Year: 1897

page_text: Date of Application, 13th May, 1897
Complete Specification Left, 31st Jan., 1898-Accepted, 9th Apr., 1898
I, OLIVER IMRAY, of No. 28, Southampton Buildings, Chancery Lane, in the
County of London, Chartered Patent Agent, do hereby declare the nature of this
invention (as communicated to me from abroad by The Farbwerke vormals:
Meister Lucius and Brüning, of Hoechst a/Main, in the Empire of Germany,
Chemical Manufacturers) to be as follows:-
Knecht and Milnes published in the Journal of the Society of Chemical Industry
1892 p. 131 the results which they obtained by the action of chlorine upon wool.
By repeating these experiments my foreign correspondents have found their state-
ments to be correct. If, for instance, moistened wool be put into a vessel and an
excess of chlorine passed over it, a violent reaction takes place, the chlorine is
absorbed by the wool with a considerable evolution of heat, and the wool soon
changes into a white pulpy substance, whilst large quantities of hydrochloric acid
are generated. The reaction takes place less violently, yet with the same result by
a prolonged process, if the wool be treated in a state of dryness, that is to say, with
only its natural moisture with an excess of chlorine.
The effect, however, is found to be quite different if the wool be treated not in
an excess, but in a measured quantity of chlorine, either in a vessel containing a
known quantity of chlorine, or by letting a known quantity of chlorine act upon
wool in a closed vessel filled with air.
In these cases the chlorine is likewise absorbed by the wool, whilst evolving
hydrochloric acid and heat, and this the more rapidly the more moist the wool is,
and the more slowly, the drier it is; but the wool remains intact and only acquires
those qualities hitherto given to it by treatment with solutions of bleaching powder
or sodium hypochlorite, namely; increased power of absorbing dyestuffs of all kinds,
increase in transparency of the fibre, in gloss and cracking feel, in power of retain-
ing a silk-like, appearance and cracking feel by a subsequent treatment of soap
solutions and acids, loss of the capability of being padded and felted, all this with-
out assuming a yellow tint, on the contrary, the wool by the treatment with chlorine
becomes rather whiter than before, being bleached at the same time.
These observations form the base of the present invention relating to the chlorina-
tion of wool.
The wool is treated with a certain quantity of chlorine, either by introducing it
into a vessel already containing chlorine in a pure state or diluted with air, or in a
suitable vessel filled with air into which is introduced the requisite quantity of
chlorine.
The damper the wool, the more quickly is the chlorine absorbed and the drier the
state in which it comes in contact with the chlorine, the more slowly is it absorbed.
On the other hand, the concentration of the chlorine, or the degree of dilution with
air in which it is employed, influences the readiness of absorption, the more diluted
the chlorine, the slower is the absorption, the less air introduced, the more quickly
is the chlorine absorbed.

