Improvements relating to the Washing or Cellulose Threads, Films and the like,
Year: 1899

page_text: Date of Application, 4th Dec., 1899
Complete Specification Left. 20th July, 1900-Accepted. 20th Oct.. 1900
PROVISIONAL SPECIFICATION.
Improvements relating to the Washing or Cellulose Threads,
Films and the like,
We, Dr. Max FREMERY, Chemist, and JOHANNES URBAN, Engineer, both of
No. 6, Dorfstrasse, Oberbruch, Reg. Bez, Aachen, in the German Empire, do
hereby declare the nature of this invention to be as follows:-
In the process described in the Specification left with our former application
for Letters Patent dated 28th March 1899, No. 6641, cellulose threads, films or
the like are washed by liquid which is caused to irrigate, successively and from
above, the rollers or spools on which the threads or nims are spooled or wound,
these rollers or spools being supported one over the other. According to the
above process, water is proposed as the washing liquid for this purpose.
Experiments have now shown that in this process, it is important that the
washing liquid shall be prepared in such a manner that-it separates or removes
the metal or the metallic compounds from their fixed combination with cellulose
and converts them into the form of a soluble salt or salts. The cellulose products
which are here considered, are prepared from cellulose solutions, for example,
fine silk-like threads. Cellulose solutions of this kind are produced by dissolving
cellulose in a suitable solvent, for example, in an ammoniacal solution of cupric
oxide, or a solution of chloride of zinc. From these solutions, cellulose threads,
for example, are obtained by conducting a fine jet of the solution through
chemicals which either decompose the solvent (such, for example, as acids), or
have themselves a coagulating action (such, for example, as alcohol, common salt
solution, and the like).
It has now been shown that, with the cellulose products so produced, a part of
the cellulose always remains in fixed combination with the particular metal or
the particular compound of the solvent.
According to the process described in the Specification of the aforesaid applica-
tion for Letters Patent, this metallic residue or residue of a metallic compound
which is scarcely removable by simple washing with water (even with large
quantities of water), is for the greater part removed, if the washing be effected
in the systematic manner indicated above.
In the above mentioned specification washing with water only is
referred to. This washing can however be also effected very easily in an analogous
manner with any liquid which is suitable for converting this metallic residue or
the residue of a metallic compound into the form of a soluble salt. It is how-
ever also in this case advantageous to irrigate the cellulose threads on the rollers
or spools supported one over the other, in accordance with the process described
in the Specification of our said former application for Letters Patent, this being
effected on the counter current principle with the washing liquid and moreover
to employ the washing liquid in as dilute a condition as possible and in the
smallest possible quantity.
If an acid, for example, is employed as a precipitating or separating agent,

page_text: the residue of acid left behind in the cellulose object, in the described method
of washing, may often suffice for dissolving out the combined residue of metal
or for decomposing the residue of the metallic compound and for removing the
same, so that, in this case, for the systematic washing, ordinary clean water
or distilled water can be used as washing water. In the researches, it however
appeared that, in this case also, an initial addition of acid will always accelerate
the washing process. It moreover appeared that, more especially in cases in
which simple coagulation, for example, by means of alcohol or a solution of salt,
is employed for the production of the cellulose object, the cellulose product did
not contain the metallic residue or residue of a metallic compound, in a suffi-
ciently soluble form, so that, according to the present invention, it is preferable, in
order to accelerate the washing process, to add some acid to the washing water
at least at the beginning and, according to circumstances, even also some of the
same salt by the solution of which the cellulose has been coagulated or precipi-
tated, for example, common salt. Acids, such as sulphuric acid, acetic acid
and the like, by way of example, fulfil the object of rendering the metallic
residue soluble. If a washing liquid of this kind be employed in the manner
described in the Specification of our said former application for Letters Patent,
it rapidly and thoroughly penetrates, by capillary action, the cellulose material,
so that only small quantities of washing acid are necessary. This acid employed
far washing only requires to be used in a very dilute state, without any risk of
an undesirable formation of basic salts being occasioned thereby, which is always
liable to take place when large quantities of water are employed.
In cases
Our improved process therefore shows itself to be very inexpensive. Any
traces of acid or salt solution that may have remained can be very easily and
rapidly removed from the cellulose material by using only small quantities of
clean water, by a washing operation carried out in a similar manner.
where acetic acid or any other volatile acid is employed, a further washing with
clean water can be dispensed with, since the remaining acetic acid evaporates
during the succeeding drying without chemically deteriorating the cellulose
articles.
D. YOUNG & Co.,
11 & 12, Southampton Buildings, London, W.C.,
Agents for the Applicants.
.
Improvements relating to the Washing of Cellulose Threads,
Films and the like.
We, Dr. Max FREMERY, Chemist, and JOHANNES URBAN, Engineer, both of
6, Dorfstrasse, Oberbruch, Reg. Bez. Aachen, in the German Empire, 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 follow-
ing statement:-
In the process described in the Specification of former Letters Patent, dated
28th March 1899, No. 6641, cellulose threads, films or the like are washed by
liquid which is caused to irrigate, successively and from above, the rollers or
spools on which the threads or films are wound, these rollers or spools being
supported one over the other. According to the above process, water is proposed
as the washing liquid for this purpose.
Experiments have now shown that in this process, it is important that the

