DIL T The Manufacture or Preparation of Improved Odorizing Substances for Artificially Imparting Odour to Gas.
Year: 1896

page_text: Date of Application, 6th July, 1896
Complete Specification Left, 17th Mar., 1897--Accepted, 8th May, 1897
PROVISIONAL ST BOIFICATION
SPECIF
PROVISIONAL SE DIL T
The Manufacture or Preparation of Improved Odorizing Substances
for Artificially Imparting Odour to Gas.
.
1, Dr. HUGO STRACHE. of 4, Pointengasse, Vienna XVII, in the Austrian
Empire, Lecturer at the K. K. Technischen Hochschule, do hereby declare the nature
of this invention to be as follows:-
Gases which, by themselves, are odourlesss or have no characteristic smell,
involve a certain danger in their use, if they have poisonous properties or are
injurious to health, or are capable of forming explosive gaseous mixtures with
atmospheric air, since, by reason of their lack of odour, escape or leakage of the
gas cannot easily be detected.
In this way, for example, the use of non-carburetted water-gas involves danger
of poisoning or explosion if an odour be not imparted to it artificially.
For making odourous (perfuming) water-gas or other gases, assafoetida or
mercaptan have heretofore been used. The smell of the first is not sufficiently
intense and characteristic, that of the other is certainly intense, yet on account of
the high price of mercaptan only a small quantity can be applied to the gas,
and the consequent dilution or weakening of the odour is so great that the
gas only possesses a weak leek-like odour which can be easily confused with other
odours.
An uncommon characteristic sinell, which cannot be mistaken for other smells, is
possessed by the carbylamines, for example, methyl-, ethyl-, phenyl-, tolyl-
carbylamine, etc., and these possess the advantage of being easily prepared and are
therefore cheap.
For producing the odourizing substance, it is not necessary to produce the
carbylamines in a pure condition, but it is sufficient to produce a substance
containing the particular carbylamine selected and to use this for perfuming the
gas. An odorizing substance of this kind is, according to the present invention
produced as follows:-
The amine to be employed, (for example, methylamine, ethylamine, aniline,
toluidine, etc.), is dissolved in alcohol, and then decomposed with an alkali (caustic
potash or caustic soda) and chloroform added thereto. After the reaction thus
produced is completed, the solution is absorbed by a porous material (such as
animal charcoal, pumice, wood-shavings, wood-wool, saw-dust, or the like) and
the gas to be perfumed is led over this substance in a suitable apparatus.
The alkali can also be dissolved in alcohol and the amine be added directly
afterwards; moreover the alcohol can be recovered after the completion of the
reaction, by distilling it off, if a carbylamine having a high boiling point be used.
Further, by using several amines, substances can be produced which contain several
carbylamines at the same time.
A practical method of preparing the odourizing material is the following:-On
the one hand about 30 grams of aniline are dissolved in 600 grams of alcohol, and
on the other hand, 100 grams of caustic soda are dissolved in 70 grams of water,

page_text: the two solutions are brought together and 45 grams of chloroform are cautiously
added thereto with stirring, the mixture is frequently shaken during one day, and
then allowed to settle. The solution of carbylamine so obtained can be used
directly for perfuming gases.
By the above mentioned process, a very dilute product is obtained, which only
contains a little over 3 per cent. of carbylamine. If it be desired to obtain a
concentrated product, which does not at the same time contain dissolved chloride
of sodium, and therefore can be vaporized without leaving behind any residue,
the following process is employed :-
Fine granular soda-lime has the calculated quantity of auiline poured over it, and
is heated to about 100°, and to the mixture, the calculated amount of chloroform
is added drop by drop with continual stirring. The reaction, which rapidly
sets in, does not proceed teo violently, if the chloroform be added cautiously
and in small quantities. The completion of the reaction can be determined from
the appearance of the substance, in which the chloride of sodium and chloride of
calcium produced form a coherent mass. After cooling, a part of the carbylamine
can be separated from the salt by decantation and can be used directly for
perfuming gas, whereby an effect can be obtained about thirty times more powerful
than by the use of the diluted product.
The part of the carbylamine clinging to the salt can be obtained by leaching
with the smallest practicable quantity of alcohol, allowing to settle, and pouring
off, and forms a less concentrated but still, however, always very strong product
(50 per cent. strength).
nonנית
11900
D. YOUNG & Co.,
11 & 12, Southampton Buildings, London, W.C.,
Agents for the Applicant.
The Manufacture or Preparation of Improved Odorizing Substances
for Artifically Imparting Odour to Gases.
I, Dr. HUGO STRACHE, of 4 Pointengasse, Vienna XVII, in the Austrian
Empire, Lecturer at the K. K. Technischen Hochschule, 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 :-
Gases which, by themselves, are odourless or have no characteristic smell, involve
a certain danger in their use, if they have poisonous properties or are injurious to
health, or are capable of forming explosive gaseous mixtures with atmospheric air,
since, by reason of their lack of odour, escape or leakage of the gas cannot easily
be detected.
In this way, for example, the use of non-carburetted water-gas involves danger
of poisoning or explosion if an odour be not imparted to it artifically.
For making odourous (perfuming) water-gas or other gases, assafoetida or
mercaptan have heretofore been used. The sinell of the first is not sufficiently
intense and characteristic, that of the other is certainly intense yet on account of
the high price of mercaptan only a small quantity can be applied or imparted to
the gas and the consequent dilution or weakening of the odour is so great that the
gas only possesses a weak leek-like odour which can be easily confused with other
odours.