page_text: :
By these means the process of chlorination can be regulated in such a manner as
to attain the greatest uniformity in the change of the wool fibre, the effect of
chlorination being quite regular so that, on subsequent dyeing, no inequalities
appear caused by uneven chlorination. This constitutes a great technical improve-
ment over the method now employed for chlorinating with acidulated solutions of
bleaching powder or sodium hypochlorite. A further technical advance is found
in the circumstance above mentioned that the wool remains white and does not
acquire a yellow tint, as is the case when other methods are employed.
Not only white wool, but also dyed wool can be chlorinated with advantage, as
a great many dyestuffs fixed on the fibre, resist this treatment.
25 litres of chlorine of normal pressure to every kilo. of wool are to be considered
as the utmost limit without danger to the fibre, whilst 5 litres per kilo. of wool is
the lowest.
The speciality of this method depends on the property of wool absorbing chlorine
in a moist state much more rapidly than in a dry state.
If woollen cloths or textures be printed with a slightly thickened solution of a
strong hygroscopic body, such, for instance, as chloride of calcium or magnesium,
or chloride of zinc, and if chlorine be subsequently allowed to act upon these pre-
viously treated goods, only the parts printed upon will, under appropriate working
conditions, be chlorinated; goods are thus obtained shewing the effect of chlorina-
tion in varied designs. In a similar way, this local effect may also be obtained by
printing certain parts with the solution of a substance which is difficult to wet
after drying or steaming, for instance aluminium acetate. If the goods, thus
previously prepared, are moistened, then the printed places absorb no moisture and
the effect of chlorination is obtained by subsequent treatment with chlorine only on
the parts of the material not printed, the previous printing acting as resisting the
chlorination.
The carrying out of the chlorination depends upon the material to be treated.
It is advisable, for piece goods and yarns, to use appliances permitting continual
movement of the goods during the chlorination in order to obtain the requisite
uniformity.
The method of working is illustrated by the following example:-
PRODUCTION OF SILK GLOSS ON 35 KILOS OF WOOLLEN KNITTING-YARN.
The previously cleansed and equally whizzed yarn is introduced into the
chlorination compartment in a moist state. This compartment is completely lined
with sheet-lead and has a capacity of about 25 cubic metres and a double bottom,
below which the supply pipe for chlorine enters; in the cover there is a ventilator
which can be connected with a chimney having a good draught, a pump or an
exhauster. In one of the sides a door is fitted which allows the introduction of the
goods and can be hermetically closed by suitable means. The yarn is placed upon
spools, covered with cloth fast to chlorine; the spools are moved from outside and
are constructed so as to cause the yarn to continually change its place. 500 litres
of chlorine at a normal pressure are then slowly introduced during half an hour;
after another half hour the exhauster is put in action at the ventilator, the process
of chlorination being ended, till the residue of chlorine not absorbed is removed,
which requires only half an hour.
opened and the yarn is taken out.
chloric acid thus formed, and by the
hydroextraction acidulation with
cracking feel is obtained.
Dated this 19th
JJ
The exhauster is then stopped, the door is
It is thoroughly washed to remove the hydro-
usual subsequent treatment with soap solution,
hydrochloric acid, rinsing and drying, the
1007
ABEL & IMRAY,
Agents for the Applicant..

page_text: I, OLIVER IMRAY, of Birkbeck Bank Chambers, Southampton Buildings,
Chancery Lane, in the County of London, Chartered Patent Agent, do hereby
declare the nature of this invention (as communicated to me from abroad by The
Farbwerke vormals: Meister Lucius and Brüning, of Hoechst */Main, in the
Empire of Germany, Chemical Manufacturers) and in what manner the same is to
be performed, to be particularly described and ascertained in and by the following
statement:-
Knecht and Milnes published in the Journal of the Society of Chemical Industry
1892 p. 131 the results which they obtained by the action of chlorine upon wool.
By repeating these experiments my foreign correspondents have found their state-
ments to be correct. If, for instance, moistened wool be put into a vessel and an
excess of chlorine passed over it, a violent reaction takes place, the chlorine is
absorbed by the wool with a considerable evolution of heat, and the wool soon
changes into a white pulpy substance, whilst large quantities of hydrochloric acid
are generated. The reaction takes place less violently, yet with the same result by
a prolonged process, if the wool be treated in a state of dryness, that is to say, with
only its natural moisture with an excess of chlorine.
The effect, however, is found to be quite different if the wool be treated not in
an excess, but in a measured quantity of chlorine, either in a vessel containing a
known quantity of chlorine, or by letting a known quantity of chlorine act upon
wool in a closed vessel filled with air.
In these cases the chlorine is likewise absorbed by the wool, whilst evolving
hydrochloric acid and heat, and this the more rapidly the more moist the wool is,
and the more slowly, the drier it is; but the wool remains intact except that it acquires
those qualities hitherto given to it by treatment with solutions of bleaching powder
or sodium hypochlorite, namely; increased power of absorbing dyestuffs of all kinds,
increase in transparency of the fibre, in gloss and cracking feel, in power of retain-
ing a silk-like appearance and cracking feel by a subsequent treatment of soap
solutions and acids, loss of the capability of being padded and felted, all this with-
out assuming a yellow tint, on the contrary, the wool by the treatment with chlorine
becomes rather whiter than before, being bleached at the same time.
These observations form the base of the present invention relating to the chlorina-
tion of wool.
The wool is treated with a certain quantity of chlorine, either by introducing it
into a vessel already containing chlorine in a pure state or diluted with air, or in a
suitable vessel filled with air into which is introduced the requisite quantity of
chlorine.
The damper the wool, the more quickly is the chlorine absorbed and the drier the
state in which it comes in contact with the chlorine, the more slowly is it absorbed.
On the other hand, the concentration of the chlorine, or the degree of dilution with
air in which it is employed, influences the readiness of absorption, the more diluted
the chlorine, the slower is the absorption, the less air introduced, the more quickly
is the chlorine absorbed.
By these means the process of chlorination can be regulated in such a manner as
to attain the greatest uniformity in the change of the wool fibre, the effect of

