IMPROVEMENTS IN THE MANUFACTURE OF COLOURING MATTERS SUITABLE FOR DYEING AND PRINTING "
Year: 1883

page_text: LETTERS PATENT to Ivan Levinstein of the City of Manchester in the
County of Lancaster, Chemist for an Invention of "IMPROVEMENTS IN THE
MANUFACTURE OF COLOURING MATTERS SUITABLE FOR DYEING AND PRINTING "
PROVISIONAL SPECIFICATION left by the said Ivan Levinstein at the
Office of the Commissioners of Patents on the 9th February 1883.
IVAN LEVINSTEIN, of the City of Manchester, in the County of Lancaster,
Chemist, "IMPROVEMENTS IN THE MANUFACTURE OF COLOURING MATTERS
SUITABLE FOR DYEING AND PRINTING,"
My invention relates to, and consists in, a new method or methods of producing
sulpho acids of beta Naphtol and of obtaining Red colouring matters by combining
these sulpho acids or their salts with certain diazo compounds.
To carry out my invention I proceed as follows:
I dissolve 10 lbs of dry and finely powdered beta Naphtol in 30 lbs of sulphuric
acid, of a strength 170 Twaddell, taking care that the temperature does not rise
above 30° C-I then keep this solution under constant stirring from 10 to 12
hours at 30° to 35° C, or until a sample of it dissolves in diluted carbonate of soda,
or nearly so.
In order to avoid the dilution of the sulphuric acid, by the absorption of
moisture from the atmosphere, I cover the mixture with a layer of Paraffin, or
with any other substance not acted upon by sulphuric acid, or, in order to facilitate
the solution and conversion of the Naphtol into a sulpho acid, I dissolve the
Naphtol previously in a solvent indifferent to sulphuric acid.
The formed sulpho acid of beta Naphtol thus obtained is not of one uniform
composition but consists of a mixture of several modifications of sulpho acids,
which modifications I separate from each other in the following manner.
I dilute the whole with about 20 gallons of water, add lime sufficient to
neutralize the sulphuric acid and to convert the sulpho acids of Naphtol into
their lime salts, I then heat it to boiling-filter and concentrate the clear filtered
liquor until a small sample of it does not show a perceptible precipitate on further
concentration.

page_text: I then allow the whole to cool and separate the precipitate, which consists chiefly
of the more difficultly soluble lime salt of the mono-sulpho acid of beta Naphtol, by
filtration or otherwise from the solution.
The solution which is the easier soluble lime salt of the mono-sulpho-acid of
beta Naphtol I convert into its sodium salt, and combine the same, in a manner
well known with certain diazo compounds.
Bright Reds for instance are obtained by combining this sulpho acid with the
diazo compound of Amidoazobenzole or of the sulpho acids of Amidoazobenzole or
by combining the same with the diazo compounds of the difficultly soluble mono-
sulpho acids of Alpha Naphthylamine.
The precipitate or the more difficultly soluble lime salt does also give reds with
the corresponding diazo compounds, but these Reds are of a much bluer shade and
are dull and of little commercial value. In order to produce from this precipitate
a valuable sulpho acid which will produce by combination with certain diazo
compounds very bright and blueshade Reds,-I dry the precipitate and dissolve-
10 parts by weight of it in 20 parts of sulphuric acid, 170 Twaddell, and heat the
solution for 2 hours at 110 Centigrade, I then add 20 parts more sulphuric acid,
170 Twaddell, and heat the mixture for 4 hours at 130. C.
I allow to cool to about 110-C, when Ladd another 20 parts of sulphurie-acid,
and I then heat this mixture to 150 C, and keep it at this temperature from about
2 to 3 hours or until a sample of-it-when combined for instance, with diazo sulpho
naphthaline will produce red colouring matter, but practically no Red colouring-
matter when combined with diazo xylol, taking care that the heating is not
continued longer than necessary.
==
=
I then convert this new sulpho acid into its sodium salt in a manner well known
by chemists.
In order to make new Red colouring matters from this sulpho acid by combining
the same with certain diazo compounds I proceed for example as follows.
I dissolve 10 lbs of the dry sodium salt in about 5 gallons of water and add to it
Ammonia, taking care that the solution contains a slight excess of ammonia until
the color is finished, I then add to it diazo mono-sulpho-naphthaline prepared
in a well known manner from about 4 lbs of the difficultly soluble mono-sulpho
acid of Alpha naphthylamine as soon as the whole of the diazo compound is
added I add salt to it when the colour will be precipitated as a green powder
which I filter off and dry when it is ready for use. This powder dyes a very
bright Red of a blueish hue.
Instead of combining this new sulpho acid with the diazo compounds of the
difficultly soluble mono-sulpho acids of of Alpha Naphthylamine bright red colouring
matters may be also obtained by combining the same with the diazo compounds of
the sulpho acids of beta naphthylamine with the diazo compounds of Amidoazo-
benzole or with the diazo compounds of the sulpho acids of Amidoazobenzole.
This new sulpho acid of beta Naphtol produces further a bright red similar to
Archil when combined (in a manner well understood by chemists) with the diazo
compound of Alpha Naphthylamine.
If I desire to obtain larger quantities of the precipitated lime salt of the
mono-sulpho acid of beta Naphtol in the process above described, I heat the
mixture of three parts of sulphuric acid and beta Naphtol at a higher temperature
than 30° to 35° C, viz-by preference between 60° to 80° C, when much more of
the difficultly soluble lime salt is formed.
I do not confine myself to the exact time at which the sulphuric acid is acting
on the difficultly soluble lime salt of the beta Naphtol, or to the exact proportions
of the sulphuric acid used, or to its concentration, as fuming sulphuric acid may be
also employed or the monochlorhydrine instead of it, but use by preference ordinary
sulphuric acid 170° Twaddell, substantially as specified,

