IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE OF COLORING MATTERS
Year: 1884

page_text: I WILLIAM ROBERT LAKE of the firm of Haseltine Lake & Co Patent Agents
Southampton Buildings in the County of Middlesex do hereby declare the nature
of said invention for "IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE
OF COLORING MATTERS to be as follows:-
,,
This invention relates to the manufacture of orange-red and violet coloring
matters, obtained by causing the diazo-compounds of amines or of their sulpho-
conjugated derivatives to act upon the disulpho a naphthol (disulfo a napthol) and
to the preparation of disulpho a naphthalic acid (acide disulfo a naptholique).
Preparation of the disulpho a naphthalic acid (acide disulfo a naptholique).
I heat a mixture of 30 kilograms of a naphthol and 90 kilograms of mono-
hydrated sulphuric acid to a temperature of from 100 to 110 degrees centigrade for
a period of from 8 to 10 hours. At the expiration of this period of time, the
resulting product is poured into 600 kilograms of cold water, converted into a
calcium salt by saturation with milk of lime, and then into a soda salt.
Preparation of the coloring matter.
By causing the diazo-derivatives (derivés diazoiqúes) of amines or of their
sulpho-conjugated derivatives (sulfo-conjugués) to act upon the disulpho a naphtho-
late of sodium, (disulfo a naptholate de sodium) in solution in water, a series
of coloring matters are obtained the shades of which vary from orange-red to
violaceous red.
Thus can be obtained
With diazo-benzol (diazobenzol) an orange coloring matter.
With diazo-sulpho aniline (diazosulfanilique) a reddish orange coloring matter.
With their higher homologous compounds, orange coloring matters gradually
becoming more and more red.
With diazo-naphthylamine (diazonapthylamine), a violet red coloring matter.
With diazo-naphthionic acid (diazonapthionique) a violet color.
With their homologous compounds, violet coloring matters.

page_text: With mono-sulpho-diazo-azo-benzol, (monosulfodiazo-benzol) a violet coloring
matter.
With disulpho-diazo-azo-benzol, (disulfo-diazo-azobenzol) a violet coloring.
matter.
With their homologous compounds, violet coloring matters.
These coloring matters are characterised by the peculiar property which they
have, of becoming slowly fixed, in acid tinctorial baths, upon textile animal fibres.
They resemble in this particular vegetable coloring matters.
I will mention in particular, the derivatives of xylidine, of amido-azo-benzol)
(amido azo benzol) and of its sulpho-conjugated derivatives which may advan-
tageously replace litmus in the dyeing of wool and silk.
For example, I take 10 kilograms of aniline, 30 kilograms of hydro-chloric acid
and 100 kilograms of water, and after cooling this solution by means of ice to
0° centigrade I add thereto a concentrated aqueous solution of 7.4 kilograms
of nitrite of sodium perfectly pure whilst the temperature is maintained at
2° centigrade.
The solution of hydro-chlorate of diazo-benzol (chlorhydrate de diazobenzol) thus
obtained is poured into a solution containing an excess of disulpho-a-naphthalate
of sodium (disulfo a naptholate de sodium) that is to say a quantity corresponding
to 30 kilograms of a naphthol, to which is added an excess of ammonia, in such a
manner as to render the liquor alkaline after the complete addition of diazo-benzol
(diazo-benzol).
The coloring matter formed is precipitated by the salt, filtered, pressed, re-
dissolved in boiling water and precipitated a second time; after this treatment, it
is collected, pressed and dried.
HASELTINE, LAKE & Co.,
For the Applicant.

