Improvements relating to the Separation of Fat and Fatty Acids from Compounds Containing the same.
Year: 1886

page_text: Date of Application, 15th Sept., 1886.
Complete Left, 13th June, 1887.
Complete Accepted, 15th July, 1887.
Improvements relating to the Separation of Fat and Fatty Acids
from Compounds Containing the same.
I, WILHELM GRAFF, of Lesum, near Bremen, in the Empire of Germany,
Manufacturer do hereby declare the nature of this invention to be as follows
This invention relates to the treatment of water in which wool has been washed in
order to obtain the grease and fatty acids therefrom.
As is known, the washing water of wool-washing-and-combing works contains
principally fat, soap, and carbonate of an alkali. By treating the said water by a
neutral calcium chloride solution, as frequently practised, lime, soap, and grease are
precipitated as well as a quantity of calcium carbonate, which is produced by the
decomposition of the calcium chloride by the carbonate of an alkali. The presence of
calcium carbonate however retards the separation of the said substances from the
liquid, increases the density of the precipitate and renders difficult the subsequent
operations for extracting the grease and fatty acids.
According to the present invention these defects are obviated by effecting the
precipitation through the medium of an acid calcium chloride solution, that is to say a
solution of calcium chloride which contains free hydrochloric acid, instead of by a
neutral calcium chloride solution. Hydrochloric acid may be added to the water to
be treated before addition of the calcium chloride for effecting the precipitation..
In order to carry out this process I prefer, however, to first prepare a solution of
calcium chloride and with this mix so much hydrochloric acid that the reaction of the
liquid filtered from the deposit to be subsequently obtained is not acid. This solution
is next added to the waters contained in the collecting vessels of the wool-washing
works, and stirred or agitated by blowing in steam or air.
Owing to the presence of the hydrochloric acid, the carbonate of an alkali is
converted into soluble sodium chloride or potassium chloride, while carbonic acid
escapes, whereas the precipitate contains sebate of lime (lime soap) and fat, and very
little, if any, calcium carbonate, according as sufficient care has been taken in adding

page_text: the hydrochloric acid. The following two formulæ shew the chemical actions in the
precipitation by acid and neutral calcium chloride. In the application of the former
Ca Cl + 2 HCI + 2 NaF + Na, CO, = Ca F, + 4 Na Cl + CO2 + H, O takes place;
whilst by the application of the latter 2 Ca Cl, + Na, CO, + 2 Na F = Ca F,
+4 Na Cl + Ca CO₂, is the result.
In these formulæ, the letter F is to indicate concisely the quantity of fatty acids
contained in the wash waters. The quantity of the acid calcium chloride solution to
be added to the wash waters depends upon the proportion of soap and carbonate of an
alkali in each case.
The quantity of acid added to the calcium chloride solution should be such that
after the precipitation of the wash waters the reaction of the liquid is neutral, and
under no circumstances acid. Moreover so much solution of calcium chloride is to be
added to the wash waters that no deposit takes place after further addition.
The wool fat contained in the precipitate can be extracted in the known manner
with benzine. But in this operation not only neutral non-saponifiable fats are
extracted, but also fatty acids, free as well as combined with cholesterine. Further-
more the benzine takes up undecomposed soap which always remains in the deposit.
These defects are not only shewn in the deposit caused by the acid calcium chloride
solution but also in the deposit caused by neutral calcium chloride,
If however a quantity of caustic lime is added to the calcium chloride deposit
immediately after the precipitation, for the purpose of combining all the fatty acids
which are free or combined with cholesterine or alkali, all the said fatty acids are
found combined with lime, after the drying of the deposit separated from the liquid
in a steam bath. In the ensuing treatment with benzine, the fats which are non-
saponifiable are extracted, and the remaining mass contains, besides the mechanical
impurities, lime soap, which treated with hydrochloric acid, produces fatty acids.
A further advantage of this decomposition of the lime soap by hydrochloric acid
is that, owing to the want of calcium carbonate, considerably less quantities of hydro-
chloric acid are required.
Whilst the deposit obtained by acid calcium chloride requires only two equivalents
of hydrochloric acid to effect its decomposition according to the first of the above
stated formulæ, four equivalents are required for decomposing the deposit obtained by
neutral calcium chloride.
As hydrochloric acid has always to be added in excess when the decomposition
takes place, the acid calcium chloride solution necessary for precipitating the wash
waters is obtained and is therefore continually used again in the process.
As compared with the treatment of wool washing waters by lime milk for effecting
the precipitation, the present process has the great advantage that the water running
from the deposit contains chiefly common salt or potassium chloride, and can thus be
led into rivers without any risk; whilst, when using lime milk, the water led away,
owing to its containing caustic potash or soda must previously be freed from the
latter.
Dated thin 15th dow of Santamba 1006
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C.,
Agents for the Applicant.