page_text: chlorination being quite regular so that, on subsequent dyeing, no inequalities
appear caused by uneven chlorination. This constitutes a great technical improve-
ment over the method now employed for chlorinating with acidulated solutions of
bleaching powder or sodium hypochlorite. A further technical advance is found
in the circumstance above mentioned that the wool remains white and does not
acquire a yellow tint, as is the case when other methods are employed.
Not only white wool, but also dyed wool can be chlorinated with advantage, as
a great many dyestuffs fixed on the fibre, resist this treatment.
25 litres of chlorine of normal pressure to every kilo. of wool are to be considered
as the utmost limit without danger to the fibre, whilst 5 litres per kilo. of wool is
the lowest.
The speciality of this method depends on the property of wool of absorbing
chlorine in a moist state much more rapidly than in a dry state.
If woollen cloths or textures be printed with a slightly thickened solution of a
strongly hygroscopic body, such, for instance, as chloride of calcium or magnesium,
or chloride of zinc, and if chlorine be subsequently allowed to act upon these pre-
viously treated goods, only the parts printed upon will, under appropriate working
conditions, be chlorinated; goods are thus obtained shewing the effect of chlorina-
tion in varied designs. In a similar way, this local effect may also be obtained by
printing certain parts with the solution of a substance which it is difficult to wet
after drying or steaming, for instance aluminium acetate. If the goods, thus
previously prepared, are moistened, then the printed places absorb no moisture and
the effect of chlorination is obtained by subsequent treatinent with chlorine only on
the parts of the material not printed, the previous printing acting as resisting the
chlorination.
The carrying out of the chlorination depends upon the material to be treated.
It is advisable, for piece goods and yarns, to use appliances permitting continual
movement of the goods during the chlorination in order to obtain the requisite
uniformity.
".
The method of working is illustrated by the following example:
PRODUCTION OF SILK GLOSS ON 35 KILOS OF WOOLLEN KNITTING-YARN.
The previously cleansed and equally whizzed yarn is introduced into the
chlorination compartment in a moist state. This compartment is completely lined
with sheet-lead and has a capacity of about 25 cubic metres and a double bottom,
below which the supply pipe for chlorine enters; in the cover there is a ventilator
which can be connected with a chimney having a good draught, a pump or an
exhauster: In one of the sides a' door is fitted which allows the introduction of the
goods and can be hermetically closed by suitable means. The yarn is placed upon
spools, covered with cloth fast to chlorine; the spools are moved from outside and
are constructed so as to cause the yarn to continually change its place. 500 litres
of chlorine at a normal pressure are then slowly introduced during half an hour;
after another half hour the exhauster is put in action at the ventilator, the process
of chlorination being ended, till the residue of chlorine not absorbed is removed,
which requires only half an hour. The exhauster is then stopped, the door is
opened and the yarn is taken out. It is thoroughly washed to remove the hydro-
chloric acid thus formed, and by the usual subsequent treatment with soap solution,
hydroextraction, acidulation with hydrochloric acid, rinsing and drying, the
cracking feel is obtained.
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. Chlorinating wool by treating it loose, spun or woven, dry or moist, with
chlorine or chlorine mixed with air, in quantity not exceeding 25 litres of chlorine
for 1 kilogram of wool substantially as described.
2. Chlorinating dry "woollen goods, previously printed with the solution of a

page_text: hygroscopic body or moist woollen goods previously printed with the solution of a
substance which it is difficult to wet after drying, substantially as and for the
purposes set forth.