Improvements in the Manufacture and Application of a New Diazo Compound for Use in Dyeing and Printing.
Year: 1894

page_text: This Print is in accordance with the Original Specification as it stands after
Amendment (under Section 11 of the Patents, &c. Act, 1883), as required by
the decision of the Chief Examiner of the 3rd day of October 1895.
Date of Application, 8th Mar., 1894
Complete Specification Left, 12th Dec., 1894-Accepted, 8th Mar., 1895
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture and Application of a New Diazo
Compound for Use in Dyeing and Printing.
I, Dr. JULIUS ALTSCHUL, Chemist, of 45 Woodland Street, Cheetham Hill,
Manchester do hereby declare the nature of this invention to be as follows:-
I have lately described the production and application of a new diazocompound
for use in dyeing and printing. The new product, which could, by dissolving it in
acids, he converted into a solution of p-nitrodiazobenzene, was supposed to be a
sodium salt of the latter compound and has indeed proved to be of a composition
indicated by the formula C.H.(NO2) N₂ONa, the rational constitution of which
I need not discuss here, as it does not influence the nature of my invention.
'
As to the manufacture and application of the above product, for which I
have used the name of "nitraniline S" I have made the following new
observations:
1) Nitraniline S, as prepared by neutralizing a solution of a p-nitrodiazobenzene
salt with alkali, and salting out, has been found to possess, in a dry and pure state,
considerable explosive power, being decomposed under violent detonation, at a
temperature of about 230° C.
It is my invention to have found, that this explosive character can be easily
overcome by mixing nitraniline S either before or after drying, with suitable
anorganic matter especially with metallic salts containing water of crystallisation.
Even a small amount of anorganic matter will diminish the explosive character of
nitraniline S considerably and by increasing the amount of the addition, for
instance of common salt, Glaubers salt, sulphate of magnesia and so on, mixtures
are obtained which decompose, when heated to high temperature, without any
violent reaction. The technical value of nitraniline S is consequently much
increased by the addition of the anorganic matter.
2) I have stated that nitraniline S prepared as shown above can be converted
into the p-nitrodiazobenzene solution, required for developing nitraniline red, by
dissolving it in acids and, if mineral acids have been used, saturating the same by
addition of sodium acetate.
As to the application of organic acids in this process, I have found that, at low
temperature, nitraniline S dissolves only slowly in acetic acid, but that the
solution can quickly be gained at a somewhat bigher temperature. I dissolve for
instance
Oil nitroniling Sin

page_text: I then heat the mixture a short time to about 50°-60° C. when a solution is
quickly obtained, which after filtring and cooling down is at once ready for use,
the addition of sodium acetate being of course spared as no mineral acid has
been used.
The proportions and other details of the above example may be varied in many
respects without materially affecting the result.
Dated this 7th day of March 1894.
Improvements in the Manufacture and Application of a New Diazo
Compound for Use in Dyeing and Printing.
I, Dr. JULIUS ALTSCHUL, Chemist, of 45 Woodland Street, Cheetham Hill,
Manchester, 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 :-
I have lately described the production and application of a new diazo compound
for use in dyeing and printing.
The new product, which could, by dissolving it in acids, be converted into a
solution of para-nitro-diazobenzene, was supposed to be a sodium salt of the latter
compound and has indeed proved to be of a composition indicated by the
formula C&H (NO2)N,ONa, the rational constitution of which I need not discuss.
here, as it does not influence the nature of my invention.
As to the manufacture and application of the above product, for which I
have used the name of "nitraniline S" I have made the following new
observations.
1) Nitraniline S as prepared by saturating a solution of para-nitro-diazobenzene
salt with alkali and salting out has been found to possess in a dry and pure state,
considerable explosive power, being decomposed with violent detonation, at a
temperature of about 230° C.
According to my invention this explosive character is removed by mixing the
nitraniline S before or after drying with suitable inorganic matter especially with
metallic salts containing water of crystallisation. Even a small addition of
inorganic matter considerably lessens the explosive character, and by increasing
the amount added for instance of common salt, Glauber salt, sulphate of magnesia
and the like mixtures are obtained, which when heated to high temperature are
decomposed without any violent reaction. The technical value of nitraniline S is
consequently much increased by the addition of the inorganic matter.
2) Nitraniline S, mixed as above described can be converted into the para-nitro-
diazobenzene solution required for developing nitraniline red, by dissolving it in
acids, and when mineral acids are used, saturating them by addition of sodium
acetate.
As to the application of organic acids in this process, I have found that, at low
temperature nitraniline S dissolves only slowly in acetic acid, but that the solution
can be quickly obtained at a somewhat higher temperature. I dissolve for
instance
Lituanilion α in

page_text: addition of sodium acetate being of course dispensed with as no mineral acid
is used.
The proportions and other details in the above example may be varied without
materially affecting the result.
If for instance, instead of pure "nitrauiline S" its mixture with salts as
described under head 1) is to be used, the quantities of water and acid should
of course be reduced to suit the contents of pure "nitraniline S" in the
mixture.
As to the proportions in which inorganic matter should be added I have found
that a mixture containing one part of one of the salts named and one part of
"nitraniline S" may be safely used for all practical purposes; an addition of
more salt, though scarcely necessary, can of course only increase the safety of the
product.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I hereby declare that
I am aware of Johnson's Specification No. 20605 of 1893 and I make no claim to
anything described and claimed therein. I am also aware that the substance
I have herein called nitraniline S is identical with the new nitrosamine in the form
of sodium compound mentioned in the said Specification and which substance I do
not claim, and I declare that what I claim is :
.1. The herein described method of rendering inexplosive the "nitraniline S"
obtained on saturating a solution of para-nitrodiazo-benzene salt with alkali and
salting out, by mixing it with inorganic matter of the kinds hereinbefore
mentioned.
2. The conversion of the mixture referred to in the preceding claim into a
nitro-diazo-benzene solution suited for dyeing or printing, substantially as
described.
Dated this 8th day of December 1894.
ABEL & IMRAY,
Agents for the Applicant.