Improvements relating to the Dyeing or Printing of Woollen and other Goods.
Year: 1891

page_text: Date of Application, 7th Oct., 1391
•
Complete Specification Left, 28th Apr., 1892-Accepted, 16th July, 1892 :
PROVISIONAL SPECIFICATION.
[Communicated. from abroad by K. OEHLER, of Offenbach */m, in the Grand.Dachy
of. Hessen, in the Empire of Germany.]
Improvements relating to the Dyeing or Printing of Woollen and
other Goods.
I, HENRY HARRIS LAKE of the firm of Haseltine Lake & Co., Patent Agents,
45 Southampton Buildings in the County of Middlesex, do hereby declare the
nature of this invention to be as follows :-.
All the trials which have been made for the purpose of obtaining an aniline
black on wool either by dyeing or printing have heretofore been unsuccessful.
These failures are attributed to the reducing qualities of the wool which do not
allow the formation of an aniline black, this process being based upon oxydation..
By treating wool with oxydizing agents however such as chlorine and hydrogen-
dioxyde, and the like the wool fibre will fix the aniline black in a manner similar to
cotton fibre
The dyeing or printing of aniline black on wool is performed as follows:-
The prepared wool is padded or printed with the composition, generally used for
producing aniline black on cotton that is to say, either an oxydising black or a
steam black. The former is developed in the ordinary way, the latter by steaming;
the steam black is to be preferred on account of its easy working and because it
does not turn green. The dyeing can be performed in a bath which contains an
aniline salt or toluidine salt or a mixture of both and substances fit for oxydation.
The treatment of the wool with chlorine as well as the production of aniline
black on cotton are well known; it is also known that for printing wool, the latter
previously prepared by various combinations of tin, is treated with chlorine in order
to obtain more intensity and brightness of the shade. The treating of the wool
by chlorine has been recommended to facilitate the fixing of acid colours.
(Oesterreich's Wollen und Leinen Industrie 1889 No. 8 page 340. Method of
Dyeing Naphtol Black on Wool by Leop, Cassella & Co.)
The various methods of fixing aniline black on cotton are also common property;
but the combination of both methods in order to produce aniline black on wool is
quite new, as well as the fact that the same effect which was supposed to be only
obtainable by treating wool. with chlorine, can also be obtained by using other:
oxydising agents such as hydrogen-dioxyde and the like.

page_text: black; too great an extent of concentration and steaming however will produce an
inferior brownish black.
The treatment of the wool with chlorine may also be performed in the following
manner:
Sulphuric acid or any other acid having a similar effect, and hypochlorite of lime
are brought together in the same bath.
The oxydising by means of hydrogen dioxyde requires a concentrated solution
(previously neutralized with ammonia to a slight alkaline reaction) and a temperature
of about 30° C.
The oxydation black requires an aniline black with coppersalts or vanadate.
After padding the black is developed by oxydation at about 33-36° C. or more
(or by slightly steaming and then passed through a bichrome bath..
The dyeing in the usual way is performed in a cold bath containing,
1.. A solution of aniline or toluidine salt or a mixture of both.
2: Free chromic acid either alone or combined with other oxydising agents such
as coppersalts.
The previously oxydised wool is for some time manipulated in this cold bath and
the latter is then gradually brought to the boiling point.
It is evident that for printing purposes the addition of a thickening to the aniline
black mixture for padding black is required. The above described method can
also be applied to mixed goods viz. half wool and half cotton, half wool and half
silk, or half wool and half linen.
.
Dated this 7th day of October 1891.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements relating to the Dyeing or Printing of Woollen and
other Goods.
·I, HENRY HARRIS LAKE of the firm of Haseltine Lake & Co. Patent Agents,
45 Southampton Buildings, in the County of Middlesex 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 :-
In my Provisional Specification I have described the production of aniline black
on wool by dyeing in a single bath and the developing of the black on padded or
printed goods in the oxidizing chamber. I have found that this part of my process
has already been known and I therefore desire to confine my invention to the
production of aniline black by padding and printing and developing by steaming.
The goods are first oxidized in a proper manner and then heated by a process
similar to that producing steam aniline black ou cotton.
I am well aware that John Lightfoot has stated in the Specification of his English
Patent No. 2327 of 1865 that it was necessary to paralyse the reducing_quality of
wool by oxidation to render it fit for the production of aniline black. His process
differs essentially from mine by his method of dyeing and printing and therefore
yields other results...
Lightfoot oxidizes the wool to its maximum by treating with different oxidizing
agents, using by preference chlorine mixtures; for instance, 12% of hypochlorite
of lime (chemick or chlorine) 15-6 % muriatic acid by weight of the dyeing goods
and treating at a temperature of 100° F. until the wool is quite yellow. When
the oxidation is finished the said Lightfoot dyes according to the process described
in his Patent No. 151 of 1863 riz. he takes a solution containing chlorate of potash,
equal quantities of aniline and muriatic acid, further acetic acid, perchloride of
copper, sol ammoninc or other alkaline chloride; the goods are steeped in this

