Improvements in the Manufacture of Colouring Matters.
Year: 1890

page_text: Date of Application, 3rd Feb., 1890
Complete Specification Left, 1st Nov., 1890-Accepted, 6th Dec., 1890
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I, ROBERT HOLLIDAY of the firm of Read Holliday & Sons, of Huddersfield, in the
County of York, Manufacturing Chemist do hereby declare the nature of this invention
to be as follows:-
This invention relates to the treatment of thio-paratoluidine in order to obtain new
sulphonic acid preparations thereof and the use of their diazo compounds combined
or admixed with phenols or their sulphonic acid derivatives or preparations.
One part of the thio-paratoluidine is added to from (say) 3 to 4 parts of fuming
sulphuric acid (containing say 30 per cent. of anhydride) until a sample taken out of
the mixture dissolves to a clear solution in water. Heat may also be applied by
means of a hot water steam jacket or other suitable means to hasten the solution of
the thio base.
Some of the properties of this new sulphonic acid are that it differs from the
sulphonic acids of thio-paratoluidine base previously described by being entirely
soluble in water, while the other acids are insoluble to a great extent.
When these new sulphonic acid preparations are dyed on the fibre and afterwards
diazotised and brought into an alkaline solution of beta raphthol much yellower
shades are produced on the fibre than is the case with those preparations of thio-
paratoluidine, previously known when similarly treated.
This new sulphonic acid can be used for combining its diazo compound with phenols
and their sulphonic acid derivatives.
Dated the 3rd day of February 1890
WM. BROOKES & SON,
55 & 56, Chancery Lane, London, Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Colouring Matters.
I ROBERT HOLLIDAY of the firm of Read Holliday & Sons, of Huddersfield, in the
County of York, Manufacturing Chemist 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 thio-paratoluidine in order to obtain new
sulphonic acid preparations thereof, and the use of their diazo compounds combined
or admixed with phenoles or their sulphonic acid derivatives or preparations.
By thio-paratoluidine, I mean especially the product which is formed when 3 parts
of sulphur are heated with 4 parts by weight of para-toluidine at a temperature
of 200-250° C. for twelve hours, and from which the dehydrothio-toluidine has been
removed by treatment with hot dilute hydrochloric acid.
One part of thio-paratoluidine is added to from (say) 3 to 4 parts of fuming
sulphuric acid (containing 30% anhydride) and agitated together, until a sample
taken out of the mixture dissolves to a clear solution in water.
Heat may also be applied by means of a hot water, or steam jacket, or by other
suitable means to hasten the solution of the thio-base.
Some of the properties of this new sulphonic acid are that it differs from the
sulphonic acids of thio-paratoluidine base previously described by being entirely
soluble in water, while the other acids are insoluble to a great extent.
When these new sulphonic acid preparations are dyed on the fibre and afterwards
diazolised and brought into an alkaline solution of ẞ naphthol much yellower shades

page_text: are produced than is the case with those preparations of thio-paratoluidine previously
known when similarly treated.
This new sulphonic acid can be used for combining its diazo-compound with phenoles,
and their sulphonic acid derivatives.
As an example of the use of this new sulphonic acid for combining with phenoles,
I take 20 lbs of thio-paratoluidine, and add it by degrees to from 60-80 lbs. fuming
sulphuric acid (30% anhydride) stirring the whole time, until a sample taken from
the mixture dissolves to a clear solution in cold water.
The sulphonation can be promoted by heat applied to the outside of the operating
pan.
The liquid sulphonate is then poured on ice or into waters, and can then be salted
out, or diazotised direct.
In the latter case I add to the aqueous solution of the sulphonate thus prepared,
5 (five) lbs. of nitrite of soda dissolved in water; the nitrite solution being slowly
added accompanied by stirring.
When the sulphonate has been diazotised it is run into a solution of 5 (five) pounds
of ẞ naphthol dissolved in caustic soda, sufficient soda being added to keep the mixture
alkaline.
The solution which contains the colouring matter is boiled, filtered, and the colour
salted out, pressed and dried.
Other phenoles such as a naphthol, carbolic acid, resorcine, oxy-naphtholic acid,
salicylic acid or their sulphonic acid derivatives can be substituted for the ẞ naphthol
in the above example.
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
Improvements in the manufacture of colouring matters by combining the diazo
compounds of the new sulphonic acid of thio-paratoluidine with phenoles or their
sulphonic acid derivatives, substantially as herein described.
Dated the 31st day of October 1800.
WM. BROOKES & SON,
55 & 56, Chancery Lane, London, Agents for the Applicant.