Improvements in Pyroxyline Compounds, Solutions, and Solvents.
Year: 1893

page_text: Date of Application, 18th Nov., 1893
Complete Specification Left, 29th Nov., 1893-Accepted,
27th
Jan., 1894
PROVISIONAL SPECIFICATION.
Improvements in Pyroxyline Compounds, Solutions, and Solvents.
I, LEONARD PAGET, of 300 Fourth Avenue, New York City, United States
of America, do hereby declare the nature of this invention to be as follows:-
The object of my invention is, first, to improve in solvent power those weak
solvents of soluble nitro-cellulose or pyroxyline that are otherwise, from their
characteristic volatility and other properties, useful in the art, but which are too
weak in solvent power to become usefully employed in their normal condition :
secondly, to impart solvent power to menstrua otherwise non-solvent without
addition to their volume or bulk or without material change in their practical
properties; thirdly, to render certain solvent essential oils that are impaired in
their utility in the art by reason of their fixed or non-volatile character, more
easily drying or siccative; fourthly, to determine in those camphoraccous oils and
balsams such development of the so-called camphor as may bring about, in con-
junction with alcohol, fusel oil, and other inactive solvents, an active agent for the
solution of soluble pyroxyline. The desirability of these ends is in the art fully
recognized. I have found that these ends are attained by selecting suitable
menstrua (which are or are not solvents as may be best suited to the particular case)
and submitting the menstrua or menstruum to an ozonizing process. Whilst the
material treated may and does vary according to the product desired and its
application, and whilst the method of applying the ozone may and does vary
according to the character of the material to which it is applied, the ozone itself
is always used as ozone and never as oxygen, and is generated as ozone as a distinct
and separate entity, and is not applied as ozone liberated or set free by chemical
reactions within the liquid or the liquid equivalent under treatment. It is further
requisite not only that ozone should be merely present in the course of the treatment
which is the subject of my invention, but it must exist in considerable quantity and
generally very much in excess of what might be judged to be a theoretically
chemical combining proportion as calculated from the hypothetical reactions of
oxidation assumed to occur in a given result. Otherwise I have met with failure
in my trials. This condition therefore in the present state of chemical science
practically limits the means of producing the ozone employed to the electrification
of oxygen gas; and it is necessary that the ozone be used dry, that is, free from
aqueous vapor. In certain cases its temperature may be advantageously raised
above the atmospheric temperature, to within say 120° F., but generally full effects
will be produced at ordinary atmospheric temperatures. Whilst the temperature of
the gas may be increased with advantage, it is not to be implied that the temperature
of the material treated can also be advantageously raised, because the contrary is
generally the case, and it may be stated as a general instruction that the menstruum
or menstrua under treatment are best artificially cooled to below ordinary atmo-
spheric temperature, and to a degree differing with the substance treated.
The method of treating a given menstruum differs with the nature of the
menstruum. For instance, it suffices ordinarily to pass a current of ozone through
the liquid menstruum in the manner well known in chemical manipulation,
accelerating the passage of the same by aspiration or pressure. But in cases where
the menstruum quickly yields solid or semi-solid products of ozonization, or in cases
where a viscis liquid such as one of the viscid essential oils is to be treated to
render it more quickly drying, the bubbles of gas in their passage through the
menstruum are apt to become coated or surrounded with a film of some tenacity,
which causes a waste of the gas by preventing its further action on the menstruum,