page_text: from Compounds Containing the same.
1, WILHELM GRAFF of Lesum, near Bremen, in the Empire of Germany,
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 the treatment of water in which wool has been washed in
order to obtain the grease and fatty acids therefrom.
As is known the washing water of wool-washing and combing works contains
principally fat, soap, and carbonate of an alkali. By treating the said water by a
neutral calcium chloride solution, as frequently practised, lime soap and grease are
precipitated as well as a quantity of calcium carbonate, which is produced by the
decomposition of the calcium chloride by the carbonate of an alkali. The presence of
calcium carbonate however retards the separation of the said substances from the
liquid, increases the quantity of the precipitate, and renders difficult the subsequent
operations for extracting the grease and fatty acids.
According to the present invention these defects are obviated by effecting the
precipitation through the medium of an acid calcium chloride solution that is to say
a solution of calcium chloride which contains free hydrochloric acid, instead of by a
neutral calcium chloride solution. Hydrochloric acid may be added to the water to
be treated before addition of the calcium chloride for effecting the precipitation.
In order to carry out this process I prefer, however, to first prepare a solution of
calcium chloride and with this mix so much hydrochloric acid that the reaction of the
liquid filtered from the deposit to be subsequently obtained is not acid. This solution
is next added to the waters contained in the collecting vessels of the wool washing
works, and stirred or agitated by blowing in steam or air.
Owing to the presence of the hydrochloric acid, the carbonate of an alkali is
converted into soluble sodium chloride or potassium chloride, while carbonic acid
escapes, whereas the precipitate contains sebate of lime (lime soap) and fat, and very
little, if any, calcium carbonate, according as sufficient care has been taken in adding
the hydrochloric acid. The following two formulæ show the chemical actions in the
precipitation by acid and neutral calcium chloride. In the application of the former
Ca Cl, +2 HCl + 2 Na F + Na, CO, = Ca F, + 4 Na Cl + CO, + H, O takes place;
whilst by the application of the latter, 2 Ca Cl, + Na, CO, + 2 Na F
Ca F,
+4 Na Cl + Ca CO,, is the result.
=
In these formulæ, the letter F is to indicate concisely the fatty acids contained in
the wash waters. The quantity of the acid calcium chloride solution to be added to
the wash waters depends upon the proportion of soap and carbonate of an alkali in
each case..
The quantity of acid added to the calcium chloride solution should be such that after
the precipitation of the wash waters the reaction of the liquid is neutral, and under no

page_text: .
circumstances acid. Moreover so much solution of calcium chloride is to be added to
the wash waters that no deposit takes place after further addition.
The wool fat. contained in the precipitate can be extracted in the known manner
with benzine. But in this operation not only neutral non-saponifiable fats are
extracted, but also fatty acids, free as well as combined with cholesterine. Further-
more the benzine takes up undecomposed soap which always remains in the deposit.
These defects are not only shown in the deposit caused by the acid calcium chloride
solution but also in the deposit caused by neutral calcium chloride.
If however a quantity of caustic lime is added to the calcium chloride deposit
immediately after the precipitation, for the purpose of combining all the fatty acids
which are free or combined with cholesterine or alkali, all the said fatty acids are
found combined with lime, after the drying of the deposit separated from the liquid
in a steam bath. In the ensuing treatment with benzine, the fats which are non-
saponifiable are extracted, and the remaining mass contains besides the mechanical
impurities, lime soap, which treated with hydrochloric acid, produces fatty acids.
A further advantage of this decomposition of the lime soap by hydrochloric acid is
that, owing to the want of calcium carbonate, considerably less quantities of hydro-
chloric acid are required.
Whilst the deposit obtained by acid calcium chloride requires only two equivalents
of hydrochloric acid to effect its decomposition according to the first of the above
stated formulæ, four equivalents are required for decomposing the deposit obtained by
neutral calcium chloride.
As hydrochloric acid has always to be added in excess when the decomposition
takes place, the acid calcium chloride solution necessary for precipitating the wash
waters is obtained and is therefore continually used again in the process.
As compared with the treatment of wool washing waters by lime milk for effecting
the precipitation, the present process has the great advantage that the water running
from the deposit contains chiefly common salt or potassium chloride, and can thus be
led into rivers without any risk; whilst, when using lime milk, the water led away,
owing to its containing caustic potash or soda must previously be freed from the
latter.
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 treatment of waters in which wool has been washed and which chiefly
contain fat fatty acids and carbonate of an alkali with calcium chloride, hydro-
chloric acid being added, to prevent the formation of carbonate of lime, for the
purpose specified.
Second. Mixing the lime deposit obtained by precipitation with acid or neutral
calcium chloride from water in which wool has been washed with caustic lime, and
drying the mixture in a steam bath or by the application of other heat, for the purpose
of combining with lime all the fatty acids which are still free or combined with
cholesterine or an alkali, with lime thus rendering the deposit suitable for further
treatment for the extraction of the non-saponifiable fats by means of benzine or the
like.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London,
Agents for the Applicant.