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed
by the said Ivan Levinstein in the Great Seal Patent Office on the 28th June
1883.
IVAN LEVINSTEIN, of the City of Manchester, in the County of Lancaster,
Chemist, IMPROVEMENTS IN THE MANUFACTURE OF
"
SUITABLE FOR DYEING AND PRINTING.
COLOURING MATTERS
My invention relates to, and consists in a new method or methods of producing
sulpho acids of beta Naphtol, and of obtaining Red colouring matters by combining
these sulpho acids or their salts, with certain diazo compounds.
To carry out my invention I proceed as follows.
I dissolve 10 lbs of dry and finely powdered beta Naphtol in 30 lbs of sulphuric
acid of a strength 170 degrees Twaddells hydrometer taking care that the
temperature does not rise above 30° centigrade-I then keep this solution con-
stantially stirred from 10 to 12 hours at a temperature of 30° to 35° centigrade or
until a sample of it (a) dissolves in diluted carbonate of soda or nearly so.
order to avoid the dilution of the sulphuric acid, by the absorption of moisture
from the atmosphere, I cover the mixture with a layer of Paraffin, or with any
other substance not acted upon by sulphuric acid.
In
Instead of using the Naphtol as a fine powder as above described, and in order
to facilitate the solution and conversion of it into a sulpho acid, the Naphtol is or
may be dissolved in a solvent indifferent to sulphuric acid, preferably a coal tar
Naphtha (6) from which the aromatic hydro carbons have been previously separated
and which boils at 135° to 150° centigrade such a Naphtha for example as that
which is obtained, as a by-product in the manufacture of xylidine.
The sulpho acid of beta Naputol obtained by the above methods (a or b) is not
of one uniform composition but consists of a mixture of several modifications of
sulpho acids, which modifications may be separated from each other in the
following manner namely.
I dilute the whole mixture (a or a and b) with about 20 gallons of water and
add lime sufficient to neutralize the excess of sulphuric acid and convert the sulpho
acids of Naphtol into their lime salts. I then heat this mixture to boiling then
filter it and concentrate the clear filtered liquor until a small sample of it does not
show a perceptible precipitate on further concentration.
I then allow the whole concentrated liquor to cool and the precipitate (c) which
consists chiefly of the more difficultly soluble lime salt of the mono-sulpho acid of
beta Naphtol; I separate from the solution by filtration or otherwise.
The solution (d) which is the easier soluble lime salt of the mono sulpho-acid of
beta Naphtol I convert into its sodium salt in a manner well understood and
combine the same in a manner well known by Chemists with certain diazo
compounds such for example as those hereinafter mentioned.
Bright Reds for instance are obtained by combining this easily soluble sulpho
acid (d) with the diazo compounds of Amidoazobenzene or of the sulpho acids of
Amidoazobenzene or by combining the same (d) with the diazo compounds of the
difficultly soluble mono sulpho-acids of Alpha Naphthylamine (e).
The precipitate (c) or the more difficultly soluble lime salt does also give reds
with the corresponding diazo compounds but these Reds are of a much bluer shade,
and are dull and of little commercial value. In order to obtain from this said
precipitate (c) a valuable sulpho acid which will produce very bright and blue
shade reds by combination with diazo compounds such for example as the diazo
compound of Amidoazobenzene sulpho acids of Amidoazobenzene, diazo Naphtha-
ene, sulpho acids of diazo Naphthalene etc-I dry the said precipitate (c) and

