A Process or Processes for Separating the Different Betanaphtol- monosulpho-acids from a Mixture of the same, and for Obtaining Colouring Matters therefrom.
Year: 1884

page_text: A Process or Processes for Separating the Different Betanaphtol-
monosulpho-acids from a Mixture of the same, and for
Obtaining Colouring Matters therefrom.
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 SEPARATING
THE DIFFERENT BETANAPHTOLMONOSULPHO-ACIDS FROM A MIXTURE OF THE SAME
AND FOR 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:-
This invention is based on the discovery, that the substance known as: Armstrongs
Betanaphtolmonosulpho-acid is in reality a mixture of two isomeric Betanaphtol-
monosulpho-acids, which may be easily separated.
The invention consists substantially in dividing Armstrong's Betanaphtolmono-
sulpho-acid into two different Betanaphtolmonosulpho-acids by treating its acid or
neutral soda salts with common salt, and in producing coloring matters by the
action of the thus separated monosulpho-acids of Betanaphtol upon certain Diazo-
compounds in alkaline solution and in the well known way.
By treating Betanaphtol at 100° C with the quantity of concentrated sulphuric
acid theoretically necessary to form the monosulpho-acid, there results according to
Armstrong a naphtolsulpho-acid.
This sulpho-acid may be very easily divided into two parts by treating its acid
or neutral soda salts with common salt; and the resulting two parts give coloring
matters of different shades.
I prefer to divide the acid soda salts.
For this purpose the raw naphtolsulpho-acid is dissolved in boiling water, half
of the employed sulphuric acid neutralized with soda, and the solution completely
saturated with common salt.
After cooling, the product is filtered and the residue washed with saltwater
until the liquid passing through the filter has only a slight acid reaction.
The residue and the filtered liquid may now be directly employed for the
production of coloring matters.

page_text: .
By a previous experiment the quantity of naphtolmonosulphonate of soda
contained in the residue as well as in the filtered liquid is ascertained, whereupon
the neutral salts are formed by the addition of more soda; the solution is made
alkaline by ammonia or milk of lime (the alkaline reaction must be maintained
until the end of the operation) and a diazocompound is added equivalent in
quantity to the salts found by the previous experiment, whilst the solution is well
cooled.
The coloring matter is at once precipitated and is not easily soluble in water.
Example: 246 Kilogrammes of the acid soda salt of the naphtol monosulpho-acid
(divided in the above way) are dissolved in 1500 litres of water; 5.5 Kilogrammes
of calcined soda and 10 Kilogrammes of ammonia are added, and thereupon, a
solution of 14 Kilogrammes of Diazobenzolchloride. The colouring matter is at
once precipitated in the form of an orange colored powder.
The following colours are in this way obtained-:-
af from that part of the salts which is not soluble in saltwater, by combination
with:
· .Diazobenzol
Diazotoluol
.Diazoxylol
Diazocumol
Alpha-Diazonaphtalin
Alphia-Diazonaphtalinsulpho-acid
Diazoazobenzol
yellowish orange
yellowish orange
reddish orange;
yellowish-ponceau ;
yellowish bordeaux';
blueish bordeaux;
red.
6. The part soluble in saltwater gives the following colours;
with Diabenzol
Diazotoluol
Diazoxylol
Diazocumol
Alpha Diazonaphtalin
Alpha Diazonaphtalinsulpho-acid
Diazoazobenzol
yellowish orange;
reddish orange;
reddish orange;
yellowish ponceau ;
reddish bordeaux ;
reddish bordeaux';
red.

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
SEPARATING THE DIFFERENT BETANAPHTOL-MONOSULPHO-ACIDS FROM A MIXTURE
OF THE SAME, AND FOR OBTAINING COLOURING MATTERS THEREFROM," a communi-
cation 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 at 100° centigrade with the quantity of concentrated
sulphuric acid theoretically necessary to form the monosulphoacid, there results
according to Armstrong, a naphtolsulphoacid.
:
This sulphoacid is not, however, a homogeneous product, but may be very easily
divided into two parts by treating its acid or neutral-soda salts with common salt;
and the resulting two parts give colouring matters of different shades.
I prefer to divide the acid soda salts.
3
For this purpose the raw naphtolsulphoacid is dissolved in boiling water, half of
the employed sulphuric acid neutralized with soda, and the solution completely
saturated with common salt.
After cooling, the product is filtered and the residue washed with saltwater,
until the liquid passing through the filter has only a slight acid reaction.
The residue and the filtered liquid may now be directly employed for the
production of colouring matters.
By a previous experiment the quantity of naphtolmonosulphonate of soda
contained in the residue, as well as in the filtered liquid, is ascertained; where-
upon the neutral salts are formed by the addition of more soda; the solution is
made alkaline by ammonia or milk of lime (the alkaline reaction must be
maintained until the end of the operation) and a diazocompound is added
equivalent in quantity to the salts found by the previous experiment, whilst the
solution is well cooled.
"
The colouring matter is at once precipitated and is not easily soluble in water.
Example:
24-6 Kilograms of acid soda salt of the naphtolmonosulpho-acid (divided in the
above way) are dissolved in 1500 litres of water; 5.5 Kilograms of calcined soda
and 10 Kilograms of ammonia are added, and thereupon-while the mixture is
allowed to cool-a solution of 14 Kilograms of diazobenzolchloride.
The colouring matter is at once precipitated in the form of an orange coloured
powder.
The following colours are in this way obtained:
a, from that part of the salts which is not soluble in saltwater, by combination
with:
diazobenzol
diazotoluol
diazoxylol
diazocumol
yellowish orange
yellowish orange
reddish orange
yellowish scarlet
yellowish bordeaux
blueish bordeaux
alpha-diazonaphtaline
alpha-diazonaphtalinesulph oacid
diazoazobenzol
red.

page_text: . b. The part soluble in saltwater gives the following colours:
with diazobenzol
diazotoluol
diazoxylol
diazocumol
alphadiazonaphtaline
alpha-diazonaphtalinesulpho'acid
diazoazobenzol
yellowish orange
reddish orange
reddish orange
yellowish scarlet
reddish bordeaux
⚫ reddish bordeaux
red.
It may be remarked, that the colours obtained from that portion of the salts
which is soluble in salt water are generally redder than those derived from the
insoluble portion.
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
1. Dividing Armstrong's betanaphtolmonosulphoacid into two different beta-
naphtolmonosulpho acids by treating its acid or neutral soda salts with common
salt.
2. Producing colouring matters by the action of the thus separated monosulpho-
acids of betanaphtol upon alkaline solutions of the diazo.compounds hereinbefore
specified.