Improvements in the Manufacture of Colouring Matters.
Year: 1891

page_text: Date of Application, 24th July, 1891
Complete Specification Left, 8th Apr., 1892-Accepted, 18th June, 1892
PROVISIONAL SPECIFICATION.
[Communicated from abroad by KALLE & Co., of Biebrich on the Rhine, in the
Empire of Germany, Manufacturers.]
Improvements in the Manufacture of Colouring Matters.
I, HENRY HARRIS LAKE, of the firm of Haseltine Lake & Co., Patent Agents,
45 Southampton Buildings, in the County of Middlesex, do hereby declare the
nature of this invention to be as follows:-
In British Letters Patent No. 15259 A.D. 1888 of the Badische Anilin and
Sodafabrik the products of the reaction of fuming sulpharic acid on phenylrosin-
duline are described. I have now found that valuable products can be obtained by
treating the same base with concentrated sulphuric acid.
If one part of phenylrosinduline is heated with about 10 to 20 parts of concen-
trated sulphuric acid to a temperature of 150-170 degrees centigrade the
disulphoacid mentioned in Claim 2 of the above mentioned patent is produced.
This disulphoacid is then converted by further heating into a new disulphoacid
(which may be termed ẞ disulphoacid) of essentially different propertice, it is very
easily soluble in water and alcohol, and dyes wool more bluish shades than the
disulphoacid hitherto known. Whereas the salts of the latter disulphoacid when
heated with water under pressure give the rosindone C.HNO, the salts of the
new disulphoacid give by the same treatment a monosulphoacid of the said
rosindone and of the formula C„H₁N,OSO,H. If the hereinbefore mentioned
mixture of phenylrosinduline with concentrated sulphuric acid is further heated, I
finally obtain a sulphoacid which is not precipitated from its aqueous solution by
mineral acids, thus essentially differing from the ẞ disulphoacid.
In preparing the phenylrosinduline-ß disulphoacid I proceed as follows: one
part of phenylrosinduline is dissolved in fifteen parts of concentrated sulphuric acid
and the mixture is heated for about 12 hours to 170 degrees centigrade. The
reaction is finished when a sample precipitated with water and filtered is easily
soluble in cold pure water. The mixture is then poured into 75 parts of water, the
precipitate is filtered off, dissolved in alcohol, thereby separating the a disulphɔacid
which may not have been transformed and this alcoholic solution is then evaporated
to crystallization. The ß disulphoacid gives like the phenylrosinduline and its
already known sulphoacids a bright green solution with concentrated sulphuric
acid. In its behaviour it resembles the trisulphoacid, forming the subject of German
Patent B 11280 applied for by the Badische Anilin- and Sodafabrik and filed on
the 9, April 1891, the solubility of the ẞ disulphoacid being however somewhat
inferior.
In practice it is not necessary to separate the herein before described sulphoacids.
After the mixture is heated for a sufficiently long time and poured into water, a
sodium salt is produced by adding common salt and the dyestuff thus separated is
then filtered, pressed and dried.
Dated this 24th day of July 1891.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.

page_text: COMPLETE SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I HENRY HARRIS LAKE of the firm of Haseltine Lake & Co. Patent
Agents 45 Southampton Buildings in the County of Middlesex 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:-
In British Letters Patent No. 15259 A.D. 1888 of the Badische Anilin- and
Sodafabrik the products of the reaction of fuming sulphuric acid on phenylrosin-
duline are described. I have now found that valuable products can be obtained by
treating the same base with concentrated sulphuric acid.
If one part of phenylrosinduline is heated with about 10 to 20 parts of concen- |
trated sulphuric acid to a temperature of 150-170 degrees centigrade this
disulphoacid mentioned in Claim 11 of the above mentioned patent is produced.
This disulphoacid is then converted by further heating into a new disulphoncid
(which may be termed ẞ disulphoacid) of essentially different properties it is very
easily soluble in water and alcohol and dyes wool more bluish shades than the
disulphoacid hitherto known. Whereas the salts of the latter disulphoacid when
heated with water under pressure give the rosindone CH₁N,O the salts of the
new disulphoacid give by the same treatment a monosulphoacid of the said
rosindone and of the formula C₂H₁₂O SO₂H. If the hereinbefore mentioned
mixture of phenylrosinduline with concentrated sulphuric acid is further heated I
finally obtain a sulphoacid which is not precipitated from its aqueous solution by
mineral acids, thus essentially differing from the ẞ disulphoacid.
14
14
In preparing the phenylrosinduline-ẞ-disulphoacid I proceed as follows: one
part of phenylrosinduline is dissolved in fifteen parts of concentrated sulphuric acid
and the mixture is heated for about 12 hours to 170 degrees centigrade. The
reaction is finished when a sample precipitated with water and filtered is easily
soluble in cold pure water. The mixture is then poured into 75 parts of water the
precipitate is filtered off, dissolved in alcohol, thereby separating the a-disulphoacid
which may not have been transformed and this alcoholic solution is then evaporated
to crystallization. The B-disulphoacid gives like the phenylrosinduline and its
already known sulphoacids a bright green solution with concentrated sulphuric
acid. In its behaviour it resembles to the trisulphoacid. forming the subject of
German Patent B 11280 applied for by the Badische Anilin and Sodafabrik and
filed on the 9th April 1891, the solubility of the B-sulphoacid being however
somewhat inferior.
In practice it is not necessary to separate the hereinbefore described sulphoacids.
After the mixture is heated for a sufficiently long time and poured into water, a
sodium salt is produced by adding common salt and the dyestuff thus separated is
then filtered pressed and dried.
I am well aware that sulphoacids easily soluble in water have already been
prepared by treating the rosinduline C₂H№¸ with fuming sulphuric acid.
19 3
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 correspondents I declare that what I claim is.
The production of sulphoacids easily soluble in water by treating the rosin-
duline C₂,H,N, with concentrated sulphuric acid substantially as above specified.
Dated this 8th day of April 1892.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.