# US 5,708,162 A · Process for the preparation of low molecular weight polysaccharide ethers > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,708,162 A - Document ID: US5708162A - Status: Granted - Kind: A - Application number: 08/416,185 - Filed: 1995-04-04 - Granted: 1998-01-13 - Earliest claimed: 1994-04-05 - Assignees: Hoechst Aktiengesellschaft - Inventors: Josef Hilbig; Reinhard Doenges - Web page: https://patentgrep.com/patent/US5708162A ## CPC - C08B 37/0087: {Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof} - C08B 11/20: Post-etherification treatments of chemical or physical type, {e.g. mixed etherification in two steps}, including purification - C08B 31/08: Ethers - C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21) ## Abstract Process for the preparation of low molecular weight polysaccharide ethers which can be employed in binders for improving adhesive power and film-forming properties, by oxidative degradation of relatively high molecular weight polysaccharide ethers, which comprises initially introducing a relatively high molecular weight polysaccharide ether in suspension (e.g. in a slurry), adding a perborate or a mixture of perborate and perborate activator, and carrying out the oxidative degradation at a temperature of between 25.degree. and 90.degree. C. ## Claims ### Claim 1 A process for lowering the molecular weight of a cellulose ether or starch ether by oxidative degradation, comprising: adding to a cellulose ether or starch ether starting material a perborate and carrying out the oxidative degradation at a temperature in the range of about 25.degree. to about 90.degree. C. to obtain the oxidatively degraded product. ### Claim 2 (depends on 1) The process as claimed in claim 1, wherein the cellulose ether or starch ether starting material is in suspension in a suspension medium and has an average molecular mass M of from 10,000 to 350,000 g/mol, and wherein the resulting oxidatively degraded cellulose ether or starch ether is recovered from the suspension medium. ### Claim 3 (depends on 1) The process as claimed in claim 1, wherein the ether starting material comprises a cellulose ether, and the cellulose ether is a carboxyalkylcellulose ether, hydroxyalkylcellulose ether, alkylcellulose ether, alkylhydroxyalkylcellulose ether, alkylhydroxyalkylcarboxyalkylcellulose ether, sulfoalkylcellulose ether, carboxyalkylsulfoalkylcellulose ether, alkylhydroxyalkylsulfoalkylcellulose ether, alkyloxyhydroxyalkylhydroxyalkylcellulose ether or hydroxyalkylsulfoalkylcellulose ether. ### Claim 4 (depends on 3) The process as claimed in claim 3, wherein the cellulose ether contains a C.sub.1 -C.sub.4 -alkyl group. ### Claim 5 (depends on 1) The process as claimed in claim 1, wherein the cellulose ether or starch ether starting material comprises a starch ether, and the starch ether is a carboxyalkylstarch ether, hydroxyalkylstarch ether or a mixed ether thereof. ### Claim 6 (depends on 1) The process as claimed in claim 1, wherein a said perborate is an alkali metal perborate, an alkaline earth metal perborate or a mixture thereof. ### Claim 7 (depends on 6) The process as claimed in claim 6, wherein the alkali metal perborate is sodium perborate tetrahydrate, sodium perborate monohydrate, or a mixture thereof. ### Claim 8 (depends on 1) The process as claimed in claim 1, wherein the oxidative degradation comprises adding an oxidatively-active ingredient which consists essentially of a said perborate alone or in combination with a perborate activator. ### Claim 9 (depends on 8) The process as claimed in claim 8, wherein said oxidatively-active ingredient is added in the form of a solution, a crystal suspension or as a solid. ### Claim 10 (depends on 8) The process as claimed in claim 8, wherein said oxidatively-active ingredient is added in the form of a solution, and the solvent for said solution comprises water. ### Claim 11 (depends on 8) The process as claimed in claim 8, wherein the suspension medium employed for the crystal suspension is water, a water-miscible organic solvent or an aqueous mixture thereof. ### Claim 12 (depends on 11) The process as claimed in claim 11, wherein the water-miscible organic solvent employed is a C.sub.1 -C.sub.6 alcohol, an ether or a ketone. ### Claim 13 (depends on 8) The process as claimed in claim 8, wherein said oxidatively-active ingredient is added in the form of an aqueous solution, and wherein said solution contains an amount of perborate ranging from an oxidatively effective amount up to 2.5% by weight, based on the weight of solution. ### Claim 14 (depends on 9) The process as claimed in claim 9, wherein said oxidatively-active ingredient is added in the form of a crystal suspension in a suspension medium, and the ratio of perborate or perborate/perborate activator combination to suspension medium is from 1:2 to 1:15. ### Claim 15 (depends on 1) The process as claimed in claim 1, wherein the oxidative degradation is carried out in the presence of a perborate activator, and wherein said perborate activator contains an acyl group. ### Claim 16 (depends on 15) The process as claimed in claim 15, wherein the molar quantity of perborate, based on the perborate activator, is equal to the molar quantity of peroxy acid which is formed from one mole of perborate activator. ### Claim 17 (depends on 1) The process as claimed in claim 1, wherein the quantity of perborate is from 0.1 to 20% by weight, based on the dry weight of the cellulose ether or starch ether starting material. ### Claim 18 (depends on 1) The process as claimed in claim 1, wherein the oxidative degradation is carried out at an alkaline pH above 7. ### Claim 19 (depends on 1) The process as claimed in claim 1, wherein the cellulose ether or starch ether starting material is suspended in a suspension medium for the oxidative degradation, and the suspension medium is a C.sub.1 -C.sub.6 alcohol, an ether, a ketone or an aqueous mixture thereof. ### Claim 20 (depends on 19) The process as claimed in claim 19, wherein the suspension comprising the cellulose ether or starch ether starting material is a slurry, said suspension medium being a slurrying medium, and wherein the weight ratio of slurrying medium to cellulose ether or starch ether starting material is from 1:1 to 5:1. ### Claim 21 (depends on 19) The process as claimed in claim 19, wherein the weight ratio of suspension medium to cellulose ether or starch ether starting material is from 6:1 to 25:1. ### Claim 22 (depends on 1) The process as claimed in claim 1, wherein, if water is present in the reaction mixture during the oxidative degradation, the water content of the reaction mixture during the oxidative degradation does not exceed 30% by weight. ### Claim 23 (depends on 1) The process as claimed in claim 1, wherein the oxidative degradation is carried out in a slurrying medium, and wherein the slurrying medium is removed by distillation after the end of the oxidative degradation. ### Claim 24 (depends on 1) The process as claimed in claim 1, wherein the cellulose ether or starch ether starting material has an average molecular mass greater than 10,000 g/mol and is relatively high in molecular weight by comparison to the product of said oxidative degradation, said relatively high molecular weight cellulose ether or starch ether having been obtained from a cellulose either or starch by alkali treatment and etherification in an etherification reaction mixture, and wherein the resulting relatively high molecular weight cellulose either or starch ether obtained from said alkali treatment and etherification is subjected to said oxidative degradation without isolation of the relatively high molecular weight cellulose either or starch ether from said etherification reaction mixture.