A New or Improved Material for use in the Production of Colouring Matters.
Year: 1891

page_text: Date of Application, 14th Feb., 1891
Complete Specification Left, 28th Oct., 1891-Accepted, 28th Nov., 1891
PROVISIONAL SPECIFICATION.
A New or Improved Material for use in the Production of Colouring
Matters.
I, IVAN LEVINSTEIN of Minshull Street Manchester in the County of Lancaster,
Manufacturing Chemist, do hereby declare the nature of this invention to be as
follows:-
When naphthaline is heated at comparatively high temperatures with from four
to five parts of concentrated sulphuric acid, several naphthaline disulpho acids are.
obtained which are known as alpha and beta-naphthaline-disulpho acids. (Ebert
and Merz, Berichte IX., 592.) It is also known that upon treating these naphtha-
linedisulpho acids with nitric acid and converting the nitrodisulpho acids thus
obtained into amidonaphthalinedisulpho acids, a mixture of amidonaphthalinedisulpho
acids is obtained.
This invention relates to a new naphthylaminedisulpho acid which differs from
any of the similar acids hitherto known and which is produced by a different
process to those which have been hitherto adopted.
In proceeding according to my improvements, I may add the sodium salt of
alpha-naphthaline-monosulpho acid to concentrated sulphuric acid which has
previously been heated to from 150 to 160 degrees Centigrade and keep the mixture
at this temperature for several hours. If the new disulpho acid thus produced is
then treated with nitric acid a new mononitrodisulpho acid results, which upon
reduction gives a new amidonaphthalinedisulpho acid.
This new acid possesses valuable properties, and it is especially useful in the
production of colouring matters.
Similar results may be obtained according to these improvements by first con-
verting naphthaline into alpha-naphthalinemonosulpho acid and by heating this acid
for several hours with an addition of anhydrous sodium or potassium sulphate at a
temperature of about 150 to 160 degrees Centigrade.
In carrying out my invention I may proceed as follows-
EXAMPLE I.
100 pounds of alpha-naphthalinemonosulphonate of soda are quickly added
with stirring to 300 pounds of concentrated sulphuric acid previously heated to
150 degrees Centigrade, and the mixture is kept at this temperature for from two
to four hours, when the alpha-naphthalinemonosulpho acid will have been converted
into a new naphthalinedisulpho acid. After cooling to about from 10 to 20 degrees
Centigrade, 45 pounds of nitric acid (40 degrees Baumé) are allowed to run into the
acid mixture, care being taken to stir the mixture well and not to allow its tempera-
ture to rise above 40 degrees Centigrade. After all the nitric acid has been added,
the mixture is carefully poured into 700 pounds of a saturated solution of ordinary
salt, when the new nitronaphthalinedisulpho acid will separate in a crystalline form.
This acid is then filtered off and washed with concentrated salt solution, in which it
is only sparingly soluble, and the crystals thus separated and washed are afterwards
pressed. The pressed nitro-acid is dissolved in 400 pounds of hot water and reduced.
boiling with 50 parts of iron borings. The solution is kept at the boiling tempera-
ture until the reduction is completed and it is afterwards made alkaline, for
example, by means of soda, filtered, concentrated by boiling, and left for crystallisa-
tion. The crystals are then filtered, pressed, and dried, and represent the sodium
salt of the new naphthylaminedisulpho acid.

