The Manufacture or Production of Blue Dye-stuffs for Cotton.
Year: 1898

page_text: BAYER & Co, of Elberfeld, Germany.]
The Manufacture or Production of Blue Dye-stuffs for Cotton.
I, IIFNRY EDWARD NEWTON, of The Office for Patents, G, Biram'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 found some time since that blue dye-stuffs for cotton
are obtained from the products resulting from the melting of alpha, alpha,
amidonaphtholsulphonie acids with sulphur and alkaline sulphides, with sulphur
and alkalies, with alkaline polysulphides, on the like substances acting in the same
oi a similar manner, which process consists in tieating the said products with hot
water, until the more readily soluble component part thereof has been wholly
dissolved out, filtering the so-formed solutions, and subsequently isolating the
finished dye-stuffs from the joint filtiates by precipitation with salts, or in
another suitable manner.
My foreign correspondents have now found that coloning matters possessing the
same properties are produced in an analogous way, f, in place of the said
amidonaptholsulphonic acids, certain denvatives thereof, such as the corresponding
apha, alpha, chloro naphthol sulphonic acids, or the azo dye-stuffs obtainable from
the combination of diazo compounds with the above alpha, alpha, amidonaphthol-
sulphonic acids, are heated with sulphur and alkaline sulphide, or the like sub-
stances, and if the so-formed products are subjected to the treatment herembefore
specified
In order to illustrate this process, the following examples are given The
COLOURING MATTER FROM ALPHA CHLORO ALPHA NAPHTHOL. ALPHA BETA1
DISULPHONIC ACID
50 parts of alpha, alpha, chloio naphthol alpha, beta, disulphonic acid, are
stured with 15 litres (in case the pails are kilos by weight) of soda-lve, at
40 degrees Baumé After adding 81 parts of diy sodium sulphide and 75 parts
of flowers of sulphur, the mixture is slowly heated in an non vessel, with con-
tinuous stiring, to 200 degrees Centigrade, and kept at this temperature until
the mass is diy, and can be finely divided with readiness The vessel 16 then
closed, and the temperature is 1aised to 240 degrees Centigrade, at which tempera-
tuie the mass is kept until test portions of the melt dissolve in water with a

page_text: pure blue colour, and the intensity of this colour no longer increases. The greyish-
black mass thus obtained is allowed to cool, and subsequently subjected to a
repeated treatment with small quantities of hot water. The resulting solutions
are filtered, and this extraction is continued until the solution is colourless.
From the joint filtrates, the blue dye is precipitated by means of common salt, or,
more practically, by means of zinc chloride. It is finally filtered off, pressed, dried,
and pulverized, in the usual manner
The dye-stuff thus obtained has, in general, the same properties as that resulting,
in an analogous manner, fiom alpha, alpha, amido naphthol alpha, beta, disulphonic
acid When applied to cotton, either in boiling baths, with the addition of reduc-
ing agents (such as grape sugar and sodium carbonate, alkaline sulphide, or the
like), or in cold baths, containing alkaline sulphide, or the like reducing substances,
it yields at first brownish shades, which turn into indigo blue, fast to light and
alkalies, if the wet dved goods are exposed to the air, or if the dyed material is
rinsed It directly yields blue shades, when used in baths containing caustic
alkalies
It may be remarked that the less readily soluble component part which remains
on subjecting the above mentioned melted mass to a repeated treatment with hot
water, vields brown shades when it is used in baths containing alkaline sulphides.
The process is carried out in a manuet analogous to that described in the fore-
going example, if other alpha, alpha, chloronaphtholsulphonic acids are used, and
the products resulting from the melting thereof with sulphur and alkaline sulphide.
on the like alkaline-sulphide-carving compounds, are subjected to the treatment
helen before specified
COLOURING MATTER OBTAINED FROM THE AZO DYE-STUFF RESULTING FROM THE
COUPLING OF DIAZO BENZENE WITH ALPHA ALPHA AMIDO NAPHTHOL-ALPHA
BETA DISULPHONIC ACID
50 parts of the azo dyestuff resulting by combining equi-molecular proportions
of diazo benezene and alpha, alpha-amido naphthol-alpha, beta,-disulphonic acid,
in a sodium carbonate solution, are mixed with 100 litres (in case the parts are
kilos by weight) of hot water After the addition of 10 litres (in case the parts are
kilos by weight) of soda-lve, at 40 degrees Baumé, 80 parts of dry sodium sulphide
and 75 parts of flowers of sulphun are added The mixture is slowly heated in an
11on vessel, with continuous sting to 200 degrees Centigrade, until the mass
has become dry, and can be finely divided with leadiness. After the vessel has
been closed the temperature, is raised to from 240 to 250 degrees Centigrade.
Heating is continued at this temperature for, say, 4 hours. The resulting mass,
when cool, is repeatedly treated with small quantities of hot water; the so-formed
solutions are filtered, and this extraction is continued until the solutions are
colourless. From the joint filtiates, the blue dye is precipitated by the addition of
common salt, zinc chloride, or the like The precipitate thus obtained is filtered
off, pressed, dued, and pulverised
This colouring matter dyes cotton, in hot baths, to which grape sugar and sodium
carbonate, alkaline sulphide, or the like reducing agents are added, and in cold
baths, likewise in the presence of reducing substances, such as alkaline sulphide, at
first brown shades, which turn into a clear blue, fast to alkalies and light, if the dyed
wet material is exposed to the action of the air, or if it is rinsed It duectly yields
blue shades, when it is applied to cotton in baths contaming caustic alkalies
Other blue colouring matters are obtained if, in place of the aforesaid azo
dvestuff, other azo products resulting from the combination of diazo compounds
with alpha, alpha, amidonaphthol-mono- o poly-sulphonic acids are first heated
with sulphur and alkaline sulphide, or the like alkaline-sulphide-carrying com-
pounds, and if the so-formed products are subjected to the treatment hereinbefore
defined

