Improvements in the Manufacture of Soap for use in Dyeing and Finishing Textile Fabrics and Materials and for other Purposes.
Year: 1897

page_text: Date of Application, 27th Oct., 1897-Accepted, 24th Dec., 1897
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Soap for use in Dyeing and
Finishing Textile Fabrics and Materials and for other Purposes.
I. JULIUS STOCKHAUSEN of 105 Fischelnerstrasse Crefeld in the German Empire,
Soap Manufacturer. 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.
This Invention relates to improvements in the process of manufacturing a
gelatinous soap ("Monopole Soap") from sulphonated oils, fats, sebacic acids
and oleic acids, as described in the specification of Letters Patent No. 2896 of
1896.
My present Improvements consist essentially in heating the sulphonated sub-
stance with a large amount of the base as compared with that used in the pre-
paration of "Turkey-red-oil" so that there is obtained a more perfect soap
containing a larger proportion of the base. Suitable bases are alkalies and
metallic oxides and hydrates.
The sulphonated substance may be obtained in the ordinary way of commerce
or it may be specially prepared. In the latter case, 100 parts by weight of
Castor Oil or of other similar or suitable oil, oleic acid or fat, are mixed, with
constant stirring, with about 30 parts by weight of Sulphuric acid having a
strength of about 66° Be. If the mixture is carefully made no sulphurous acid
should be produced. The product is kept in a cool place for one or two days with
an occasional stirring. From whatever source the sulphonated substance may be
obtained, it will hereinafter be called, for the sake of brevity, "sulphonised oil."
In preparing the soap according to the present invention I may proceed in
various ways as will be indicated by the following examples.
EXAMPLE. I.
To 100 parts by weight of the Sulphonised oil there are added 60 parts by
weight of soda lye 30° to 37° Be, all at once, with vigorous stirring. The mix-
ture becomes clear when heated and has a yellowish colour. It is allowed to stand
for some days until the sodium sulphate (Glauber's salt) has crystallised out and
the soap has precipitated. These two substances are then separated and the
soap is boiled until it ceases to foam and a sample becomes gelatinous when cold
and exhibits the characteristics of soap.
EXAMPLE: II.
To 100 parts by weight of the Sulphonised oil there are added from 100 to 200
parts by weight of a lukewarm solution of common salt 25° to 30° Be. for the
purpose of separating the sulphuric acid and other substances. After vigorous
stirring, the mixture is allowed to stand for several days or as long as may be
required until the oil has been completely separated and can be removed by
decantation. To 100 parts of this decanted or separated oil there are added 39
parts of soda lye 36° to 37° Be. all at once, with vigorous stirring. The soap is

page_text: then boiled as described under Example 1, until a cooled sample becomes gelatinous
and shews the characteristics of soap.
It is not always necessary to induce the heating of the mixture by applied heat.
In many cases, especially if there is an excess of sulphuric acid present, the
chemical reaction will produce sufficient heat in itself.
"
It will be evident that weaker solutions than those above specified may be
employed in proportionately larger quantities. In any case the product obtained
is diluted "Monopole soap
and it may be commercially used in this condition
or be previously dried. If a larger quantity of lye or alkali be used an alkaline
soap will be produced.
In Knetch, Rowson & Lowenthal's "Handbuch der Farberei," it is stated, and
the statement is confirmed by other authorities, that the sulphonised oil used in
the preparation of turkey-red oil, is only partially saturated in the ordinary pro-
cess of its preparation by the addition of from 5 to 6 parts of soda lye to 100 parts
of sulphonated oil, the soda lye having a strength of 36° to 37° Be. On the other
hand, by my present improvements I employ three times the quantity or there-
abouts of the base and still obtain, after boiling, an acid or neutral soap. Further,
in the manufacture of turkey-red oil, heating is carefully avoided. The reason
for this is that without the addition of an alkali or with the addition of a small
quantity of alkali, the sulphonised oil becomes decomposed when heated. (See
the before mentioned "Handbuch der Farberei," page 268.) On the contrary with
the addition of a greater quantity of alkali or base according to this invention,
the decomposition of the oil by heating is avoided and complete saponification is
effected, and per contra, if in carrying out my invention, I avoid the application or
production of heat during the process I find it impossible to obtain my product.
The soap I produce differs therefore from turkey-red oil by the facts that I utilise
heat in my process; that I use a larger quantity of alkali or base; that I obtain
a perfect saponification, that I have a solid concentrated product whereas con-
centrated turkey-red oil (85 per cent), is still fluid; and that the properties of
the two substances in use are different. The gelatinous soap which I produce
is not only different but possesses certain advantages as compared with turkey-red
oil and with other soaps. For example, this is the case when dyeing fibres with
benzidines, diamines, and substantitive colouring matters, alone or in combination
with Glaubers salt, common salt, soda and other salts, or in combination with
acids. In such cases my soap is not precipitated and no sediment of soap or
sebacic acid is produced upon the fibre: Also, since the lime salt of sebacic acid
is soluble in water, no precipitate will be produced when water containing lime
is used in the dyeing bath. The dye bath is more perfectly utilised when my new
soap is used in it and a darker shade can be thus obtained, which means a saving
of colouring matter. For these reasons, semi-silk materials dyed in baths con-
taining the soap, become especially bright and the cotton is dyed a darker shade
than the silk, which result is very desirable. If Marseilles soap were used alone,
only light and faint shades would be produced by the colouring matters as com-
pared with the result from the same bath if my soap be employed. Moreover,
if when Marseilles soap is used and Glauber's and other salts are added, the soap
is precipitated, or if acids be added the soap is decomposed and sebacic acid will
be precipitated, in either case the precipitate settles in the fibres and the product
cannot therefore be so bright and stains will occur. If again, turkey-red oil is
used, in a similar way, the silk will be dyed darker than the cotton, which is
disadvantageous. The same or similar differences will occur in the dyeing of
semi wool or other fabrics composed of mixed animal and vegetable fibres. The
- fibres become bright and soft when the "Monopole soap" is used whilst the use
of turkey-red oil renders them dull and sticky. In the dyeing of all silk or semi
silk fabrics in a bath containing my soap, with alkali blue, a better extraction
of the colouring matter is effected. I have already shewn that my soap does not
produce a precipitate of lime or magnesia soap from baths containing lime or
magnesia, and it may therefore be advantageously used in all cases where ordinary