page_text: after such a film is formed, as well as spirting at the surface of the liquid when the
bubble breaks there, and the formation of a scum or skin on the surface of the
liquid hindering the passage of the gas. In such cases it is preferable to inject
the menstruum as. a spray into a chamber in which an ozone atmosphere is
maintained.
I wish it to be distinctly understood as an induction to which I have been led by
my researches, and from theoretical considerations that would be out of place if
stated in the Specification of a Letters Patent, that I do not consider the treatment
with ozone to which the menstrua are subjected as a process of mere oxidation,
because I have found that the ozone enters into solution and becomes in many
instances compounded into the substance ultimately formed; and whether the
result may be brought about as the result of a solution of ozone, or as the result of
compounding either with ozone or with allotropic oxygen is immaterial to my
claim, and as relates to my invention in procuring solvents and solutions of
pyroxyline.
To instance applications of my invention, I cite the following, but I do not limit
myself to the mentioned applications, because it is obvious that my invention is
applicable to so many of the series of essential oils as are too numerous to include,
and the principle being given a chemist skilled in this branch of his art can readily
apply the same.
Oil of turpentine is practically non-solvent of pyroxyline; treated with ozone to
saturation it becomes an active solvent.
Oil of camphor is greatly increased in solvent power by being sprayed into a
chamber or vessel in which an ozone atmosphere is maintained.
Oil of carraway-seed, which is practically non-drying though a good solvent of
pyroxline, becomes possessed of drying properties.
Methyl alcohol that gives cloudy films and a pitted and striated character to the
films from solutions in which it enters too largely, when treated with ozone
yields a clear film, and becomes possessed of greater solvent power, as indicated by
the greater fluidity of a solution containing like amount of pyroxyline to oue made
with methyl alcohol not so treated. Acetone is rendered a more certain solvent by
ozone treatment.
Acetal yields after treatment with ozone a clear solution and not a merely
disintegrated mass as occurs with pyroxyline dissolved in acetal not so treated.
Ethyl-amyl ether saturated with ozone becomes a powerful solvent of soluble
pyroxyline.
Fusel oil which is non-solvent of pyroxyline becomes to a certain degree solvent
when treated with ozone.
Whilst my invention is intended to apply more particularly to liquid solutions of
pyroxyline, I do not limit myself to such liquid solutions, because I can by suitable
modifications produce masses pre-eminently suited to the manufacture of solid
'compounds. For instance, by placing in a chamber soluble pyroxyline and by intro-
ducing into that chamber the vapor of camphene together with ozone and a very finely
divided spray of an alcohol, the pyroxyline is very rapidly converted under the
influence of the vapor of camphor that is formed, and becomes a converted mass
containing the smallest possible quantity of the alcohol (which under certain
mechanical manipulation may be omitted). In this case camphene is the menstruum
in the vapor condition.
As a particular application of an ozonized menstruum used in addition to or used
with other solvents, I have found the following very suitable as a metal lacquer,
namely aceto-acetate of amyl twenty gallons; ozonized fusel oil five gallons;
wood-alcohol five gallons; benzine fifteen gallons; pyroxyline fifteen to twenty
pounds.
:
Dated this 18th dow of Nam 1000
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.

page_text: Improvements in Pyroxyline Compounds, Solutions, and Solvents.
I, LEONARD PAGET, of 300 Fourth Avenue, New York City, United States,
America, 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 :-
The object of my invention is, first, to improve in solvent power those weak solvents
of soluble nitro-cellulose or pyroxyline that are otherwise, from their characteristic
volatility and other properties, useful in the art, but which are too weak in solvent
power to become usefully employed in their normal conditions; secondly, to impart
solvent power to menstrua otherwise non-solvent without addition to their volume
or bulk or without material change in their practical properties; thirdly, to render
certain solvent essential oils that are impaired in their utility in the art by reason
of their fixed or non-volatile character, more easily drying or siccative; fourthly,
to determine in those camphoraceous oils and balsams such development of the
so-called camphor as may bring about, in conjunction with alcohol, fusel oil, and
other inactive solvents, an active agent for the solution of soluble pyroxyline. The
desirability of these ends is in the art fully recognised. I have found that these
ends are attained by selecting suitable menstrua (which are or are not solvents as
may be best suited to the particular case) and submitting the menstrua or menstruum
to an ozonizing process.
Whilst the material treated may and does vary according
to the product desired and its application, and whilst the method of applying the
ozone may and does vary according to the character of the material to which it is
applied, the ozone itself is always used as ozone and never as oxygen; and is
generated as ozone as a distinct and separate entity, and is not applied as ozone
liberated or set free by chemical reactions within the liquid or the liquid equivalent
under treatment. It is further requisite not only that the ozone should be merely
present in the course of the treatment which is the subject of my invention, but it
must exist in considerable quantity and generally very much in excess of what
might be judged to be a theoretically chemical combining proportion as calculated
from the hypothetical reactions of oxidation assumed to occur in a given result.
Otherwise I have met with failure in my trials. This condition therefore in the
present state of chemical science practically limits the means of producing the
ozone employed to the electrification of oxygen gas; and it is necessary that
the ozone be used dry, that is, free from aqueous vapour. In certain cases its
temperatures may be advantageously raised above the atmospheric temperature, to
within say 120° F., but generally full effects will be produced at ordinary atmospheric
temperatures. Whilst the temperature of the gas may be increased with advantage,
it is not to be implied that the temperature of the material treated can also be
advantageously raised, because the contrary is generally the case, and it may be
stated as a general instruction that the menstruum or menstrua under treatment
are best artificially cooled to below ordinary atmospheric temperature, and to a
degree differing with the substance treated.
The method of treating a given menstruum differs with the nature of the
menstruum. For instance, it suffices ordinarily to pass a current of ozone through
the liquid menstruum in the manner well known in chemical manipulation,
accelerating the passage of the same by aspiration or pressure. But in cases where
the menstruum quickly yields solid or semi-solid products of ozonization, or in cases
where a viscis liquid such as one of the viscid essential oils is to be treated to
render it more quickly drying, the bubbles of gas in their passage through the
menstruum are apt to become coated or surrounded with a film of some tenacity,
which causes a waste of the gas by preventing its further action on the menstruum,
after such a film is formed, as well as spirting at the surface of the liquid when
the bubble breaks there, and the formation of a scum or skin on the surface of the

