Improvements in Treating Alizarine Blue for the Obtainment of New Compounds thereof and Alizarine Blue S.
Year: 1890

page_text: Date of Application, 28th May, 1890
Complete Specification Left, 15th Jan., 1891-Accepted, 21st Feb., 1891
PROVISIONAL SPECIFICATION.
Improvements in Treating Alizarine Blue for the Obtainment of
New Compounds thereof and Alizarine Blue S.
I, JAMES YATE JOHNSON, of 47, Lincoln's Inn Fields, in the County of
Middlesex, Gentleman, do hereby declare the nature of this invention (which has
been communicated to me from abroad by The Badische Anilin and Soda Fabrik of
Ludwigshafen on Rhine, in the Empire of Germany) to be as follows:-
As is well known, alizarine blue can be converted into a .compound soluble in
water and named alizarine blue S by causing it to combine with the elements of the
alkaline sulphites.
The conversion of alizarine blue into alizarine blue S is the subject of Letters
Patent No. 3603 A.D. 1881 granted to John Henry Johnson.
In the processes already known for effecting this conversion the combination has
been brought about in the following ways, namely
(1) By treating alizarine blue in its ordinary commercial form or in the form of
an alkaline salt with a strong solution of an alkaline bisulphite or of neutral
ammonium sulphite.
=
(2) By treating an alkaline salt of alizarine blue or alizarine bluc in suspension
in an aqueous solution of an alkali with excess of sulphurous acid gas.
According to the present invention the conversion is effected by
(1) Substituting the sulphite of a suitable organic base for the alkaline bisulphites
used in the process described in the Specification of the aforesaid Letters Patent
No. 3603 of 1881 and treating the new compound thus obtained with a solution of
an alkaline salt preferably sodium acetate. According to the nature of the organic
base used and the conditions of manufacture the alizarine blue S formed may
be mixed with a varying quantity of double compounds as hereinafter described,
but these do not interfere with the application of the product to dyeing and
printing.
(2) Treating commercial alizarine blue suspended in water with sulphurous acid
gas, and so obtaining a new, compound alizarine blue sulphite which by treatment
with sodium acetate or other suitable alkaline compound gives alizarine blue S.
The following examples illustrate the way in which the processes may be carried
into effect the parts being by weight.
EXAMPLE 1. FIRST PROCESS.
(1) All common organic bases that yield sulphites readily soluble in water can be
used in carrying out the first process, such as for instance-aniline, its homologues
riding chinaline and the like. The use of
allatitution wamnaunds

page_text: acetate to practically completely precipitate colouring matter, from solution. Filter,
wash, press and dry at a low temperature or preserve for use in the form of paste.
The product thus obtained is alizarine blue S which may contain some double
sulphite of aniline which escapes double decomposition. The proportion of double
sulphite present varies according to the conditions of the manufacture.
The aniline salt in the mother liquor can be recovered in the usual way.
The new compound alizarine blue aniline sulphite obtained in the above process
as an intermediate product is characterized by the following properties:-It is not
readily soluble in cold water but is easily soluble in hot water and on heating with
excess of a caustic alkali it splits up with separation of aniline.
EXAMPLE 2. SECOND PROCESS.
Pass sulphurous anhydride into alizarine blue paste containing from 10 to 20 per
cent. of dry substance until it is saturated. The new alizarine blue sulphite is
thus formed. To convert this into alizarine blue S add a solution of sodium acetate
or other alkaline compound which yields a sulphite with sulphurous acid, filter if
necessary salt out the dyestuff formed, filter, wash, press and dry at a low
temperature or preserve for use in the form of paste.
The new compound alizarine blue sulphite obtained as an intermediate product in
the above process can be isolated by filtering pressing and drying at a low
temperature.
It is a reddish brown powder insoluble in cold water, on heating alone or in
water or with strong acids, it decomposes forming alizarine-blue and sulphurous
anhydride.
DL 11000
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, London, W.C., Agents.
COMPLETE SPECIFICATION.
Improvements in Treating Alizarine Blue for the Obtainment of
New Compounds thereof and Alizarine Blue S.
JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of Middlesex
Gentleman do hereby declare the nature of this invention which has been com-
municated to me from abroad by The Badische Anilin & Soda Fabrik of Ludwigshafen
on the Rhine in the Empire of Germany and in what manner the same is to be
performed to be particularly described and ascertained in and by the following
statement :-
As is well known alizarine blue can be converted into a compound soluble in
water and named alizarine blue S by causing it to combine with the elements of the
alkaline sulphites.
The conversion of alizarine blue into alizarine blue S is the subject of Letters
Patent No. 3603 A..D. 1881 granted to John Henry Johnson.
In the processes already known for effecting this conversion the combination has
been brought about in the following ways, namely
:-
1. By treating alizarine blue in its ordinary commercial form or in the form of
an alkaline salt with a strong solution of an alkaline bisulphite or of neutral
ammonium sulphite.
2. By treating an alkaline salt of alizarine blue or alizarine bluc in suspension in
an aqueous solution of an alkali with excess of sulphurous acid gas.
According to the present invention the conversion is effected by,
1. Substituting the sulphite of a suitable organic base for the alkaline bisulphites
used in the process described in the Specification of the aforesaid Letters Patent
No. 3603 of 1881 and treating the new compound thus obtained with a solution of
an alkaline salt preferably sodium acetate. According to the nature of the organic
base used and the conditions of manufacture, the alizarine blue S formed, may be

