Manufacture of Cellulose Esters.
Year: 1898

page_text: Date of Application, 19th Oct., 1898
Cannifination Loft 18th May 1899-Accepted. 1st July, 1899
Manufacture of Cellulose Esters.
We, CARL OTTO WEBER, of Greengate, Salford, Lancashire, Chemist, CHARLES
FREDERICK CROSS, of 4, New Court, Lincoln's Inn, in the County of London,
Analytical Chemist, and ISIDOR FRANKENBURG, of Greengate Works, Salford,
Lancashire, do hereby declare the nature of this invention to be as follows:-
-
Compounds of cellulose with acetic acid have been manufactured by treating
structureless cellulose with zinc or magnesium acetate, acetic anhydride and
acetyl chloride, the reaction being moderated by addition of a diluent such as
nitro benzene.
The present invention relates to the manufacture of compounds of cellulose
with the higher fatty acids or aromatically substituted fatty acids, thus obtain-
ing esters of cellulose differing from and in some respects superior to those
obtained by the acetic acid treatment.
For this purpose one molecule of cellulose in structureless form preferably such
as that obtained in the known manner from solutions of cellulose sulphocarbonate
has added to it one moleule of the zinc or magnesium, salt of any one of the
fatty acids or of a mixture of zinc or magnesium salts of any of these acids.
The salt or salts are preferably employed as a cencentrated solution which is
added to and thoroughly mixed with the cellulose, the mixture being then dried
on the water bath. To the dried mixture are added two molecules of acyl
chloride and a small quantity of acid anhydride these being both derivatives
of the acid contained in the zinc or magnesium salt or each of them being a
derivative of any of the higher fatty acids or aromatically substituted acids.
The whole mixture of cellulose, salt, chloride and anhydride is heated on the
water bath until it begins to thicken, whereupon nitro-benzene is added, first
in small doses, then in larger and larger quantities as the reaction proceeds. The
nitro benzene acts merely as a diluent moderating and controlling the reaction
Other diluents
and preventing aggregation of the product into a solid mass.
might be employed such as homologues of nitro-benzene, or epichlorhydrin or
dichlorhydrin and the diluent should be added in such quantity that the material
under reaction should not become heated above 70° C.
The result of the reaction is a solution from which the cellulose ester is pre-
cipitated in fine light flakes on pouring the solution into alcohol, which, as well
as the diluent can be recovered. The cellulose ester being washed retains its
flocculent condition, so that when dried it still consists of fine light flakes solubla
in any of the solvents for cellulose acetate.
11:
104
day of October 1898.
ABEL & IMRAY,
Agents for the Applicants.

page_text: We, CARL OTTO WEBER, of Greengate, Salford, Lancashire, Chemist, CHARLES
FREDERICK CROSS, of 4, New Court, Lincoln's Inn, in the County of London.
Analytical Chemist, and ISIDOR FRANKENBURG, of Greengate Works, Salford,
Lancashire, 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:--
Compounds of cellulose with acetic acid have been manufactured by treating
structureless cellulose with zinc or magnesium acetate, acetic anhydride and
acetyl chloride, the reaction being moderated by addition of a diluent such as
nitro benzene.
The present invention relates to the manufacture of compounds of cellulose
with the higher fatty acids or aromatically substituted fatty acids, thus obtain-
ing esters of cellulose differing from, and in some respects superior to those
obtained by the acetic acid treatment.
a
For this purpose one molecule of cellulose in structureless form preferably such
as that obtained in the known manner from solutions of cellulose sulphocarbonate
has added to it one molcule of the zinc or magnesium salt of any one of the
fatty acids or of a mixture of zinc or magnesium salts of any of these acids.
The salt or salts are preferably employed as a concentrated solution which is
added to and thoroughly mixed with the cellulose, the mixture being then dried
on the water bath. To the dried mixture are added two molecules of acyl
chloride and a small quantity of acid anhydride these being either both derivatives
of the acid contained in the zinc or magnesium salt or each of them. being
derivative of any of the higher fatty acids or aromatically substituted fatty acids.
The whole mixture of cellulose, salt, chloride and anhydride is heated on the
water bath until it begins to thicken, whereupon nitro-benzene is added, first
in small doses, then in larger and larger quantities as the reaction proceeds. The
nitro-benzene acts merely as a diluent moderating and controlling the reaction
and preventing aggregation of the product into a solid mass. Other diluents
might be employed such as homologues of nitro-benzene, or epichlorhydrin or
dichlorhydrin and the diluent should be added in such quantity that the material
under reaction should not become heated above 70° C.
The result of the reaction is a solution from which the cellulose ester is pre-
cipitated in fine light flakes on pouring the solution into alcohol, which, as well
as the diluent can be recovered. The cellulose ester being washed retains its
flocculent condition, so that when dried it still consists of fine light flakes soluble
in any of the solvents for cellulose acetate.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed, we declare that what we
claim is
T
1. The herein described manufacture of cellulose esters by mixing structureless
cellulose with the zinc or magnesium salt of any of the higher fatty acids or
aromatically substituted fatty acids and treating this mixture with the acyl
chlorides and anhydrides of any of these acids.
2. The herein described manufacture of mixed cellulose esters by mixing
structureless cellulose with the zinc or magnesium salt of any of the higher
fatty acids, or acetic acid, or aromatically substituted fatty acid, and treating
this mixture with the acyl chloride and anhydride of any of these acids, not

page_text: being derivatives of the acids employed in the form of their before named zinc
or magnesium salts.
3. Cellulose esters and mixed cellulose esters manufactured as above set forth.
Dated this 18th day of May 1899.
ABEL & IMRAY,
Agents for the Applicants.