page_text: liquid hindering the passage of the gas. In such cases it is preferable to inject
the menstruum as a spray into a chamber in which an ozone atmosphere is
maintained.
I wish it to be distinctly understood as an induction to which I have been led
by my researches, and from theoretical considerations that would be out of place if
stated in the Specification of a Letters Patent, that I do not consider the treatment
with ozone to which the menstrua are subjected as a process of mere oxidation,
because I have found that the ozone enters into. solution and becomes in many
instances compounded into the substance ultimately formed; and whether the
result may be brought about as the result of a solution of ozone, or as the result
of compounding either with ozone or with allotropic oxygen is immaterial to my
claim, and as relates to my invention in procuring solvents and solutions of
pyroxyline.
To instance applications of my invention, I cite the following, but I do not limit
myself to the mentioned applications, because it is obvious that my invention is
applicable to so many of the series of essential oils as are too numerous to include,
and the principle being given a chemist skilled in this branch of his art can readily
apply the same.
Oil of turpentine is practically non-solvent of pyroxyline; treated with ozone to
saturation it becomes an active solvent.
Oil of camphor is greatly increased in solvent power by being sprayed into a
chamber or vessel in which an ozone atmosphere is maintained.
Oil of carraway-seed, which is practically non-drying though a good solvent of
pyroxyline, becomes possessed of drying properties.
Methyl alcohol that gives cloudy films and a pitted and striated character to the
films or from solutions in which it enters too largely, when treated with ozone yields
a clear film, and becomes possessed of greater solvent power, as indicated by the
greater fluidity of a solution containing like amount of pyroxyline to one made with
methyl alcohol not so treated. Acetone is rendered a more certain solvent by
ozone treatment.
Acetal yields after treatment with ozone a clear solution and not a merely
disintegrated mass as occurs with pyroxyline dissolved in acetal not so treated.
Ethyl-amyl ether saturated with ozone becomes a powerful solvent of soluble
pyroxyline.
Fusel oil which is non-solvent of pyroxyline becomes to a certain-degree solvent
when treated with ozone.
Whilst my invention is intended to apply more particularly to liquid solutions of
pyroxyline, I do not limit myself to such liquid solutions, because I can by suitable
modifications produce masses pre-eminently suited to the manufacture of solid
compounds. For instance, by placing in a chamber soluble pyroxyline and by
introducing into that chamber the vapour of camphor together with ozone and a
very finely divided spray of an alcohol, the pyroxyline is very rapidly converted
under the influence of the vapour of camphor that is formed, and becomes a
converted mass containing the smallest possible quantity of the alcohol (which under
certain mechanical manipulation may be omitted). In this case camphene is the
menstruum in the vapour condition.
As a particular application of an ozonized menstruum used in addition to or used
with other solvents, I have found the following very suitable as a metal lacquer,
namely aceto-acetate of amyl twenty gallons, ozonized fusel oil five gallons;
wood-alcohol five gallons; benzine fifteen gallons; pyroxyline fifteen to twenty
pounds.
:
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 :-
1. A solution of pyroxyline consisting of pyroxyline dissolved in an ozonized
menstruum.

page_text: 2. A compound of pyroxyline consisting of pyroxyline converted in au ozonized
menstruum.
3. A solution or compound of pyroxyline consisting of pyroxyline a solvent and
an ozonized menstruum.
4. As an article of manufacture a metal lacquer which consists of pyroxyline
dissolved in a mixture of aceto-acetate of amyl, ozonized fusel oil, wood alcohol and
benzine.
Dated this 29th day of November 1893.
HASELTINE, LAKE & Co.,
45, Southampton Buildings, London, W.C., Agents for the Applicant.