Method and manufacture of carboxyalkylinulin
View Patent ↗A method for the manufacture of carboxyalkylinulin is disclosed comprising preparing an aqueous medium containing dispersed therein a halogenoalkylcarboxylate, adding to the carboxylate containing medium, under substantially neutral pH conditions, an inulin followed by heating this mixture to a temperature in the range of from 60° C. to 90° C. and proceeding with the reaction at alkaline conditions, pH 8-12, while simultaneously adding additional halogenoalkylcarboxylate and alkalihydroxide. The carboxyalkylinulin so formed is recovered in a manner known per sé.
1. A method for the manufacture of carboxyalkylinulin by reacting inulin with a halogenoalkylcarboxylate under alkaline conditions, characterized in that:
(a) from 25 to 150 molar-%, expressed in relation to the molar amount of monosaccharide units in the inulin (100%), of the X-halogenoalkylcarboxylate, wherein the halogen is selected from chlorine, bromine and iodine, the alkyl chain contains from 1 to 5 carbon atoms, and X is an alkaline ion from the group of sodium and potassium, is dispersed into an aqueous medium, the aqueous medium containing optionally up to 35% by weight of inulin;
(b) adding to and dispersing into the halogenoalkylcarboxylate medium (a) the inulin to yield a slurry, having a pH, measured on the slurry at a temperature of from 20° C. to 70° C., in the range of from about 5 to 8, containing from about 25% to about 70% by weight of the inulin, expressed in relation to the amount of water (100%-by weight) in the slurry;
(c) heating the slurry (b) to a temperature from about 60° C. to about 90° C., followed by concurrently adding additional halogenoalkylcarboxylate, to yield a molar ratio of halogenoalkylcarboxylate:inulin of from 1.0 to 5.0, and an alkaline hydroxide, from the group of sodium and potassium hydroxide, in a quantity equimolar to the total level of halogenoalkylcarboxylate, plus an additional amount of the alkaline hydroxide of from 10 to 50 molar-%, expressed in relation to the molar amount of fructose units in the inulin (100%), to yield a reaction mixture pH in the range of from 8 to 12, measured at the reaction temperature (60° C. to 90° C.);
(d) continuing the reaction, after all the reagents have been added, for a period up to 90 minutes, at the reaction temperature; and
(e) recovering the carboxyalkylinulin reaction product in a manner known per se.
2. The method in accordance with claim 1 wherein the halogenoalkylcarboxylate in step (a) represents from 70% to 100 molar-% and wherein the slurry (b) contains from 40% to 60% by weight of inulin.
3. The method in accordance with claim 1 wherein the molar ratio of halogenoalkylcarboxylate:inulin in step (c) is the range of from 1.5 to 4.5.
4. The method in accordance with claim 1 wherein the slurry (b) is heated to a temperature in the range of from 70° C. to 90° C.
5. The method in accordance with claim 4 wherein the pH of the reaction mixture in step (c) is in the range of from 9.5 to 11.5.
6. The method in accordance with claim 4 wherein the reaction is continued for a period of from 20 to 60 minutes after all the reagents have been added.
7. The method in accordance with claim 1 wherein the alkyl moiety in the carboxyalkylinulin is represented by a carbon chain having from 1 to 3 carbon atoms.
8. The method in accordance claim 1 wherein the slurry (b) is heated to a temperature in the range of from 75° C. to 85° C.
9. The method in accordance with claim 1 wherein the carboxyalkylinulin is carboxymethylinulin.
10. The method in accordance with claim 1 wherein the aqueous medium in step (a) contains from about 10% to about 30%-by weight of the inulin.