New Process for the Production of an Amidonaphtholsulphonic Acid.
Year: 1899

page_text: (Communicated from abroad by THE FARBENFABRIKEN vormals FRIEDRICH
BAYER & Co., of Elberfeld, Germany.)
New Process for the Production of an Amidonaphtholsulphonic Acid.
I, HENRY EDWARD NEWTON, of the Office for Patents, 6, Bream's Buildings,
Chancery Lane, in the County of London, Patent Agent, do hereby declare the
nature of this invention to be as follows:-
My foreign correspondents have discovered a new process for the production
of a material described in the Specification to Letters Patent No. 13443% as
alpha-alpha-amidonaphthol-beta-beta-disulphonic acid.
The new process consists in treating alpha,-alpha-dinitro-naphthalene-beta-
beta-disulphonic acid, which is described in the Specification to Letters Patent
No. 15,34690 with sulphites or bisulphites.
In order to illustrate the new process more fully, the following examples are
given, the parts being by weight.
EXAMPLE A.
A mixture prepared from 200 parts of alpha,-alpha,-dinitronaphthalene-beta-
beta, disulphonate of sodium, 400 parts of water, and 1100 parts of a 40 per cent.
sodium bisulphite solution, is heated in an autoclave lined with lead, at from
about 100 to 150 degrees Centigrade, while being continuously stirred, until,
on testing, the quantity of amidonaphthol-disulphonic acid formed during the
process is found to increase no longer. The resulting mass is then stirred into
about 1000 parts of water, rendered slightly alkaline, and filtered, if necessary.
Subsequently it is heated to about from 80 to 90 degrees Centigrade, and finally
acidulated by means of a mineral acid. The acid sodium salt of the alpha-
alpha-amidonaphthol-beta, beta-disulphonic acid is thus separated. After filter-
ing off, pressing, and drying, the same can be used, directly for the preparation
of coloring-matters.
EXAMPLE B.
A mixture prepared from 100 parts of alpha,-alpha,-dinitronaphthalene beta-
beta-disulphonate of sodium, 200 parts of water, and 100 parts of a 40 per cent.
sodium bisulphite solution, is heated in an open vessel lined with lead, and pro-
vided with a stirrer, at from 90 to 100 degrees Centigrade, until the whole
mass has dissolved. Subsequently, about 500 parts of hydrochloric acid of
19 degrees Baumé, are added, with stirring, the acid sodium salt of amidonaphthol-
disulphonic acid being thus separated. After further stirring, the mixture is
cooled, and finally the precipitated salt is isolated by filtration.
The process proceeds in an analogous manner, if neutral salts of sulphurous
acid are employed. In order to illustrate this manner of proceeding, the follow-
ing Example C may be given, the parts being likewise by weight.

page_text: EXAMPLE C.
A mixture prepared from 100 parts of alpha,-alpha-dinitronaphthalene-beta,-
beta-disulphonate of sodium, 400 parts of water, and 400 parts of neutral sodiumi-
sulphite, is boiled in an enamelled vessel provided with a stirrer and a reflux-
condenser. After a short time, the whole mass will have dissolved, an active
evolution of ammonia taking place. Boiling is continued until the ammonia
is almost entirely removed. Subsequently the hot mass is acidulated by means
of hydrochloric acid, the acid sodium salt of alpha₁-alpha-amidonaphthol-beta,-
beta-disulphonic acid being thus precipitated.
As a matter of course, my foreign correspondents do not intend to confine
themselves to the particulars given in the above examples, as these are merely
typical, and can be varied within wide limits.
Thus, for instance, instead of sodium bisulphite used in the above Examples A
and B, other bisulphites, as potassium bisulphite, or solutions of bisulphites of
alkaline earths, may be used.
T1 th: 02.. de of Databou 1900
NEWTON & SON,
Agents for the Applicant.
New Process for the Production of an Amidonaphtholsulphonic Acid.
I, HENRY EDWARD NEWTON, of the Office for Patents, G, Bream's Buildings,
Chancery Lane, in the County of London, Patent 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:―
My foreign correspondents have discovered a new process for the production of
the material described in the Specification of Letters Patent No. 134430, as
alpha,-alpha-amidonaphthol-beta-beta,-disulphonic acid.
The new process consists in treating alpha,-alpha,-dinitro-naphthalene-beta-
beta, disulphonic acid, which is described in the Specification of Letters Patent
No. 15346, with sulphurous acid, or with sulphites or bisulphites.
In order to illustrate the new process more fully, the following examples are
given, the parts being by weight.
EXAMPLE A.
A mixture prepared from 200 parts of alpha,-alpha,-dinitronaphthalene-beta,-
beta-disulphonate of sodium, 400 parts of water, and 1100 parts of a 40 per cent.
sodium-bisulphite solution, is heated in an autoclave lined with lead, at from
about 100 to 150 degrees Centigrade, while being continuously stirred, until,
on testing, the quantity of amidonaphthol-disulphonic acid formed during the
process is found to increase no longer. The resulting mass is then stirred into
about 1000 parts of water, rendered slightly alkaline, and filtered, if necessary.
Subsequently it is heated to about from 80 to 90 degrees Centigrade, and finally
acidulated by means of a mineral acid. The acid sodium salt of the alpha-
alpha-amidonaphthol-beta,-beta,-disulphonic acid is thus separated. After filter-
ing off, pressing, and drying, the same can be used, directly for the preparation
of coloring-matters.
EXAMPLE B

page_text: sodium bisulphite solution, is heated in an open vessel lined with lead, and pro-
vided with a stirrer, at from 90 to 100 degrees Centigrade, until the whole
mass has dissolved. Subsequently, about 500 parts of hydrochloric acid of
19 degrees Bé are added, with stirring, the acid sodium salt of amidonaphthol-
disulphonic acid being thus separated. After further stirring, the mixture is
cooled, and finally the precipitated salt is isolated by filtration.
The process proceeds in an analogous manner, if neutral salts of sulphurous
acid are employed. In order to illustrate this manner of proceeding, the follow-
ing Example C may be given, the parts being likewise by weight.
EXAMPLE C.
A mixture prepared from 100 parts of alpha,-alpha-dinitronaphthalene-beta-
betag-disulphonate of sodium, 400 parts of water, and 400 parts of neutral sodium-
sulphite, is boiled in an enamelled vessel provided with a stirrer and a reflux-
condenser. After a short time, the whole mass will have dissolved, an active
evolution of ammonia taking place. Boiling is continued until the ammonia
is almost entirely removed. Subsequently the hot mass is acidulated by means
of hydrochloric acid, the acid sodium salt of alpha,-alpha,-amidonaphthol-beta.-
beta-disulphonic acid being thus precipitated.
As a matter of course, my foreign correspondents do not intend to confine
themselves to the particulars given in the above examples, as these are merely
typical, and can be varied within wide limits.
Thus, for instance, instead of sodium-bisulphite used in the above Examples A.
and B, other bisulphite, as potassium bisulphite, or solutions of bisulphites of
alkaline earths, may be used.
Having now particularly described and ascertained the nature of the said in-
vention and in what manner the same is to be performed, as communicated to
me from abroad, I declare that what I claim is:.
The new process for the production of alpha,-alpha-amidonaphthol-beta,-beta-
disulphonic acid, which process consists in treating alpha,-alpha,-dinitronaph-
thalene-beta-beta-disulphonic acid, or salts thereof, with sulphurous acid or its
salts, substantially as herein before described.
Dated this 13th dox of Jul 1900