A PROCESS OR PROCESSES FOR PRODUCING BETANAPHTOL-DISULPHO-ACIDS, SEPARATING THE SAME, AND OBTAINING COLOURING MATTERS THEREFROM
Year: 1884

page_text: I, JASPER WETTER, Engineer, of 67, Strand, in the City of Westminster, do hereby
declare the nature of said invention for A PROCESS OR PROCESSES FOR PRODUCING
BETANAPHTOL-DISULPHO-ACIDS, SEPARATING THE SAME, AND OBTAINING COLOURING
MATTERS THEREFROM, a communication to me from abroad by the Leipziger
Anilinfabrik, Beyer and Kegel, of Lindenau-Leipzig, in the kingdom of Saxony,
to be as follows:-
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This invention relates to the production of Betanaphtoldisulpho-acids by first
heating concentrated sulphuric acid above the melting point of the Betanaphtol,
then adding the latter and maintaining the temperature at 125-145° Centigrade
during 4 to 5 hours.
Also to the separation of the thus obtained Betanaphtoldisulpho-acids by treating
their acid or neutral soda salts in aqueous solution with common salt.
Also to the production of azo-colors by the combination of the thus separated
Betanaphtoldisulpho-acids with diazo-bodies.
The process may be carried out as follows: 4 parts of sulphuric acid of 66° Bé
are heated to 125-135° Centigrade, after which 1 part of Betanaphtol is quickly
introduced and the temperature maintained at 125-145° Centigrade during
4-5 hours.
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The product is dissolved in three times its own weight of water, calcined soda is
added, equal, in weight to half the quantity of sulphuric acid employed, after which
the solution is saturated with common salt. When the solution is cooling, a portioni
of the acid salts of the sulpho-acids crystallize, while another. portion remains ini
solution (those salts which give more yellow shades).
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Now the whole is filtered and washed with a concentrated solution of common.
salt until the filtered liquid is no. longer fluorescent.
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174 34 *
The residue and the filtered, liquid may now be directly employed for the pro-
duction of colors.
Instead of the acid salts, the neutral salts may be produced, by the complete-
saturation of the sulphuric acid with soda, and thereupon the separation effected

