# US 9,752,062 B2 · Switchable adhesive and objects utilizing the same > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,752,062 B2 - Document ID: US9752062B2 - Status: Granted - Kind: B2 - Application number: 14/722,381 - Filed: 2015-05-27 - Published: 2015-09-10 - Granted: 2017-09-05 - Earliest claimed: 2009-08-17 - Assignees: Interface International B.V. - Applicants: Interface International B.V. - Inventors: John Robert Mantle; James Hanley Clark; Peter Samuel Shuttleworth - Web page: https://patentgrep.com/patent/US9752062B2 ## CPC - C09J 103/06: Esters - B32B 37/1284: {Application of adhesive} - B32B 37/18: involving the assembly of discrete sheets or panels only - B32B 38/00: Ancillary operations in connection with laminating processes - B32B 38/10: Removing layers, or parts of layers, mechanically or chemically - C08B 31/04: of organic acids {, e.g. alkenyl-succinated starch} - C09J 5/00: Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers - C09J 11/06: organic - D06N 7/0071: {characterised by their backing, e.g. pre-coat, back coating, secondary backing, cushion backing} - B32B 37/12: characterised by using adhesives - B32B 2471/02: Carpets - C09J 2403/00: Presence of starch - D06N 2209/067: Flame resistant, fire resistant - D06N 2213/068: Releasability between at least two of the layers - Y10T 428/23979: Particular backing structure or composition - C09J: ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES (preparation of glue or gelatine C09H) - B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM - 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) - D06N: WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract A carpet material with at least one of its components made easier for recycle by use of an adhesive which can be selectively altered to change the adhesion strength to allow component carpet layers to be separated. ## Claims ### Claim 1 Method for preparing a hot aqueous solvent switchable adhesive, the method comprising the steps of a. providing starch; b. subjecting the starch to hot aqueous solvent treatment in order to gelatinize the starch; c. treating the gelatinized starch to induce retrogradation in said gelatinized starch to obtain expanded starch; d. adding non-aqueous water-soluble solvent to precipitate the expanded starch, substantially separating the precipitated expanded starch from the solvent and further washing of the expanded starch with a non-aqueous water-soluble solvent until at least 90 vol. % of the aqueous solvent added under step b is removed, e. suspending the expanded starch in inert water-free organic solvent, adding of a catalyst, adding of a fatty acid anhydride and either i. keeping the mixture at a temperature and for a period of time sufficient to allow the formation of an esterified expanded starch, or ii. treating the mixture in a micro-wave oven at 100-1000 W and for a period of 1 to 10 minutes sufficient to allow the formation of an esterified expanded starch; f. adding non-aqueous water-soluble solvent to precipitate the esterified expanded starch, and drying of the esterified expanded starch; or addition of water which also facilitates precipitation of the esterified expanded starch; g. admixing a plasticizer to the esterified expanded starch, allowing the formation of a plasticized esterified expanded starch. ### Claim 2 (depends on 1) Method according to claim 1 wherein the drying of the obtained expanded starch is performed in step d. ### Claim 3 (depends on 1) Method according to claim 1 wherein the starch has an amylose content (w/w) of at least 20% or a debranced starch with a greater proportion of linear chains. ### Claim 4 (depends on 1) Method according to claim 1 wherein the gelatinized starch is obtained by hot aqueous solvent treatment at a temperature in the range of from 50° C. to 200° C. ### Claim 5 (depends on 1) Method according to claim 1 wherein retrogradation is induced by storing the hot aqueous solvent treated starch at a temperature below 25° C. but above −5° C., for at least 10 hours. ### Claim 6 (depends on 1) Method according to claim 1 wherein the non-aqueous water-soluble solvent is selected from the group consisting of ethanol, methanol, propanol, and butanol. ### Claim 7 (depends on 1) Method according to claim 1 wherein the non-aqueous water-soluble solvent is added under step d) in a ratio of from 