Improvements in the Manufacture of Colouring Matters.
Year: 1890

page_text: Date of Application, 26th Feb., 1840
Complete Specification Left, 14th Mar., 1890-Accepted, 19th Apr., 1890
PROVISIONAL SPECIFICATION.
[Communicated from abroad by RUPERT GREVILLE WILLIAMS, of Albany, in the
County of Albany, State of New York, U.S.A., Manufacturing Chemist.]
Improvements in the Manufacture of Colouring Matters.
I, HENRY HARINGTON LEIGH, Fel. Inst. P.A., Assoc. M. Inst. C.E., practising
as Phillips & Leigh, at No. 22 Southampton Buildings, Chancery Lane, in the
County of Middlesex, Engineer and Patent Agent, do hereby declare the nature of
this invention to be as follows:-
In my Specification No. 12767, 1889, I have described a process for the produc-
tion of cotton colors by combining naphthalene-azo-naphthylamines and their sulpho
acids with tetrazo bodies to form compound intermediates, and then reacting on
these bodies with amines or phenols.
I have now ascertained that valuable cotton colors can be as well made by
combining one molecule of diazo benzene, or its homologues, or its sulpho acids, with
one molecule of alpha or beta naphthyalamine, or its sulpho acids, to produce a
body that can be substituted for the naphthalene-azo-naphthyalamines or their sulpho
acids which I previously employed.
I have also ascertained that the product formed by combining one molecule of
diazo naphthalene or its sulpho acids with one molecule of aniline or its homologues,
or sulpho acids, can also be advantageously used for the same purpose.
The following are examples of how I carry out my invention practically.
Example 1.-17.3 lbs. of sulphanilic acid are diazotized with 7 lbs. of nitrite of
soda and 12 lbs. of H CI, 22 Beaumé, in the usual and well known manner.
The diazo-benzene-sulpho-acid thus produced is combined with 25 lbs. of
naphthionate of soda, in presence of enough acetate of soda to bind all mineral acid
present.
After standing several hours, a brownish-red wool dye is produced, and this is
combined, in presence of acetate of soda, with the tetrazo-ditolyl formed from
32 lbs. of tolidine sulphate, or its equivalent of the base, and 14 lbs. of nitrite of
soda.
As soon as all the tetrazo has entered into combination, 25 lbs. of naphthionate of
soda, dissolved in water, are added.
The color is formed very slowly, and should be stirred for several days.
The completion of the reaction is accomplished when dye tests show no
improvement.
The temperature is then raised to boiling point, and enough soda-lye added to
convert the color into its soda-salt.
It is then precipitated with common salt, filtered off, pressed, and dried.
The color dyes unmordanted cotton a bright red in an alkaline or soap bath, and
is fast to washing.
It is similar in shade to that of the color produced by substituting diazo-a- naphtha-
lene-mono-sulpho acid for the diazo-benzene-sulpho acid used for the production of
the red wool dye, (see Specification No. 1276789).
The fact, that in some cases diazo sulpho acids of benzene can be substituted for
diazo sulpho acids of naphthalene, without altering the shade of the color produced,
is well known. (See Specification No. 1065389, Charles Denton Abel, page 4,
lines 16, 17 and 18).
66
In corroboration, Dr. Bayer also says: (on page 3, lines 19, 20 and 21, in
Patent No. 1649387) Dye-stuffs of the same color and possessing the same
properties as the above-mentioned are also obtained, when in place of chrysoidines