page_text: An uncommon characteristic smell, which cannot be mistaken for other smells, is
possessed by the carbylamines, for example, methyl-, ethyl-, phenyl-, tolyl-
carbylamine, etc. and these possess the advantage of being easily prepared and are
therefore cheap.
For producing the odorizing substance, it is not necessary to produce the
carbylamines in a pure condition, but it is sufficient to produce a substance
containing the particular carbylamine selected and to use this for perfuming the
gas. An odorizing substance of this kind is, according to the present invention,
produced as follows:-
The amine to be employed, (for example, methylamine, ethylamine, aniline,
toluidine, etc.) is dissolved in alcohol, and then decomposed with an alkali (caustic
potash or caustic soda) and chloroform added thereto. After the reaction thus
produced is completed, the solution is absorbed by a porous material (such as
animal charcoal, pumice, wood-shavings, wood-wool, saw-dust, or the like) and the
gas to be perfumed is led over this substance in a suitable apparatus.
The alkali can also be dissolved in alcohol and the amine be added directly
afterwards; moreover the alcohol can be recovered after the completion of the
reaction, by distilling it off, if a carbylamine having a high boiling point be used.
Further, by using several amines, substances can be produced which contain several
carbylamines at the same time.
A practical method of preparing the odorizing material is the following:-On
the one hand about 30 grams of aniline are dissolved in 600 grams of alcohol, and
on the other hand, 100 grams of caustic soda are dissolved in 70 grams of water,
the two solutions are brought together and 45 grams of chloroform are cautiously
added thereto with stirring; the mixture is frequently shaken during one day, and
then allowed to settle. The solution of carbylamine so obtained can be used
directly for perfuming gases.
By the above mentioned process, a very dilute product is obtained, which only
contains a little over 3 per cent. of carbylamine. If it be desired to obtain a
concentrated product, which does not at the same time contain dissolved chloride of
sodium, and therefore can be vaporized without leaving behind any residue, the
following process is employed :-
Fine granular soda lime has the calculated quantity of aniline poured over it,
and is heated to about 100° Celcius, and to the mixture, the calculated amount of
chloroform is added drop by drop with continual stirring. The reaction, which
rapidly sets in, does not proceed too violently, if the chloroform be added
cautiously and in small quantities. The completion of the reaction can be
determined from the appearance of the substance, in which the chloride of sodium
and chloride of calcium produced form a coherent mass. After cooling, a part of
the carbylamine can be separated from the salt by decantation and can be used
directly for perfuming gas, whereby an effect can be obtained about thirty times
more powerful than by the use of the diluted product.
The part of the carbylamine clinging to the salt can be obtained by leaching
with the smallest practicable quantity of alcohol, allowing to settle, and pouring
off, and forms a less concentrated but still, however, always very strong product
(50 per cent. strength).
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 :-
1. The odorization of gases by means of a material containing one or more
carbylamines, or by means of one or more carbylamines alone.
2. A process for the manufacture of an odorizing material such as is hereinbefore
described, wherein the fluid resulting from mixing one or more amines with alcohol,
alkali and chloroform and if desired recovering the alcohol, is used to saturate
porous materials, such as animal charcoal, pumice, wood-shavings, wood-wool,
saw-dust or the like, substantially as, and for the purposes, herein before described.

page_text: 3. The manufacture of concentrated carbylamine by the action of soda lime on
aniline and chloroform without employing a solvent, substantially as hereinbefore
-described.
Deted the 17th dor of March 1807
D. YOUNG & Co.,
11 & 12 Southampton Buildings, London, W.C.,
Agents for the Applicant.