aforesaid "higher sulpho acid"
with about one hundred and fifty parts of diluted sulphuric acid (containing about
seventy five per cent. H₂SO) and boil the mixture in a vessel fitted with a reflux
condenser. for about sixteen hours or until a sample withdrawn and diluted with
about ten times the quantity of water gives a copious precipitate and the mother
liquor on pouring onto filter paper is seen to possess a yellowish red colour. Cool
and add the mixture to about one hundred and fifty parts of ice and then filter
and press. Mix the press-cakes with sufficient caustic soda-lye to make them
alkaline and then dissolve in about two hundred and fifty parts of boiling water,
filter the solution, to get rid of insoluble impurities, and acidify with dilute sulphuric
acid: Collect the colouring matter thus precipitated on the filter and wash with
water. To obtain the dye in its mercantile form of sodium salt mix the paste thus
obtained with calcined soda, taking about twelve parts of soda for every hundred
parts of dry substance in the paste. Dry the mass and grind it to powder.
This sodium salt is a yellow-brown to brown-red powder, rather readily soluble
in cold, readily soluble in hot water giving a yellowish-red solution.
Dated' this 19th day of September 1890.
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, Agents.

page_text: COMPLETE SPECIFICATION.
The Manufacture and Production of a Sulpho-acid suitable for
Dyeing and Printing.
I JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
Middlesex Gentleman do hereby declare the nature of this invention which
has been communicated to me from abroad by The Badische Anilin and Soda
Fabrik of Ludwigshafen on Rhine in the Empire of Germany and in what
manner the same is to be performed to be particularly described and ascertained
in and by the following statement :-
In the Specification to Letters Patent No. 15259 of the year 1888 granted to
me I have described three sulpho-acids of a red basic naphthalene colouring matter
differing from one another in their degrees of solubility and other properties. Of
these, the disulpho-acid and the "higher sulpho-acid "which is readily soluble in
cold water, dye wool from the acid bath a beautiful bluish-red colour, and the
former of them has a wide application in the dyeing industry being known in
commerce under the name of "azocarmine."
In their further investigations of these compounds my foreign correspondents
have discovered a new dyestuff of valuable properties, which fixes itself upon wool
from the acid bath giving yellowish-red shades, and which results from the action
of diluted sulphuric acid or of certain other mineral acids upon the above named
"higher sulpho-acid."
The production of the new dyestuff, from the said "higher sulpho-acid" by
treatment with diluted sulphuric acid, appears to take place most readily at a
temperature of about from one hundred and seventy five to one hundred and
eighty degrees Centigrade and it is preferred to use sulphuric acid diluted to such
an extent that it boils at about this temperature, that is to say, an acid containing
about seventy five per cent. of sulphuric acid (H₂SO) and the rest water. If
weaker acid be used, the production takes place more slowly, and if it be
desired to work at the above temperatures with such acids, the apparatus must be
closed, and the mixture must be heated under pressure.
As a convenient means of illustrating the nature of this invention and the manner
in which it can be carried into practical effect, I give the following example for
the production of the new sulpho-acid, without binding myself to details. The parts
are by weight.
"
Mix about ten parts of the sodium salt of the aforesaid "higher sulpho acid
with about one hundred and fifty parts of diluted sulphuric acid (containing about
seventy five per cent. H₂SO) and boil the mixture in a vessel fitted with a reflux
condenser for about sixteen hours or until a sample withdrawn and diluted with
about ten times the quantity of water gives a copious precipitate and the mother
liquor on pouring on to filter-paper is seen to possess a yellowish-red colour. Cool,
and add the mixture to about one hundred and fifty parts of ice and then filter and
press. Mix the press-cakes with sufficient caustic soda-lye to make them alkaline
and then dissolve in about two hundred and fifty parts of boiling water, filter the
solution to get rid of insoluble impurities, and acidify with dilute sulphuric acid.
Collect the colouring matter thus precipitated on the filter and wash with water.
To obtain the dye in its mercantile form of sodium salt, mix the paste thus obtained
with calcined soda taking about twelve parts of soda for every hundred parts of
dry substance in the paste. Dry the mass and grind it to powder. This sodium
salt is a yellow-brown to brown-red powder, rather readily soluble in cold water
and readily soluble in hot water, giving a yellowish-red solution.
The hereinbefore mentioned "higher sulpho-acid" is frequently a mixture of a
crystallizable trisulpho-acid, and uncrystallizable sulpho-acid readily soluble in
cold water and either of these products can be used in this invention instead of their
mixture (see Specification 19167 of 1890) the process being conducted in either

page_text: case in the same way as that hereinbefore explained, and the dyes obtained, yield
similar shades on wool.
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.
First The manufacture of yellowish-red dyes by the action of dilute sulphuric
acid or its equivalent on certain sulpho-acids of the red basic naphthalene colouring
matter hereinbefore mentioned namely the "higher sulpho-acid described in the
Specification to Letters Patent 15259 of 1888 or the crystallizable trisulpho-acid
frequently contained therein or the said "higher sulpho-acid "free from the
crystallizable trisulpho-acid, all substantially as herein before described.
Second As new articles of manufacture the new dyes such as can be obtained
as hereinbefore described.
DL 17h L
f Tune 1901
J. H. JOHNSON & Co.,
Agents.