page_text: dissolve 10 parts by weight of it in 20 parts by weight of sulphuric acid
170 degrees Twaddell, and heat the solution for 2 hours at 110 centigrade. I then
add 20 parts by weight more of sulphuric acid at 170 degrees Twaddell, and heat
the mixture for 4 hours at 130 centigrade.
I allow the mixture to cool to about 110 centigrade when I add another 20 parts
by weight of sulphuric acid and I then heat this mixture to 150 centigrade and
keep it at this temperature from about 2 to 3 hours or until a sample of it (f)
when combined for instance, with diazo sulpho naphthalene will produce red
colouring matter but practically no Red colouring matter when combined with
diazo xylol. taking care that the heating is not continued longer than necessary.
I then convert this new sulpho acid (f) into its sodium salt (g) in a manner well
known by Chemists.
In order to make new Red colouring matters from this sulpho acid (f) by
combining the same with certain diazo compounds I proceed for example as
follows.
I dissolve 10 lbs of the sodium salt (g) in about 5 gallons of water, and add to it
Ammonia taking care that the solution (h) contains a slight excess of Ammonia
until the color is finished.
I then add to the solution (6) diazo mono sulpho-Naphthalene prepared from
about 44 lts of the difficultly soluble mono-sulpho-acid of Alpha Naphthylamine (6)–
as soon as the whole of the diazo-compound is combined--I add common salt to it,
when the colour will be precipitated as a green powder (t) which I filter off and dry
when it is ready for use. This powder (i) dyes a very bright Red of a blueish hue.
Instead of combining this new sulphe acid (f) with the diazo compounds of the
difficultly soluble mono-sulpho-acids of alpha Naphthylamine (6) bright red colouring
matters may be also obtained by combining the same (f) with the diazo compounds
of the sulpho acids of beta naphthylamine with the diazo compounds of Amidoazo-
benzene or with the diazo compounds of the sulpho acids of Amidoazobenzene.
This new sulpho acid of beta Naphtol (f) produces further a bright red similar to
Archil when combined (in a manner well understood by Chemists) with the diazo
compound of alpha Naphthylamine.
If I desire to obtain larger quantities of the precipitated lime salt of the mono
sulpho-acid of beta Naphtol (c) in the process above described, I heat the said
mixture of three parts of sulphuric acid by weight and one part by weight of beta
Naphtol at a higher temperature than 30° to 35° centigrade, viz, by preference
between 60° to 80° centigrade when much more of the difficultly soluble lime
salt (c) is formed.
I do not confine myself to the exact time during which the sulphuric acid is to
act on the difficultly soluble lime salt of beta Naphtol (c) or to the exact proportions
of the sulphuric acid used, or to its concentration, as fuming sulphuric acid may be
also employed, or the monochlorhydrine instead of it, but I use by preference
ordinary sulphuric acid 170° Twaddell substantially as specified.
I have now particularly described the nature of my said invention and the modes
of carrying the same into effect and claim as my invention
Firstly. The method or methods or process or processes of producing and
separating mono sulpho-acid of Beta Naphtol, substantially as herein before
described.
Secondly. The method or process of producing the sulpho acid of Beta Naphtol
distinguished from other sulpho acids of Beta Naphtol, by not forming Red
colouring matters when combined with diazo xylol, substantially as herein before
described.
Thirdly. Red colouring matters produced by combining diazo compounds such as
those herein before referred to with the sulpho acid of Beta Naphtol which is
distinguished from other sulpho acid of Beta Naphtol by not forming Red colouring
matters when combined with diazo xylol, obtained from the difficultly soluble lime
salt of the mono sulpho acid of Beta Naphtol, substantially as hereinbefore
described.

page_text: Fourthly. The method or process of producing red colouring matters by com-
bining diazo compounds such as hereinbefore referred to with the sulpho acid of
Beta Naphtol which is distinguished from other sulpho acids of Beta Naphtol by
not forming red colouring matters when combined with diazo xylol obtained
from the difficultly soluble lime salt of the mono sulpho acid of Beta Naphtol
substantially as herein before described.
Fifthly. Red colouring matters produced by combining diazo compounds such as
those herein before referred to with easily soluble mono-sulpho acids of Beta
Naphtol, substantially as hereinbefore described.
Sixthly. The method or process of producing red colouring matters by combining
diazo compounds such as those hereinbefore referred to with easily soluble mono
sulpho acid of Beta Naphtol, substantially as hereinbefore described.
In Witness whereof I the said Ivan Levinstein have hereunto set my hand
and seal this twenty seventh day of June in the year of our Lord one
thousand eight hundred and eighty three.
IVAN LEVINSTEIN (L.S.)