page_text: EXAMPLE II.
60 pounds of finely powdered naphthaline are added to 240 pounds of cold con-
centrated sulphuric acid and stirred until a sample of the mixture dissolves in water.
The mass is then heated, preferably with an addition of anhydrous sulphate of soda
for a few hours at a temperature of 150 to 160 degrees Centigrade. The further
treatment of the acid mixture is then proceeded with as directed for Example I.
Dat this 12th day of February A D 1891
WILLIAM E. HEYS,
Agent for the Applicant.
COMPLETE SPECIFICATION.
A New or Improved Material for use in the Production of Colouring
Matters.
I, IVAN LEVINSTEIN of Minshull Street Manchester in the County of Lancaster,
Manufacturing 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
When naphthaline is treated at comparatively high temperatures with from four
to five parts of concentrated sulphuric acid, several naphthalinedisulphoacids are
obtained which are known as alpha- and beta-naphthalinedisulphoacids. (Ebert
and Merz, Bericht IX., 592.) It is also known that upon treating these naphtha- 2
linedisulphoacids with nitric acid and converting the nitrodisulphoacids thus formed
into amidonaphthalinedisulpho-acids, a mixture of amidonaphthalinedisulpho-acids
is obtained.
This invention relates to a new naphthylaminedisulpho-acid which differs from
any of the similar acids hitherto known and which is produced by a different 2
process or different processes to any of those which have been adopted up to the
present time.
In proceeding according to my invention, I may add the sodium salt of alpha-
naphthalinemonosulpho-acid to concentrated sulphuric acid which has been
previously heated to about from 150 to 160 degrees Centigrade, and keep. the
mixture at this temperature for several hours. If the new disulpho-acid thus
produced is then treated with nitric acid in the usual manner, a new mononitrodi-
sulpho-acid results which upon reduction gives the new amidonaphthalinedisulpho-
acid, naphthylaminedisulpho-acid.
This new acid possesses valuable properties and it is especially useful in the
production of colouring matters.
Similar results may be obtained according to this invention by first converting
naphthaline into alpha-naphthalinemonosulpho-acid and by heating this acid for
several hours with an addition of anhydrous sodium or potassium sulphate at a
temperature of about 150 to 160 degrees Centigrade.
In carrying out my invention I may proceed as follows-
EXAMPLE I.
100 pounds of alpha-naphthalinemonosulphonate of sodium are quickly added
with stirring to 300 pounds of concentrated sulphuric acid previously heated to
about 150 degrees Centigrade, and the mixture is kept at this temperature for from
two to four hours, when the alpha-naphthalinemonosulpho-acid will have been
converted into the new naphthalinedisulpho-acid. After cooling to about from 10
to 20 degrees Centigrade, 45 pounds of nitric acid (40 degrees Beaumé) are
allowed to run into the acid mixture, care being taken to stir the mixture well and
not to allow its temperature to rise above about 40 degrees Centigrade. After all.

page_text: the nitric acid has been added, the mixture is carefully poured into 700 pounds of a
saturated solution of ordinary salt, when the new nitronaphthalinedisulpho-acid will
separate in a crystalline form. This acid is then filtered off and washed with
concentrated salt solution in which it is only sparingly soluble, and the crystals
thus separated and washed are afterwards pressed. The pressed nitro-acid is then
dissolved in 400 pounds of hot water and reduced boiling with 50 pounds of iron
borings. The solution is kept at the boiling temperature until the reduction is
completed and it is afterwards made alkaline for example by means of soda, filtered,
concentrated by boiling, and left for crystallisation. The crystals are then filtered
off, pressed and dried, and represent the sodium salt of the new naphthylaminedi-
sulpho-acid.
EXAMPLE II.
60 pounds of finely divided naphthaline are added to 240 pounds of cold concen-
trated sulphuric acid and the mixture is stirred until a sample of it dissolves in cold
water. The mass is then heated, preferably with an addition of anhydrous
sulphate of soda for from two to four hours or so long as may be necessary, at a
temperature of about 150 to 160 degrees Centigrade. The further treatment of the
acid mixture is then proceeded with as directed for Example I.
I have described two examples of the methods by which the new products
may be obtained, but it is obvious that other processes might be adopted to obtain
similar results, and I desire it to be understood therefore that I do not limit myself
to the hereinbefore described methods for obtaining the new acid and its salts.
Having now particularly described and ascertained the nature of my said inven-
tion and in what manner the same is to be performed, I declare that what I
claim is,―
1. As a new article of manufacture, naphthylaminedisulpho-acid, prepared
substantially as hereinbefore described.
2. As a new article of manufacture, salts of naphthylaminedisulpho-acid, prepared
substantially as and for the purpose herein before described.
3. The manufacture of naphthylaminedisulpho-acid and its salts, substantially as
and by the processes herein before described.
Dated this 27th day of October A.D. 1891.
WILLIAM E. HEYS,
Agent for the Applicant.