IMPROVEMENTS IN THE TREATMENT OF CELLULOSE AND THE MANUFACTURE OF ARTICLES THEREFROM
Year: 1881

page_text: LETTERS PATENT to Alexander Parkes, of Gravelly Hill, near Birmingham,
in the County of Warwick, for an Invention of "IMPROVEMENTS IN THE
TREATMENT OF CELLULOSE AND THE MANUFACTURE OF ARTICLES THEREFROM,
PROVISIONAL SPECIFICATION left by the said Alexander Parkes at the
Office of the Commissioners of Patents on the 8th March 1881.
ALEXANDER PARKES, of Gravelly Hill, near Birmingham, in the County of
Warwick. "IMPROVEMENTS IN THE TREATMENT OF CELLULOSE AND THE MANU-
FACTURE OF ARTICLES THEREFROM, AND IN PREVENTING THE RAPID COMBUSTION
OF NITRO-CELLULOSE."
The first part of this Invention refers to the solution of cellulose or substances
of a similar nature. Preferring cotton or linen fibre or paper of these substances
or the same in a textile or felted condition or other woody cellulose.
For dissolving the cellulose substances such as above named I employ iodide
of zinc or nitrate of zinc. I have found the cellulose so treated to be strong and
colourless when the operation is completed, and it may be combined with coloring
substances or pigments, and moulded or shaped in various forms by pressure or
otherwise.
Although I prefer iodide of zinc or nitrate of zinc, chloride of zinc alone or mixed
with the above may also be used to effect the solution of the cellulose. I also use
nitrate of lime or chloride of lime.
Whether I employ nitrate of zinc, or iodide of zinc, or chloride of zinc, or any of
the above named as solvents of cellulose, I effect a complete solution of the cellulose,
so as to be able to employ it, whether combined with coloring matter or pigments
or not, in a partly fluid, plastic, or hard condition.
For this purpose I prepare a concentrated and neutral solution of nitrate of
zinc (if nitrate of zinc is used) of such degree of concentration as will at once
dissolve cotton or paper by simply immersing cellulose in the nitrate of zinc.
Preferably I employ the nitrate of zinc in a heated state of about 250 degrees

page_text: Fahrenheit, and if I wish to have a solution more or less thick I only dissolve
sufficient cellulose for the purpose, and more cellulose is dissolved in the nitrate of
zinc if I require a stiffer pasty condition, and so on until the nitrate will dissolve
no more cellulose; this thick solution may be greatly assisted by employing suitable
machinery to break or blend up the compound, and if heated the heat must not be
so high as to carbonize the cellulose; this will be readily understood by a practical
workman. I have found from 250 to 300 degrees Fahrenheit sufficient.
The cellulose as above dissolved I use as a coating to other articles, such as paper,
textile fabrics, leather, wood, metals, and such like.
Or I employ it alone or combined with other substances to form solid or hollow
articles, and whether the nitrate of zinc is removed before or after the articles are
shaped or moulded.
If I employ the dissolved cellulose as a coating to paper, textile fabrics, or other
substances, I prefer to use it with the solvent still in it, as by so doing I find it
will be firmly attached to the paper or other surface. When the coating is effected
the solvent of nitrate of zinc can be removed by washing in water or by alcoholic
solutions. The articles so coated: may be calendered or embossed or otherwise
finished, and will produce a fine and hard or flexible surface to the paper cloth, &c.
In moulding sheets or other forms or hollow ware these may be formed whilst
the solvent of the cellulose remains, and it can be afterwards removed by water or
alcoholic, or vegetable naptha solutions, and the articles so formed may be further
finished by rolling, pressing or otherwise to consolidate or produce the surface of a
finer or more ornamental character.
I have also found that the solvent of the cellulose may be first removed by
washing, and that the washed cellulose may then be pressed or rolled into sheets
or other forms, whether combined with pigments or colors or not.
I have also found that I can wash and then pulp or granulate the dissolved
cellulose and color it by dyes or pigments, and in this pulped condition it does not
loose the property of strongly adhering together by pressure, rolling, or spreading,
and by these means I am able to form a new and valuable substance as hard as
ivory, tortoise shell, or horn, and which, being free from smell and also uninflammable,
may be used for an endless variety of purposes.
The hard substance as above formed can be turned in a lathe, cut with a saw,
and shaped or finished as tubes, combs, buttons, knife handles, and other articles,
and may be white and of all delicate colors or black as desired.
In order to prevent the rapid combustion of nitro-cellulose which has been an
objection to the use of nitro-cellulose or xylodine articles, I admix with dissolved
nitro cellulose oxalates of lime or zinc, or phosphates of lime, zinc, or alumina, and
oxalates of magnesia, baryta, and strontia, and phosphate of soda and ammonia,
ammonia phosphate of magnesia, tungstate of zinc, borate of zinc, and phosphate
of zinc, or borasic acid.
By this improvement the above mentioned objection is removed and the nitro-
cellulose even rendered more perfect in color properties than hitherto.