1 volumes non-aqueous watersoluble solvent to 5 volume hot aqueous solvent added in step b) to 5 volume nonaqueous water-soluble solvent to 1 volume hot aqueous solvent added in step b). ### Claim 8 (depends on 1) Method according to claim 1 wherein after the further washing of the precipitated starch the precipitated starch is at least once washed with the inert water-free organic solvent of step e), and omitting the drying of the obtained expanded starch. ### Claim 9 (depends on 1) Method according to claim 1 wherein the inert water-free organic solvent is selected from the group consisting of toluene, benzene, and xylene. ### Claim 10 (depends on 1) Method according to claim 1 wherein the catalyst is selected from the group consisting of amines, dimethylaminopyridine (DMAP), triethylamine, and pyridine. ### Claim 11 (depends on 1) Method according to claim 1 wherein the fatty acid anhydride is from C2 fatty acid anhydride to C12 fatty acid anhydride, or mixtures thereof. ### Claim 12 (depends on 11) Method according to claim 11 wherein the fatty acid anhydride is acetic anhydride. ### Claim 13 (depends on 1) Method according to the claim 1 wherein the plasticizer is selected from the group consisting of phthalate esters, dimethyl- and diethylsuccinate, glycerol triacetate (triacetin), glycerol mono- and diacetate, glycerol mono-, di- and tripropionate, glycerol tributanoate (tributyrin), glycerol mono- and dibutanoate, glycerol mono-, di- and tristearate, and other related glycerol esters, lactic acid, esters, citric acid esters, adipic acid esters, stearic acid esters, oleic acid esters, ricinoleic acid esters, other fatty acid esters, glycerol, polycaprolactone, glyceryltrioleate. ### Claim 14 (depends on 1) Method according to claim 1 wherein the plasticizer is admixed in an amount from 10 to 40% by weight based on the esterified expanded starch. ### Claim 15 (depends on 1) Method according to claim 1 wherein further flame-retardants, fillers, preservatives, binders, antimicrobial agents are admixed to the esterified expanded starch or the plasticized esterified expanded starch. ### Claim 16 (depends on 1) Method according to claim 1 wherein the starch has an amylose content (w/w) of at least 40% or a debranched starch with a greater proportion of linear chains. ### Claim 17 (depends on 1) Method according to claim 1 wherein the starch has an amylose content (w/w) of at least 50% or a debranched starch with a greater proportion of linear chains. ### Claim 18 (depends on 1) Method according to claim 1 wherein the starch has an amylose content (w/w) of at least 60% or a debranched starch with a greater proportion of linear chains. ### Claim 19 (depends on 1) Method according to claim 1 wherein the gelatinized starch is obtained by hot aqueous solvent treatment at a temperature in the range of from 70° C. to 160° C. ### Claim 20 (depends on 1) Method according to claim 1 wherein the gelatinized starch is obtained by hot aqueous solvent treatment at a temperature in the range of from 90° C. to 130° C. ### Claim 21 (depends on 1) Method according to claim 1 wherein retrogradation is induced by storing the hot aqueous solvent treated starch at a temperature below 10° C., but above −5° C., for at least 24 hours. ### Claim 22 (depends on 1) Method according to claim 1 wherein retrogradation is induced by storing the hot aqueous solvent treated starch at a temperature below 5° C., but above −5° C., for at least 100 hours. ### Claim 23 (depends on 1) Method according to claim 1 wherein retrogradation is induced by storing the hot aqueous solvent treated starch at a temperature below 25° C., but above −5° C., for at least 500 hours. ### Claim 24 (depends on 10) Method according to claim 10 wherein the catalyst is DMAP. ### Claim 25 (depends on 1) Method according to the claim 1 wherein the plasticizer is glycerol or glycerol triacetate. ### Claim 26 (depends on 1) Method according to claim 1 wherein the plasticizer is admixed in an amount from 15 to 35% by weight based on the esterified expanded starch. ### Claim 27 (depends on 1) Method according to claim 1 wherein the plasticizer is admixed in an amount from 20 to 30% by weight based on the esterified expanded starch. ### Claim 28 (depends on 1) Method according to claim 1 wherein the fatty acid anhydride is from C2 fatty acid anhydride to C6 fatty acid anhydride.