Cellulose derivatives having gel-like rheological properties and process for the preparation thereof
View Patent ↗A description is given of cellulose derivatives having gel-like rheological properties in aqueous solution characterized in that: a) cellulose is alkalized with aqueous alkali metal hydroxide solution in the presence of a suspension medium, b) the alkalized cellulose is reacted with one or more alkylene oxides, c) then reacted with an alkyl halide present in the suspension medium d) subsequently or simultaneously the alkalized cellulose is reacted with a crosslinking agent in an amount of 0.0001 to 0.05 eq, where the unit “eq” represents the molar ratio of crosslinking agent relative to the anhydroglucose unit (AGU) of the cellulose used, and e) after, if appropriate, further addition of alkali metal hydroxide and/or alkylating agent, the resultant irreversibly crosslinked cellulose derivative is separated off from the reaction mixture, if appropriate purified and dried.
1. A process for preparing a cellulose derivative having gel-like rheological properties in aqueous solution, comprising:
a) alkanizing cellulose with aqueous alkali metal hydroxide in the presence of a suspension medium;
b) reacting the alkalized cellulose with one or more alkylene oxides, thereby forming an alkalized cellulose;
c) reacting the alkalized cellulose of step (b) with an alkyl halide present in the suspension medium;
d) reacting subsequently or simultaneously with step (c) the alkalized cellulose of step (c) with a crosslinklng agent in an amount of 0.0001 to 0.05 eq. where the unit “eq” represents the molar ratio of crosslinking agent relative to the anhydroglucose unit (AGU) of the cellulose used, thereby forming an irreversibly crosslinked cellulose derivative;
e) optionally adding a member selected from the group consisting of alkali metal hydroxide, alkylating agent and combinations thereof;
f) optionally separating off the irreversibly crosslinked cellulose derivative from the reaction mixture; and
g) optionally purifying and drying the isolated irreversibly crosslinked cellulose derivative.
2. The process of claim 1 wherein in step a), the cellulose is alkalized using aqueous alkali metal hydroxide in the presence of a suspension medium comprising alkyl halide in an amount calculated from the following formula:
[equivalents of alkali metal hydroxide per AGU minus 1.4]
to
[equivalents of alkali metal hydroxide per AGU plus 0.8],
and in step e) alkyl halide is added in an amount which is at least the difference between the number of equivalents of alkyl halide per AGU already added and the total amount of alkali metal hydroxide per AGU added, where this amount is a minimum of 0.2 equivalents per AGU, and, optionally, further alkali metal hydroxide.
3. The process of claim 1 wherein the alkyl halide is methyl chloride.
4. The process of claim 1 wherein the crosslinking agent is dissolved in solvent selected from the group consisting of methyl chloride and a mixture of methyl chloride and dimethyl ether.