page_text: SPECIFICATION in. pursuance of the conditions of the Letters Patent filed.
by the said Alexander Parkes in the Great Seal Patent Office on the 7th
September 1881.
"
ALEXANDER PARKES, of Gravelly Hill, near Birmingham, in the County of
Warwick. IMPROVEMENTS IN THE TREATMENT OF CELLULOSE AND THE MANU-'
FACTURE OF ARTICLES THEREFROM, AND IN PREVENTING THE RAPID COMBUSTION
OF NITRO-CELLULOSE."
Heretofore paper, thread, twine, and other articles composed of vegetable fibre
have been passed through a solution of chloride of zinc to partially dissolve their
surface and form a glaze or varnish over it. Sheets of paper so passed through a
solution of chloride of zinc have also been laid one upon another so as to form
them into boards, and such boards have been cut up into various forms. Sheets of
paper passed through the solution have also been wrapped around cylindrical
mandrils so as to form tubes, or have been laid one over the other upon moulds of.
various shapes, so as to form boxes and other articles. According to my Invention
I first obtain a complete solution of cellulose or such like substance from cotton or
linen fibre, or from paper or fabric made from such fibre, or from other woody
cellulose, and combine with it coloring matters or pigments, and mould or shape
the mixture into various forms by pressure or otherwise, or I employ it for coating
paper or other surfaces.
For dissolving the cellulose I employ iodide of zinc or nitrate of zinc. These
substances should be employed as neutral as possible, and concentrated to a syrupy
condition of about 1600 to 1.750 sp. gr. heated to about 200° Fahrenheit or a
higher temperature, but not so high as to cause carbonization of the cellulose or
woody fibre. Although I prefer iodide of zinc or nitrate of zinc, chloride of zinc
alone or mixed with the above may also be used to effect the solution of the
cellulose and nitrate of lime, or chloride of calcium may also be used.
Whether I employ nitrate of zinc, or iodide of zinc, or chloride of zinc, or any of
the above named as solvents of cellulose, they must be concentrated to from 1-600
to 1-800 sp. gr. and by preference heated to 180° to 250° Fahrenheit. The cotton
or paper (whether pulped or otherwise) or fibre is immersed in the nitrate of zinc
or other solvent and quickly dissolves, and I continue to add fibre or paper until
the solution arrives at a stiff, pasty condition, suitable kneading or mixing
machinery heated to the required temperature being employed to break or blend
up the compound as the dissolving of the cellulose goes on. The pasty mass may
also be put by for future use and masticated afterwards.
If the cellulose solution is to be used for coating paper, textile fabrics, leather,
wood, metals, and such like, it may be used thinner than when' articles are to be
shaped and moulded from it.
For coating paper, textile fabrics, and other surfaces, I prefer to use the cellulose.
solution in a pasty and well blended state, and heated so that it shall remain
plastic. I spread it upon the paper by the use of a gauge, knife, and rollers, or
other spreading machinery with the solvent still remaining in it, as by so doing I
find it will be firmly attached to the paper or other surface, and two or more coats
may be applied if it is desired to increase the thickness. When the coating has been
effected the nitrate of zine or other solvent can be removed by washing in water
or alcoholic solutions. The articles so coated may be calendered or embossed or
otherwise finished, and will produce upon the paper or other substance a fine hard
flexible surface.
Sheets and other forms and hollow ware may also be moulded from the cellulose
solution whilst the solvent remains in it, and the solvent can afterwards
similarly be removed by water or alcoholic or vegetable naptha solutions, and the
articles so formed may be further finished by rolling, pressing, or otherwise

page_text: to consolidate them and give to their surface a finer and more ornamental
character.
I have also found that the solvent of the cellulose may be first removed by
washing the solution in an agitating or pulping machine, and that the washed
cellulose may then be pressed or rolled into sheets or other forms whether combined
with pigments or colors or not.
I have also found that I can wash and then pulp or granulate the dissolved
cellulose and color it by dyes or pigments, and in this pulped condition it does not
lose the property of strongly adhering together when subjected to pressure and
slightly heated in moulds or in rolling or spreading machinery, it can also be
floated as in paper making upon fabrics, or can be made into a substantial sheet
alone, and on being calendered in the usual way it forms a fine vellum like sheet
or substance, and by these means I am able to form a new and valuable substance
as hard as ivory, tortoiseshell, or horn, and which being free from smell and also
uninflammable may be used for an endless variety of purposes. The hard substance
formed as above can be turned in a lathe, cut with a saw, and shaped or finished
into figures, animals, tubes, combs, buttons, knife handles, and other articles, plain or
ornamental; and may be white or black, or colored with a variety of delicate colors,
pigments, or dyes, as desired.
In order to prevent the rapid combustion of nitro-cellulose, which has been an
objection to the use of nitro-cellulose or xylodine articles, I admix with dissolved
nitro-cellulose-oxalates of lime or zinc, or phosphates of lime, zinc, or alumina, and
oxalates of magnesia, barayta and strontia, and phosphate of soda and ammonia,
ammonia phosphate of magnesia, tungstate of zinc, borate of zinc, and phosphate of
zine or borasic acid; of these substances I believe phosphate of zinc to be best
for the purpose; from 10 to 100 or 150 per cent. of the substances will be found
sufficient to prevent the rapid combustion of articles made of the cellulose or nitro-
cellulose substances.
By these improvements the above mentioned objection is removed, and the nitro-
cellulose even rendered more perfect in color properties than hitherto.
I claim,—
First. The process herein before described of making articles of cellulose and of
coating articles therewith, consisting in first dissolving cellulose in a solution of
iodide of zinc, or nitrate of zinc, or other such like solvents or mixtures of them,
then moulding the dissolved cellulose to the form required, or spreading it over
the surface to be coated, then removing the solvent by washing, and finally rolling,
pressing, or calendering the articles or coated articles to consolidate them and
improve their surface.
Second. The process herein before described of making articles of cellulose or
partly of cellulose, consisting in first dissolving cellulose as above set forth, then
washing out the solvent from the cellulose, and then moulding the cellulose to the
form required by subjecting it to pressure in moulds or otherwise, or by rolling or
spreading machinery.
Third. The combination with solutions of nitro-cellulose of one or more of the
substances hereinbefore specified to prevent the nitro cellulose compounds from
being liable to rapid combustion.
In witness whereof, I, the said Alexander Parkes, have hereunto set my
hand and seal, this First day of September, in the year of our Lord One
thousand eight hundred and eighty one.