page_text: found to be mixed with a varying quantity of double compounds as hereinafter
described, but these do not interfere with the application of the product to dyeing
and printing.
2. Treating commercial alizarine blue suspended in water with sulphurous acid
gas and so obtaining a new compound, alizarine blue sulphite, which by treatment
with sodium acetate or other suitable alkaline compound gives alizarine blue S.
The following examples illustrate the way in which the processes may be carried
into effect according to the present invention the parts being by weight.
1. All common organic bases that yield sulphites, readily soluble in water, can
be used in carrying out the first process, such as for instance-aniline, its homo-
logues and alkyl substitution compounds, pyridine, chinoline, and the like. The
use of aniline is recommended as being economical.
Make a solution of sulphite of aniline of about 1.16 specific gravity by mixing
aniline with the requisite quantity of water and saturating with sulphurous acid.
Mix about one hundred parts of this solution with about one hundred parts of
Allow
alizarine blue paste containing about twenty per cent. of dry alizarine blue.
the mixture to stand at ordinary or slightly elevated temperature until the blue
colour of the paste is completely changed into a brownish red: At ordinary tem-
peratures this operation will be completed in a few days; at a higher temperature
say 40° Centigrade a shorter time is sufficient.
Filter off the new product (alizarine-blue-aniline-sulphite) which is formed and
press (and dry if it be desired to have the new product isolated). Dissolve in water
and slowly add to the solution sufficient common salt or preferably sodium acetate
to practically completely precipitate colouring matter from solution. Filter, wash,
press and dry at a low temperature or preserve for use in the form of paste. The
product thus obtained is alizarine blue S which may contain some double sulphite
of aniline which escapes double decomposition. The proportion of double sulphite
present varies according to the conditions of the manufacture.
The aniline salt in the mother liquor can be recovered in the usual way.
The new compound alizarine-blue-aniline-sulphite obtained in the above process
as an intermediate product is characterized by the following properties:
It is not readily soluble in cold water but it is easily soluble in hot water and on
heating with excess of a caustic alkali it splits up with separation of aniline.
EXAMPLE 2. SECOND PROCESS.
Pass sulphurous anhydride into alizarine blue paste containing from 10 to
20 per cent. of dry substance until it is saturated.
The new alizarine blue sulphite is thus formed. To convert this into alizarine
blue S, add a solution of sodium acetate or other alkaline compound which yields a
sulphite with sulphurous acid, filter if necessary, salt out the dyestuff' formed, filter,
wash, press and dry at a low temperature or preserve for use in the form
of paste.
The new compound (alizarine blue sulphite) obtained as an intermediate product
in the above process can be isolated by filtering, pressing and drying at a low
temperature.
It is a reddish-brown powder insoluble in cold water, on heating alone or in
water or with strong acids, it decomposes forming alizarine blue and sulphurous
anhydride.
I am
as hereinbefore indicated aware of the invention claimed in Johnson's
Letters Patent 3603" and the first and second of the following claiming clauses are
to be read as being subject to this Patent.

page_text: of this
Having now particularly described and ascertained the nature
invention and in what manner the same is to be performed, I declare that
what I claim is-
1. The process for converting alizarine blue into alizarine blue S (which may
contain varying quantities of other bodies) consisting in treating alizarine blue with
the sulphite of a suitable organic base and then decomposing the resulting sulphite
of alizarine blue and the base with an alkaline salt preferably sodium acetate, all
substantially as hereinbefore described.
2. The process for converting alizarine blue into alizarine blue S consisting in
treating alizarine blue with sulphurous acid and then acting on the resulting
alizarine blue sulphite with a solution of an alkaline compound (preferably sodium
acetate) which yields a sulphite with sulphurous acid all substantially as herein-
before described.
3. As a new product the sulphite of alizarine blue and aniline hereinbefore
described and characterized.
4. As a new product the sulphite of alizarine blue hereinbefore described and
characterized.
Dated this 15th day of January 1891
J. H. JOHNSON & Co.,
Agents.