Improvements in the Manufacture of Aniline Lakes suitable for the Manufacture of India Rubber Cloth and other purposes.
Year: 1891

page_text: Date of Application, 30th Sept., 1891
Complete Specification Left, 30th June, 1892-Accepted, 13th Aug., 1892
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Aniline Lakes suitable for the
Manufacture of India Rubber Cloth and other purposes.
I ISIDOR FRANKENBURG of Greengate Rubber Works Salford in the County of
Lancaster India Rubber Manufacturer, do hereby declare the nature of this inven-
tion to be as follows
:-
Colours suitable for dyeing india rubber cloth for waterproof garments and other
articles must answer the following requirements.
1. The colour must not be affected by water.
2. The colour must not be affected by acids.
3. The colour must not be affected by alkalies.
4. The colour must not be affected by heat.
5. The colour must not run with any of the solvents used in the course of manu-
facturing india rubber waterproofing and other articles.
6. The colour must be capable of being easily reduced to a state of extremely
fine sub-division or solution in any of the solvents used for india rubber.
In the following way I have succeeded in preparing aniline lakes answering all
these requirements.
(A)-Lakes prepared from acid aniline colours: The aniline colour is dissolved
in hot water and a solution of soda carbonate or bicarbonate (commercial) added,
this solution is quantitatively precipitated by adding to it a solution of barium
chloride when the lake is obtained in the form of a heavy precipitate.
This colour answers the above requirements 1 to 5, but not 6; and is of a very
dull appearance. In order to complete the process as regards the two last points
the lake is heated to boiling point and kept at that temperature for about half an
hour. It is then treated with a solution of sulphate of alumina, alum, sulphate of
magnesia, chloride of alumina, or chloride of magnesia, sulphate of zinc or chloride
of zinc, when at once the colour begins to brighten and to be converted into a lake
of extremely fine structure, answering the above requirements in every respect.
The following proportions have been found to give satisfactory results :-

page_text: added for the finish. The croceines especially give good results with this method.
Suitable proportions are :—
(3)
100 lbs. sulphate alumina
50 lbs. croceine 2 B
120 lbs. barium chloride
45 lbs. soda carbonate.
(4)
112 lbs. sulphate of magnesia
50 lbs. croceine 3 B
120 lbs. barium chloride
42 lbs. soda carbonate.
The colours produced by this method are however rather inferior to those obtained
by the first process.
(B)-Lakes prepared from basic aniline colours. The base is prepared by
precipitating a solution of sulphate of alumina with soda carbonate and chloride of
barium.
To the white precipitate thus obtained the solution of the aniline colour is added,
a solution of tannic acid serving as precipitant. The mixture is then boiled and the
precipitation is made complete and the colour fastened by adding a solution of soda
acctate. The following proportions give good results :—
GEO. DAVIES & SON,
4, St. Ann's Square, Manchester, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Aniline Lakes suitable for the
Manufacture of India Rubber Cloth and other purposes.
I ISIDOR FRANKENBURG of Greengate Rubber Works Salford in the County of
Lancaster India Rubber Manufacturer, do hereby declare the nature of this inven-
tion and in what manner the same is to be performed to be particularly described and
ascertained in and by the following statement :-
Colours suitable for dyeing india rubber waterproof cloth and for dyeing rubber
in the bulk generally must answer the following requirements :-
1. The colours must not be affected by or run with water.
2. The colours must not be affected by acids.
3. The colours must not be affected by alkalies..
4. The colours must not be affected by chloride of sulphur.

page_text: 5. The colours must not be affected by sulphur at temperatures ranging from 200°
to 300° Fahrenheit.
6. The colours must not run with any of the solvents used in the manufacture
of india rubber waterproofings or other india rubber articles.
7. The colours must not be affected by heat of such temperatures as are
employed in the manufacture of india rubber waterproof and other articles.
8. The colours must be capable of extremely fine sub-division, diffusion, or
solution in any of the solvents used for india rubber.
According to my invention aniline lakes answering all these requirements can be
prepared as follows:-
(A). Lakes prepared from acid aniline colours. I have found that by converting
any of the acid or sulphonated aniline colours into compound lakes, such as barium-
alumina calcium-alumina, barium-chromium or calcium-chromium lakes, colours are
obtained answering all the above requirements and therefore eminently suitable for
the dyeing of india rubber waterproof and other articles. The aniline dyes best
suited for the production of these lakes are those known as azo- or dis-azo-colours.
From colours of this description I prepare lakes in the following manner:
.30 lbs. of orange II, or any other suitable azo- or dis-azo-colour, and 112 lbs. of
soda crystals are dissolved in 100 gallons of water at 170 degrees Fahrenheit.
This solution is then precipitated with a solution of 150 lbs. of barium chloride.
The precipitate is kept boiling for half an hour. It is then left to stand and
washed several times with fresh water. Eventually a solution of 40 lbs. of alumina.
sulphate is added very gradually, when a bright fast and flocculent lake is obtained,
which after filtration drying and pulverizing is ready for incorporation with the
india-rubber dough.
It is evident that a great many variations of the process may be devised, but in
every case the important point is the conversion of the aniline dye into one of the
above mentioned compound lakes: As regards the proportions given above, they
are of course subject to such variations as are in accordance with the molecular
weights and the commercial purity of the materials used, as well as with the
particular properties and qualities to be imparted to the lakes for the purpose they
are intended to serve.
Using in this manner the numerous azo- and dis-azo-dyes a very great variety of
lakes may be produced, comprising all conceivable shades and all suitable for the
dyeing of india rubber articles of every description. The lakes prepared from the
acid oxy-ketone dyes and most of the natural dyes are very little suitable for this
purpose, owing to their indifferent and dull shades.
(B). Lakes prepared from basic colouring matters. A large number of lakes
derived from this class of dyes are also suited for the dyeing of india rubber
articles, although many of them are lacking in fastness to light acids and alkalies.
To produce a perfect compound lake from these dyes tannic acid and antimony,
along with aluminium and barium, are used for the complete fixation and precipitation
of these lakes.
The following proportions give good results :-
128 lbs. soda carbonate
110 lbs. barium chloride
25 lbs. thioflavine
20 lbs. tannic acid
20 lbs. acetate of soda
100 lbs. sulphate of alumina.
These colours can be made faster by adding to them a small quantity of antimony
notassio-tartrate

page_text: due to the difference in the atomic weights and commercial purity of the
basic dyes.
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 :-
The manufacture of compound lake pigments in the manner above described
for the purpose of dyeing india rubber waterproof goods and all other india
rubber and similar articles and especially I claim
First. The preparation of compound aniline lakes, for the dyeing of india
rubber articles of every description by the incorporation of alumina hydrate with
barium sulphate and the lake by adding to the barium carbonate lake the alumina
sulphate, whereby both the barium sulphate and alumina hydrate meet in "statu
nascendi" thus forming a lake body eminently capable of completely diffusing through
india rubber dough and similar mixtures.
Secondly. The formation as above described of a not only physically but also
chemically perfect lake, all affinities of which are fully saturated, so that the com-
pounds used with rubber mixtures and the hot or cold vulcanizing of the rubber
can not exert any chemical action upon the incorporated pigments.
Thirdly. The use of the compound lake pigments of the above described com-
position for the incorporation with and dyeing of india rubber mixtures, suitable for
the production of india rubber waterproof and other articles.
Dated this 29th day of June 1892.
GEO. DAVIES & SON,.
4, St. Ann's Square, Manchester, Agents for the Applicant.