page_text: washing liquid shall be prepared in such a manner that it separates or removes
the metal or the metallic compounds from their fixed combination with cellulose
and converts them into the form of a soluble salt or salts. The cellulose products
which are here considered, are prepared from cellulose solutions, for example,
fine silk-like threads. Cellulose solutions of this kind are produced by dissolving
cellulose in a suitable solvent, for example, in an ammoniacal solution of cupric
oxide, or a solution of chloride of zinc. From these solutions, cellulose threads,
for example, are obtained by conducting a fine jet of the solution through
chemicals which either decompose the solvent (such, for example, as acids), or
have themselves a coagulating action (such, for example, as alcohol, common salt
solution, and the like).
It has now been shown that, with the cellulose products so produced, a part of
the cellulose always remains in fixed combination with the particular metal or
the particular compound of the solvent.
According to the process described in the Specification of the aforesaid applica-
tion for Letters Patent, this metallic residue or residue of a metallic compound
which is scarcely removable by simple washing with water (even with large
quantities of water), is for the greater part removed, if the washing be effected
in the systematic manner indicated in the said specification.
In the above mentioned specification as before stated washing with water only is
referred to. This washing can however also be effected very easily in an analogous
manner with any liquid which is suitable for converting this metallic residue or
the residue of a metallic compound into the form of a soluble salt.
ever also in this case advantageous to irrigate the cellulose threads on the rollers
It is how-
or spools supported one over the other, in accordance with the process described
in the Specification of our said former Letters Patent, this being effected on the
counter current principle with the washing liquid and moreover to employ the
washing liquid in as dilute a condition as possible and in the smallest possible
quantity.
If an acid, for example, be employed as a precipitating or separating agent,
the residue of acid left behind in the cellulose objects, in the described method
of washing, may often suffice for dissolving out the combined residue of metal
or for decomposing the residue of the metallic compound and for removing the
same, so that, in this case, for the systematic washing, ordinary clean water
or distilled water can be used as washing water. In the researches, it however
appeared that, in this case also, an initial addition of acid will always accelerate
the washing process. It moreover appeared that, more especially in cases in
which simple coagulation, for example, by means of alcohol or a solution of salt,
is employed for the production of the cellulose object, the cellulose product did
not contain the metallic residue or residue of a metallic compound, in a suffi-
ciently soluble form so that, according to the present invention, it is preferable, in
order to accelerate the washing process, to add some acid to the washing water
at least at the beginning and, according to circumstances, even also some of the
same salt by the solution of which the cellulose has been coagulated or precipi-
tated, for example, common salt. Acids, such as sulphuric acid, acetic acid
and the like, by way of example, fulfil the object of rendering the metallic
residue soluble.
In practice, 1000 parts by weight of the washing water may contain, e.g., about
1 part by weight of acid; or 100 parts by weight of the washing water may con-
tain, e.g., about 5 parts by weight of salt. When both salt and acid are added
to the same washing water, the amounts of these additions may be such that
1000 parts by weight of the washing water may contain, e.g., about 1 part by
weight of acid and about 50 parts by weight of salt.
If a washing liquid of this kind be employed in the manner described in the
pecification of our said former Letters Patent, it rapidly and thoroughly pene-
rates, by capillary action, the cellulose material, so that only small quantities of
washing acid are necessary. This acid employed for washing only requires to be

page_text: used in a very dilute state, without any risk of an undesirable formation of basic
salts being occasioned thereby, which is always liable to take place when large
quantities of water are employed.
Any
In cases
Our improved process therefore shows itself to be very inexpensive.
traces of acid or salt solution that may have remained can be very easily and
rapidly removed from the cellulose material by using only small quantities of
clean water, by a washing operation carried out in a similar manner.
where acetic acid or any other volatile acid is employed, a further washing with
clean water can be dispensed with, since the remaining acetic acid evaporates
during the succeeding drying without chemically deteriorating the cellulose
articles.
Having now particularly described and ascertained the nature of our said
invention and in what manner the same is to be performed, we declare that what
we claim is:-
In the process claimed in the Specification of Letters Patent No. 6641 of 1899,
the use of salt water or acidified water for washing the cellulose products, and
thereafter, especially when using salt water or water containing a non-volatile
acid, washing with pure water, substantially as, and for the purposes described.
Dated this 20th day of T... 1000
c
D. YOUNG & Co.,
11 & 12, Southampton Buildings, London, W.C.,
Agents for the Applicants.