page_text: I, WILLIAM ROBERT LAKE, of the firm of Haseltine, Lake & Co, Patent Agents,
Southampton Buildings in the County of Middlesex do hereby declare the nature
of my invention for "IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE OF
COLORING MATTERS and in what manner the same is to be performed, to be
particularly described and ascertained in and by the following statement :-
"
This invention relates to the manufacture of orange-red and violet coloring
matters, obtained by causing the diazo-compounds of amines or of their sulpho-
conjugated derivatives, to react upon the disulpho a naphthol (disulfo a naphtol),
and to the preparation of disulpho a naphtholic acid (acide disulfo a naphtolique).
In the preparation of the disulpho a naphtholic acid (acide disulfo a naphto-
lique) I heat a mixture of 30 kilograms of a naphthol and 90 kilograms of
monohydrated sulphuric acid to a temperature of from 100 to 110 degrees
Centigrade for a period of from 8 to 10 hours. At the expiration of this period
of time, the product is poured into 600 kilograms of cold water, converted into a
calcium salt by saturation with milk of lime, and then into a sodium salt.
In the preparation of coloring matter the diazo-derivatives (derivés diazoiqués)
of amines or of their sulphur combinations (sulfoconjugués) are caused to react
upon the disulpho a naphtholate of sodium, (disulfo a naphtolate de sodium) in
solution in water, whereby a series of coloring matters is obtained, the shades of
which vary from orange-red to violet-red.
Thus can be abtained :-
With diazo-benzol (diazobenzol) an orange coloring matter.
With diazo-sulpho aniline (diazosulfanilique) a reddish orange coloring matter.
With their higher homologous compounds, orange coloring matters gradually
becoming more and more red.
With diazo-naphthylamine (diazonaphtylamine) a violet red coloring matter.
With diazo-naphthionic acid (diazonaphtionique) a violet color.
With their homologous compounds, violet coloring matters.
With diazo-azo-benzol (diazoazobenzól) a violet red coloring matter.
With mono-sulpho-diazo-aza-benzol (monosulfodiazo-azo-benzol) a violet coloring
matter.
With disulpho-diazo-azo-benzol, (disulfo-diazo-azobenzol) a violet coloring
matter.
With their homologous compounds, violet coloring matters.
These coloring matters are characterized by the peculiar property which they
have of becoming slowly fixed, in acid tinctorial baths, upon textile animal fibres.
They resemble in this particular vegetable coloring matters. I will mention
especially the derivatives of xylidine, of amido-azo-benzol (amido azo benzol) and
of its sulphur combinations (sulfoconjugués) which may advantageously replace
litmus in the dyeing of wool and silk.
For example, I make a solution of 10 kilograms of aniline, 30 kilograms of
hydrochloric acid and 100 kilograms of water, and, after cooling this solution by

page_text: means of ice to 0° Centigrade, I add thereto a concentrated aqueous solution of
74 kilograms of nitrite of sodium, preferably pure, whilst the temperature is
maintained at 2° Centigrade.
The solution of hydrochlorate of diazo-benzol (chlorhydrate de diazobenzol) thus
obtained is poured into a solution containing an excess of disulpho-a-naphtholate
of sodium (disulfo a naphtolate de sodium), that is to say a quantity corresponding
to 30 kilograms of a napthol, to which is added an excess of ammonia, in such a
manner as to render the liquor alkaline after the complete addition of diazo-benzol
(diazo-benzol). The coloring matter formed is precipitated by salt, filtered, pressed,
re-dissolved in boiling water and precipitated a second time; after this treatment,
it is collected, pressed, and dried.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what
I claim is
First. The preparation of disulpho a naphtholic acid (acide disulfo a naphtolique)
in the manner above described.
Second. The preparation of coloring matters obtained by causing the diazo-
derivatives of amines (dérivés diazoiques des amines) or of their sulpho-conjugated
derivatives (dérivés sulfo-conjugués) to react upon the said acid, these coloring
matters (and principally those which are obtained from xylidine, from amido-azo-
benzol (amidoazobenzol), or from their sulpho-conjugated derivatives (dérivés
sulfoconjugués) having the property of becoming slowly fixed upon textile animal
fibres in acid tinctorial baths,