page_text: soaps have been precipitated. Because of its properties, my soap may be used as
an addition to ordinary soap baths, because it at once brings in to re-solution any
precipitates from these soaps; thus, decomposed baths can by its use be at onco
restored.
وو
When colouring matters have to be fixed by metallic mordants, especially the
alizarine colours, if my "Monopole" soap is used instead of "bast-soap" (the
soap derived from soap solutions in which raw silk has been boiled), the larger
quantity of alkali involved effects the better fixing of the metallic oxide. Accord-
ingly it may be used for dyeing and printing purposes with equally advantageous
effects. Not only in direct dyeing with substantive colouring matters
but also in dyeing processes involving the use of mordants and in finishing
processes such as sizing, the use of my soap is advantageous because it
will not be precipitated by larger quantities of common salt, Glauber's salt,
Epsom salt and the like, and because more saturated shades in dyeing are produced.
It is possible also to add a larger proportion of the said salts without producing the
separation of dibasic acid or dibasic salts. In finishing and sizing apart from
dyeing, the use of my soap instead of turkey-red oil, fats, and other soaps, in
combination with salts is very advantageous for the same reasons. Ordinary soaps
cannot be so used because the salts precipitate them; nor fats, because they
separate out on cooling and sometimes float on the surface of the mixture; turkey-
red oil makes the goods sticky and in the presence of large quantities of salts such as
Epsoms, produce emulsions which settle down upon the goods as oil. I may use
my soap up to 40 parts by weight with 200 parts of Epsoms and 200 parts of
dextrine per 1000 parts of finishing mixture without causing any separation. The
soap prepared as herein before described may be used alone in finishing, and, as
it becomes firm when dry, it acts as a consistent fat and so produces a better
finish than turkey-red oil which never becomes hard and is hygroscopic so that
goods finished with it soon become flabby and poor looking. A further dis-
advantage attending the use of turkey-red oil is that, especially in the case of
white goods, the fabrics soon become yellow and acquire a rancid smell. All these
disadvantages are avoided by the use of "Monopole soap," and goods treated with
it neither alter nor acquire a disagreeable smell. As it does not precipitate lime
salts and may simply be washed out even with water which contains a large
quantity of lime, it may advantageously be used for imparting such a finish to
fabrics as is now obtained by treating them with fats and oils. In such cases it
is not necessary to use so large a quantity of soda or alkali as is usual when washing.
It remains only to be added that the "Monopole" soap” can be used in connec-
tion with other soaps and with turkey-red oil.
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:-
1. The hereinbefore described process for the manufacture of a gelatinous soap
which consists in heating a sulphonised oil or a sulphonised equivalent of oil in
presence of a much larger proportion of alkali or other suitable base or salt than
is employed in the preparation of turkey-red oil, in such a manner as to produce
saponification, substantially as hereïnbefore described.
2. The herein before described process for the manufacture of a gelatinous soap
which consists in boiling a sulphonised oil or a sulphonised equivalent of oil in
presence of a much larger proportion of alkali or other suitable base or salt than
is employed in the preparation of turkey-red oil, in such a manner as to produce
saponification, substantially as hereinbefore described.
3. As a new article of manufacture, a gelatinous soap produced as set forth
in the first and second claims with reference to the description hereinbefore con-
tained.
4. The use of the gelatinous soap manufactured according to claims 1 and 2
above, in connection with dyeing by means of direct or substantive colouring

page_text: matters, either alone or in combination with salts, acids, other soaps, turkey-red
oils, or bases, or in connection with dyeing and printing processes in which mordants
are employed, or with the process of dyeing alkali-blue or silk and semi silk
goods, or with finishing and sizing processes apart from dyeing or colouring, for
fattening textures in spinning, for the renewal of decomposed soap baths, and to
prevent the generation of lime soap.