page_text: with common salt. Moreover, the acid soda salts may, of course, be produced by
the use of common salt itself or by sodic sulphate or caustic soda.
The residue, whether obtained from the acid salts, or from the neutral salts, is
still partly soluble in spirit, but the colouring matters derived from that part which
is soluble in spirit are not essentially different from those derived from the part
which is not soluble. In order to produce the colouring matters from the salts of
the Betanaphtoldisulpho-acids, thus obtained and separated, the quantity of the
salts in the residue, as well as that in the filtered liquid, is previously ascertained
by experiments, then the acid salts are converted into the neutral salts by complete
saturation with soda, the solution made alkaline with ammonia or milk of lime and
converted, in the usual way, into colouring matters, by combination with the
theoretical quantity of a diazo-compound.
In this way the following colours are produced:
a, from that portion of the salts which is not soluble in salt water,
By combination with:
Alphadiazonaphtalin
Diazocumol
bluish Bordeaux
bluish Ponceau
Diazoxylol
Diazotoluol
-Diazobenzol
Alphadiazonaphtalinsulpho-acid
Betadiazonaphtalinsulpho-acid
-
reddish Ponceau
yellowish Ponceau.
reddish Orange
Bordeaux
Ponceau
b, from the part which is soluble in salt water the following colours may be
obtained.
With Alphadiazonaphtalin
Diazocumol
Diazoxylol
Diazotoluol
Diazobenzol
Alphadiazonaphtalinsulpho-acid
Dated this 1st day of May 1884.
bluish Bordeaux
reddish Ponceau
yellowish Ponceau
reddish Orange
yellowish Orange
bluish Bordeaux.
I, JASPER WETTER, Engineer, of 67, Strand, in the City of Westminster, do
hereby declare the nature of said Invention for "A PROCESS OR PROCESSES FOR
PRODUCING BETANAPHTOL-DISULPHO-ACIDS, SEPARATING, THE SAME, AND OBTAINING
COLOURING MATTERS THEREFROM," a communication to me from abroad by The
Leipziger Anilinfabrik Beyer and Kegel, of Lindenau-Leipzig, in the Kingdom of
Saxony, and in what manner the same is to be performed, to be particularly
described and ascertained in and by the following statement:
By treating betanaphtol with concentrated sulphuric acid, there are always
formed mixtures of betanaphtolsulphoacids, each of which differs from the others,
according to the temperature at the beginning of the sulphonation, the quantity.
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page_text: and strength of the sulphuric acid employed, the duration of the process, and the
temperature maintained during the same.
Hitherto the following monosulpho-acids are known:
that of Schaeffer
and Bayer's Alphamonosulpho acid of betanaphtol.
Besides, H. E. Armstrong mentions a betanaphtolbetamonosulphoacid which he
considers identical with that found by Schaeffer, though he was not able to get the
lime salts in the form characteristic to the sulphoacid of Schaeffer.. Continued
experiments, however, have shown, that totally different products are formed by
working according to Schaeffer and by working according to Armstrong, but in no
case is a uniform naphtolsulphoacid obtained; there are always mixtures of different
sulphoacids, just as, for instance, in the production of Bayer's betanaphtol alpha-
monosulphoacid the latter acid is always obtained in mixture with another sulpho
acid supposed to be that of Schaeffer.
To divide the napholsulphoacids the different solubility of their salts in spirits
has hitherto been utilized; my correspondents have, however, succeeded in dividing
them by treating their acid or neutral soda salts in aqueous solution with common
salt, which treatment may be employed for the monosulpho-acids as well as for
the disulphoacids.
The differences between the several sulphoacids are best characterized by the
colours obtained from them by their combination with diazo-compounds.
It should be remarked, that the colours from the monosulpho acid become the
more yellowish, the smaller the quantity of sulphuric acid which was employed for
the production of the sulphoacids, and also that with the monosulphoacids, the part
of the salts precipitated with common salt gives more yellowish shades than that
part which is soluble in saltwater, but with the disulpho acids the reverse is the
case, namely the more blueish shades are obtained of that part of the salts which
is not soluble in saltwater, whilst the filtered liquid contains those sulphoacids
which give more yellowish colours..
Essentially more blueish shades are obtained, if in the production of the disulpho-
acids the temperature at the beginning of the sulphonation is raised above the
melting point of the betanaphtol, and by combination with diazo-compounds in
this way, more blueish shades are obtained, in general, than according to the
process described in German Patent N° 3229 of 19th April. 1884.
After this explanation, the actual processes of manufacture may be described as
follows:
4 parts of sulphuric acid of 66° Ré are heated to 125-135° Centigrade, after
which 1 part of betanaphtol is quickly introduced and the temperature maintained
at 125-145° C during 4-5 hours.
The product is dissolved in three times its own weight of water, calcined soda is
added, equal in weight to half the quantity of sulphuric acid employed, after which
the solution is saturated with common salt.
When the solution is cooling, a portion of the acid salts of the sulphoacids
crystallize, while another portion remains in solution (those salts which give more
yellow shades).
The whole is now filtered and washed with a concentrated solution of common
salt until the filtered liquid is no longer fluorescent.
The residue and the filtered liquid may now be directly employed for the
production of colours.
Instead of the acid salts, the neutral salts may be produced by the complete
saturation. of the sulphuric acid with soda, and thereupon the separation effected
with common salt.
Moreover, the acid soda salts may, of course be obtained by means of common
salt or sodic sulphate or caustic soda.
The residue, whether obtained from the acid salts or from the neutral salts, is
still partly soluble in spirits, but the colouring matters derived from that part

page_text: which is soluble in spirit are not essentially different from those derived from the
part which is not soluble. In order to produce the colouring matters from the salts
of the betanaphtol disulphoacids, thus obtained, and separated, the quantity of, the
salts in the residue, as well as that in the filtered liquid is previously ascertained
by an experiment, then. the acid salts are converted into the neutral salts by 5
complete saturation with soda, the solution made alkaline with ammonia or milk
of lime and converted in the usual way into colouring matters by combination with
the 'theoretical quantity of a diazo compound.
In this way, the following colours are produced:
a. from that portion of the salts which is not soluble in salt water
By combination with:
1°
alphadiazonaphtaline
'diazocumol
I.,
diazoxylol.
diazotoluol
diazobenzol
alphadiazonaphtalinesulpho acid
betadiazonaphtalinesulpho acid,
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blueish bordeaux
blueish scarlet
reddish scarlet
yellowish scarlet
reddish orange.
bordeaux 7 1
scarlet,
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b. from the part which is, soluble in saltwater, the following colours may be
obtained.
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With alphadiazonaphtaline
diazocumol
diazoxylol
diazotoluol
blueish bordeaux
reddish ponceau
yellowish ponceau
diazobenzol
alphadiazonaphtalinesulpho acid
reddish orange,
yellowish orange
blueish bordeaux.
Having now particularly described, and ascertained the nature of the said
invention, and in what manner the same is to be performed, I declare that what.
I claim is'
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1. Producing betanaphtoldisulpho acids, by first heating concentrated sulphuric 3
acid above the melting point of the betanaphtol, then adding the latter, and
maintaining the temperature at 125-145 Centigrade during 4 to 5 hours. 2
2. Separating the betanaphtoldisulphoacids thus obtained, by treating their acid
or neutral soda salts in aqueous solution with common salt...
3. Producing azocolours, by the combination of the thus separated betanapitol 3
disulpho acids with diazobodies.
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