page_text: the dye-stuff known as Bismark brown, vesuvine or phenylene brown, (triamido-azo-
benzine,) are employed."
Example 2 It the 17.3 lbs. of sulphanilic acid in Example 1 he replaced by
21-6 lbs. of sulpho-toluic acid, similar shades are obtained.
Example 3 The 25 lbs. of naphthionate of soda used for the production of the
wool colors in Example 1, may be replaced with 35 lbs. of B. B. naphthylamine-di-
sulphonate of sodium.
Example 4-The 25 lbs. of naphthionate of soda used to react on the compound
intermediate in Example 1, may be replaced with 35 lbs. of B. B. naphthylamine-
di-sulphonate of sodium.
If the wool color is formed by diazotizing one molecule of naphthionic acid and
combining it with one molecule of aniline, or its homologues, or the sulpho acids of
these bodies, yellower colors result.
By tetrazo bodies I mean :-
Tetrazo diphenyl and its homologues.
Tetrazo-naphthalene.
Tetrazo-stilbene.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I, HENRY HARINGTON LEIGH, Fel. Inst. P.A., Assoc. Mem. Inst. C.E., practising
as Phillips & Leigh, at No. 22, Southampton Buildings, Chancery Lane, in the County
of Middlesex, Engineer and 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:-
In my specification No. 12767 of 1889, I have described a process for the pro-
duction of cotton colours by combining naphthalene-azo-naphthylamines and their
sulpho-acids with tetrazo bodies to form compound intermediates, and then reacting
on these bodies with amines or phenols.
I have now ascertained that valuable cotton colours can be as well made by com-
bining one molecule of diazo-benzene, or its homologues, or its sulpho acids, with one
molecule of alpha or beta naphthylamine, or its sulpho acids, to produce a body that
can be substituted for the naphthalene-azo-naphthylamines, or their sulpho acids,
which I previously employed.
I have also ascertained that the product formed by combining one molecule of
diazo naphthalene, or its sulpho acids, with one molecule of aniline, or its homologues
or sulpho acids, can also be advantageously used for the same purpose.
The following are examples of how I carry out my invention practically.
Example 1.-17.3 lbs. of sulphanilic acid are di-azotized with 7 lbs. of nitrite of
soda and 12 lbs. of H CI, 22 Beaumé, in the usual and well known manner.
The diazo-benzene-sulpho acid thus produced is combined with 25 lbs. of
naphthionate of soda in presence of enough acetate of soda to bind all mineral acid
present.
After standing several hours, a brownish red wool dye is produced, and this is
combined in presence of acetate of soda with the tetrazo-ditolyl formed from 32 lbs.
of tolidine sulphate, or its equivalent of the base, and 14 lbs. of nitrite of soda.

page_text: As soon as all the tetrazo has entered into combination, 25 lbs. napthionate of soda,
dissolved in water, are added.
The colour is formed very slowly, and should be stirred for several days.
The completion of the reaction is accomplished when dye tests shew no improve-
ment.
The temperature is then raised to boiling point, and enough soda-lye added to
convert the colour into its soda-salt.
It is then precipitated with common salt, filtered off, pressed, and dried.
The colour dyes uninordanted cotton a bright red in an alkaline or soap bath, and
is fast to washing.
It is similar in shade to that of the colour produced by substituting diazo-a-
naphthalene-mono-sulpho acid for the diazo-benzene-sulpho acid used for the pro-
duction of the red wool dye. (See Specification No. 1276780).
The fact that in some cases diazo-sulpho acids of benzene can be substituted for
diazo-sulpho acids of naphthalene without altering the shade of the colour produced,
is well known (see Specification No. 106538 Charles Denton Abel, page 4,
lines 16, 17 and 18).
In corroboration, Dr. Bayer also says: (on page 3, lines 19, 20, and 21 in Patent
No. 1649387), "Dye stuffs of the same colour and possessing the same properties
as the above mentioned are also obtained when in place of chrysoidines, the dye
stuffs known as Bismarck brown, vesuvine, or phenylene brown (triamido-azo-
benzine) are employed."
Example 2-If the 17.3 lbs. of the sulphanilic acid in Example 1 be replaced
by 21-6 lbs. of sulpho-toluic acid, similar shades are obtained.
Example 3-The 25 lbs. of naphthionate of soda used for the production of the
wool colours in Example 1 may be replaced with 35 lbs. of B. B. naphthylamine-di-
sulphonate of sodium.
Example 4-The 25 lbs. of naphthionate of soda, used to react on the compounds
formed in Example 1, may be replaced with 35 lbs. of B. B. naphthylamine-di-
sulphonate of sodium.
If the wool colour is formed by diazotizing one molecule of naphthionic acid and
combining it with one molecule of aniline, or its homologues, or the sulpho acids of
these bodies, yellower colours result.
By tetrazo bodies, I mean

page_text: homologues, or mono, di- or tri-sulphonic acids, and afterwards acting upon the
body thus produced with one molecule of alpha or beta naphthylamine or their mono-
or di-sulphonic acids.
3. As new colouring matters, the dye-stuffs produced by the processes herein
HENRY H. LEIGH.