page_text: My foreign correspondents wish it to be understood that they do not limit them-
selves to the particulars given in the above examples, which are merely typical.
Dated this 1st day of September 1898
NEWTON & SON,
Agents for the Applicant.
COMPLETE SPECIFICATION.
The Manufacture or Production of Blue Dye-stuffs for Cotton,
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 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 found some time since that blue dyestuffs for
cotton are obtained from the products resulting from the melting of alpha, alpha
amidonaphtholsulphonic acids with sulphur and alkaline sulphides, with sulphur
and alkalies, with alkaline poly sulphides, or the like substances, acting
111 the same or B similar manner, which process consists in treating
the said products with hot water, until the more readily soluble com-
ponent part thereof has been wholly dissolved out, filtering the so formed
solutions, and subsequently isolating the finished dye-stuffs from the joint filtrates
by precipitation with salts, or in any other suitable manner
My foreign corespondents have now found that colouring matters possessing the
same dyeing properties are produced in an analogous way, if, in place of the said
amidonaphthosulphonic acids, certain derivatives thereof, such as the corresponding
alpha, alpha, chloronaphtholsulphonic acids, or the azo dye-stuffs obtainable from
the combination of diazo compounds with the above alpha, alpha, amidonaphthol-
sulphonic acids, are heated with sulphur and alkaline sulphides, or the like
substances, and if the so formed products are subjected to the treatment herein-
before specified
In order to illustrate this process, the following examples are given The narta
COLOURING MATTER FROM ALPHA, CHLORO ALPHA NAPHTHOL ALPHA, BETA₁
DISULPHONIC ACID.
50 parts of alpha, alpha, chloro naphthol alpha, beta, disulphonic acid are
stired with 15 litres, (if the parts are kilos by weight) of soda-lye, at 40 degrees
Baumé After adding 81 parts of dry sodium sulphide and 75 parts of flowers of
sulphur, the mixture is slowly heated in an non vessel with continuous stirring
to 200 degrees Centigrade, and kept at this temperature until the mass is dry and
can readily be finely divided. The vessel is then closed, and the temperature 18
raised to 240 degrees Centigrade, at which temperature the mass is kept for from
about 4 to 5 hours, until test portions of the melt dissolve in water with a pure
blue colour, and the intensity of this colour no longer increases
The greyish-
black mass thus obtained is allowed to cool, and subsequently subjected to a
repeated treatment with small quantities of hot water The resulting solutions are
filtered, and this extraction is continued until the solution is colourless From
the joint filtrates the blue dye is precipitated by means of common salt, or, more
practically, by means of zinc chloride It is finally filtered off, pressed, dried, and
pulverised in the usual manner.
The dye-stuff thus obtained has, in general, the same properties as that result-

