Manufacture of Alumina Salts of the Naphthol Sulphonic Acids.
Year: 1892

page_text: Date of Application, 4th June., 1892
Complete Specification Left. 27th Feb., 1893-Accepted, 8th Apr., 1893
PROVISIONAL SPECIFICATION.
[Communicated from abroad by THE FARBWERKE VORMALS MEISTEr Lucius
AND BRUNING, of Hoechst a- Main, Germany, Chemical Manufacturers.]
Manufacture of Alumina Salts of the Naphthol Sulphonic Acids.
I, CHARLES DENTON ABEL, of No. 28 Southampton Buildings, Chancery
Lane, in the County of London, Chartered Patent Agent, do hereby declare the
nature of this invention to be as follows:-
The alumina-salts of the alpha- and beta-naphthol-sulphonic acids (according to
Dr. Heinz and Dr. Liebrecht of Breslau) are of extraordinary astringo-antiseptic
action. My correspondents have prepared a large number of such alumina-salts.
The action of these salts is not in all cases the same. The product of greatest
value amongst them appears so far to be the alumina-salt of the beta-naphthol-
disulphonic acid R.
The manner of producing the salts is substantially the following:-the barium
lead or calcium salt of the sulphonic acid is prepared and this salt is transformed
by boiling it with the suitable quantity of sulphate of alumina.
EXAMPLE.
Production of the alumina-salt of beta-naphthol disulphonic acid R.
15 parts by weight of beta-naphtholdisulphonate of sodium R of 69 per cent. is
dissolved in 60 parts by weight of boiling water and, while being kept continually
stirred is mixed with a hot concentrated solution of 7 parts by weight of com-
mercial chloride of barium in crystals. In this operation the barium salt of the
acid R precipitates in gelatinous form, which however, after further stirring passes
over into a well washable form. It is cooled by means of ice and sucked off.
The barium salt well washed and freed from the chloride of calcium is transformed
by means of the requisite quantity of sulphate of alumina. To this effect the
barium-salt is suspended in 40 parts by weight of boiling water and mixed with
the requisite quantity of sulphate of alumina in hot concentrated solution.. The
liquid is filtered off from the sulphate of barium and the filtrate concentrated;
in this operation the alumina-salt (the alumnol) separates in the form of white
crusts which are dried and ground. The alumnol thus obtained is in form of a
white powder of astringent taste and easy solubility in water.
These alumina salts can be produced also by preparing for example from lead or
barium salt the free sulphonic acids, and boiling the same with hydrate of alumina.
This is done by admixing for example the barium salt with the requisite quantity
of sulphuric acid, filtering off from the sulphate of barium, boiling the filtrate with
hydrate of alumina, filtering again and concentrating the filtrate.
In the same manner can be produced the alumina salts of:-
Croceine sulphonic acid.
a- and -naphtholsulphonic acids of Schäffer.
Naphtholsulphonic acid F.
6-naphtholdisulphonic acid G.

page_text: All these aluminå salts have similar qualities and only differ the one from the
other in their degree of solubility in water.
Dated this 4th day of June 1892
ABEL & IMRAY,
Agents for the Applicant.
COMPLETE SPECIFICATION.
Manufacture of Alumina Salts of the Naphthol Sulphonic Acids.
1, CHARLES DENTON ABEL, of No. 28, Southampton Buildings, Chancery
Lane, in the County of London, Chartered 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 :-
The alumina-salts of the alpha- and beta-naphthol-sulphonic acids (according to
Dr. Heinz and Dr. Liebrecht of Breslau) are of extraordinary astringo-antiseptic
action. My correspondents have prepared a large number of such alumina-salts.
The action of these salts is not in all cases the same. The product of greatest
value amongst them appears so far to be the alumina-salt of the beta-naphthol-
disulphonic acid R.
The manner of producing the salts is substantially the following; the barium;
lead or calcium salt of the sulphonic acid is prepared, and this salt is transformed;
by boiling it with the suitable quantity of sulphate of alumina.
EXAMPLE.
Production of the alumina-salt of beta-naphthol disulphonic acid R.
15 parts by weight of beta-naphtholdisulphonate of sodium R of 69 per cent. is
dissolved in 60 parts by weight of boiling water and, while being kept continually
stirred, is mixed with a hot concentrated solution of 7 parts by weight of
commercial chloride of barium in crystals. In this operation, the barium salt of
the acid R precipitates in gelatinous form, which however, after further stirring,
passes into a condition in which it can be well washed. It is cooled by means of
ice and sucked off. The barium salt well washed and freed from the chloride of
calcium is transformed by means of the requisite quantity of sulphate of alumina.
To this effect, the barium-salt is suspended in 40 parts by weight of boiling water
and mixed with the requisite quantity of sulphate of alumina in hot concentrated
solution. The liquid is filtered off from the sulphate of barium and the filtrate is
concentrated.
In this operation the alumina salt, which may be termed aluminol, separates in
the form of white crusts which are dried and ground. The alumina compound or
aluminol thus obtained is in the form of a white powder of astringent taste, easily.
soluble in water.
These alumina salts can also be produced, provided that the free acid is stable ;
by preparing, for example, from lead or barium salt, the free sulphonic acids and
boiling the same with hydrate of alumina. This is done by mixing, for example,
the barium salt with the requisite quantity of sulphuric acid, filtering off from the
sulphate of barium, boiling the filtrate with hydrate of alumina, filtering again and
concentrating the filtrate."
In the same manner can be produced the alumina salts of the other sulphonic
acids of the alpha and beta-naphthol, as for example of
a- and -naphtholsulphonic acids of Schäffer.
a-naphtholmonosulphonic acid 1. 3.
a-naphtholsulphonic acid of Liebmann and Studer.
a-naphtholsulphonic acid S.
a-naphtholdisulphonic said S

page_text: попотаватрпоите аста 1, 4, 7,
a-naphtholdisulphonic acid 1. 4. 6.
a-naphtholdisulphonic acid 1. 4. 7.
a-naphtholtrisulphonic acid (for Chromotrops).
a-naphtholsulphonic acid 1. 4.
a-naphtholdisulphonic acid (for dinitro-a naphthol).
a-naphtholtrisulphonic acid (for naphthol yellow Ś).
a-naphthol-e-disulphonic acid (German Letters Patent 145776) croceine sulphonic
acid.
B-naphtholsulphonic acid F.
B-naphtholdisulphonic acid G.
B-naphtholsulphonic acid 2. 5.
B-naphtholtrisulphonic acid (German Letters Patent 22038).
B-naphthol-y-monosulphonic
acid.
B-naphtholdisulphonic acid C.
B-naphthol-8-disulphonic acid (German Letters Patent 44079).
All these alumina salts have similar qualities, and only differ the one from the
other, in their degree of solubility in water.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, I declare that what I
claim is :-
1. The manufacture of alumina salts of the alpha and beta naphtholsulphonic
acids by transforming the barium, lead or calcium salt of these acids by means of
sulphate of alumina or by treating the free sulphonic acids with hydrate of
alumina.
2. The alumina salts produced in the manner above referred to, examples of
which are hereinbefore mentioned.
Dated this 27th day of February 1893
ABEL & IMRAY,
Agents for the Applicant.