page_text: solution, dried, aged for two nights and then passed through water or a weak
solution of alkaline or metallic salts.
:
Mixed fabrics are steeped in a mixture of aniline salt, chlorate of potash, sal
ammoniac and sulphate of copper and are further treated as above described.
Printed fabrics must pass through a solution of hyposulphite or sulphite of soda to
restore the white destroyed by the chlorage.
The improved process is as follows:-
The goods are well washed and treated whilst still moist, at the ordinary
temperature for to 1 hour in a bath containing about 6% of hypochlorite of lime
for printing, and 10% for a uniform black and about 9 to 15% muriatic acid of
34° Tw. (by the weight of the goods). By this feeble treatment the white of the
wool is but little affected.
After this oxidation the goods are well washed, dried and padded or printed with
a mixture suitable for producing steam aniline black on cotton.
40 "
11 tartaric acid.
By the term "leiogomme" is to be understood a kind of dextrine obtained by
simply roasting potato starch. It is well known as a means for thickering dissolved
or liquid dyes.
The fabrics padded or printed are dried and steamed for some minutes to of
an hour or more, washed and if necessary soaped or passed through a weak acid
bath.
I do not confine myself to the use of chlorate of soda, as equivalent quantities of
the salts of potassium, ammonium, or barium will serve as well; also the yellow
prussiate of potash (or of soda or ammonium) can be replaced by the red prussiate
or by a mixture of both and the chlorhydrate of aniline or toluidine by the
nitrates.
-
The concentration of the padding solution or of the printing colour can be
changed according to the intensity of the black desired. The proportion of the
aniline salt to the oxidizing agents and that of the glycerine or sugar and tartaric
acid may also be changed.
Although I prefer the process in which the mixture of hypochlorite of lime and
muriatic acid, is used I may moreover use the following modifications:
Muriatic acid and hypochlorite of lime separately, cold or warm at 176° F.
Sulphuric acid and hypochlorite of lime separately or mixed in a bath cold or
warm at 176° F.
Cold watery solution of chlore. Mixtures developing hypochlorous acid instead
of chlore, for instance the hypochlorite of lime and acetic acid, rendering the wool
very yellow and can only be used for uni goods. Besides the hypochlorite of lime
other hypochlorites and other oxidizing agents may be used for instance permanganate

page_text: of potash, mixtures of chromic acid and hydrogen dioxide. I prefer: the latter
however using it at a temperature of 86° F. in a concentrated solution. of
about 3% and neutralized with ammonia until it gives a slight alkaline reaction.
In the Lightfoot process the following inconveniences have to be contended with,
mis. :-
1. Complicated machinery is necessary for the production of a uniform. (plain)
black which nevertheless becomes uneven.
2. By the maximum oxidation the wool becomes yellow in so high a degree that
the simultaneous use of other colours is impossible, as they would not stand the
sulphurizing which has to follow.
3. Chemically considered Lightfoot's black is an emeraldine, which can be trans-
formed into nigraniline which does not turn green, only on uni dyed goods as
associated colours would be destroyed by the oxidizing agents such as chromates.
4. Even if the said inconveniences did not exist, the process would be still a very
complicated one; the black must first be developed in the oxidizing chamber,
then passed through gaseous ammonia and finally the associated colours are fixed by
steaming.
According to the improved process the developing of the black goes on more
rapidly and quite even and only simple steaming apparatus is required.
The improved method allows the association of other colours as the wool remains
white and no sulphurizing is required. The said process yields directly black which
does not turn green, of a higher degree of oxidation and contains Prussian blue
moreover a small quantity of mauvéine is formed.
;
The said process further allows of the fixing of the black and the other colours
together by one steaming operation.
As a proof that Lightfoot's process was of no practical value .I may mention
that until now, no aniline black on wool is to be found in the trade.
The improved process compared with Lightfoot's is not only more simple and
gives better results but it also yields a new technical effect.
Moreover in the Patent of Lightfoot there are other indications in the literature
treating of aniline black on wool, for instance J. J. Hummel: The dyeing of textile
fabrics 1885 p. 396 Jean Henri Chaudet: French Patents No. 190,280 and No.
200,061, but nowhere is the production of steam aniline black.spoken. of and I there-
fore may consider my process new.
Having now particularly described and ascertained the nature of the said inven-
tion and in what manner the same is to be performed as .communicated to me
by my foreign correspondent, I declare that what I claim is :-
The method of producing aniline black on wool or mixed fabrics containing
wool consisting in first oxidizing the goods and then padding or printing with a
mixture suitable for producing steam aniline black on cotton and finally developing
the black and fixing other colours by steaming substantially as set forth.
Dated this 28th day of April 1892.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, Agents for the Applicant.