page_text: ing, in an analogous manner, from alpha alpha̸ amidonaphthol alpha beta,
disulphonic acid. When applied to cotton, either in boiling baths with the addition
of reducing agents (such as grape sugar and sodium carbonate, alkaline sulphide or
the like), or in cold baths containing alkaline sulphide or the like reducing sub-
stances, it yields, at first, -brownish shades, which fuin into indigo-blue shades fast
to alkalies, and withstanding, to a considerable extent, the action of light when
the wet dyed goods are exposed to the an, or when the dyed material is rinsed.
It directly yields blue shades when used in baths containing caustic alkalics.
It may be remarked that the less readily soluble component part which remains
on subjecting the above mentioned melted mass to a repeated treatment with hot
water, yields brown shades when it is used in baths containing alkaline sulphides.
The process is carried out in a manner analogous to that described in the fore-
going example, if other alpha, alpha, chloronaphtholsulphonic acids are used, and
the products resulting from the melting thereof with sulphur and alkaline sulphide,
or the like alkaline-sulphide-carrying compounds, are subjected to the treatment
hereinbefore specified.
COLOURING MATTER OBTAINED FROM THE AZO DYE STUFF RESULTING FROM THE
COUPLING OF DIAZOBENZENE WITH ALPHA ALPHA, AMIDONAPHTHOL-ALPHA-
BEFA, DISULPHONIC ACID
50 parts of the azo dye-stuff resulting from combining equimolecular proportions
of diazobenzene and alpha, alpha, amido naphthol alpha, beta, disulphonic acid,
in a sodium carbonate solution, are mixed with 100 litres (if the parts are kilos
by weight) of hot water After the addition of 10 lities (if the parts are kilos by
weight) of soda Ive at 40 degrees Baumé, 80 parts of dry sodium sulphide and
75 parts of flowers of sulphur are added 'The mixture is slowly heated in an iron
vessel, with continuous stirring, to 200 degrees Centigrade, until the mass has
become dry and can readily be finely divided After the vessel has been closed,
the temperature is raised to from 240 to 250 degrees Centigrade Heating 18 con-
tinued at this temperature for, say, 4 hours The resulting mass, when cool, is
repeatedly treated with small quantities of hot water. the so-formed solutions are
filtered, and this extraction is continued until the solutions are colorless From the
joint filtrates, the blue dye is precipitated by the addition of common salt, zinc
chloride, or the like The precipitate thus obtained is filtered off, pressed, dried,
and pulverised
This colouring matter dyes cotton in hot baths, to which grape sugar, and
sodium carbonate, alkaline sulphide, or the like reducing agents, are added, and
in cold baths, likewise in the presence of reducing substances, such as alkaline
sulphide, at first brown shades, which turn into a blue, fast to alkalies and also to
light, when the dyed wet material is exposed to the action of the air, or when it is
rinsed It directly yields blue shades when it is applied to cotton in baths
containing caustic alkalies
Other blue colouring matters are obtained if, in place of the aforesaid azo
dye-stuff other azo products resulting from the combination of diazo compounds
with alpha, alpha, amidonaphthol mono- or polysulphonic acids, are first heated
with sulphur and alkaline sulphide, or the like alkaline sulphide-carrying com-
pounds, and if the so-formed products are subjected to the treatment hereinbefore
defined
My foreign corespondents wish it to be understood that they do not limit
themselves to the particulars given in the above examples, which are merely typical
Having now particularly described and ascertained the nature of the said
invention and in what manner the same is to be performed (as communicated
to me from abroad), I declare that what I claim is
1 The production of blue dye-stuffs for cotton from alpha, alpha, chloro-

page_text: naphtholsulphonic acids, or the azo colouring matters obtainable by combining
diazo compounds with alpha, alpha, amidonaphtholaulphonic acids, which process
consists in heating the said chloro acids or azo dye-stuffs with sulphur and alkaline
sulphide, or the Like alkaline-sulphide-carrying compounds at elevated tempera-
tures, extracting from the so-formed melts the more readily soluble component part
thereof, with the aid of hot water, filtering the resulting solutions, and finally
isolating from the joint filtrates the blue colouring matters in any suitable
manner
2 As articles of manufacture, the new blue dyestuffs for cotton obtainable by
means of the process claimed in the foregoing Claim One