# US 11,898,095 B2 · Crosslinking of cellulose fibers > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,898,095 B2 - Document ID: US11898095B2 - Status: Granted - Kind: B2 - Application number: 17/818,129 - Filed: 2022-08-08 - Published: 2022-12-22 - Granted: 2024-02-13 - Earliest claimed: 2016-10-12 - Assignees: Schlumberger Technology Corporation - Applicants: Schlumberger Technology Corporation - Inventors: Giselle Refunjol; Jazmin Godoy-Vargas; Mohan Kanaka Raju Panga - Web page: https://patentgrep.com/patent/US11898095B2 ## CPC - C09K 8/035: Organic additives - C09K 8/685: {containing cross-linking agents} - C09K 2208/08: Fiber-containing well treatment fluids - C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE ## Abstract Methods of treating a subterranean formation include forming a treatment fluid including a hydrophilic fiber coated with a water soluble polymer and a crosslinking agent. ## Claims ### Claim 1 A method of treating a subterranean formation, the method comprising: forming a treatment fluid, comprising: at least one hydrophilic, pulp cellulose-based fiber, wherein an outer wall of the at least one hydrophilic, pulp cellulose-based fiber is coated with a water soluble polymer comprising carboxymethylcellulose, and the at least one hydrophilic, pulp cellulose-based fiber is dried after being coated with the water soluble polymer; and at least one crosslinking agent tetraethylenepentamine; and placing the treatment fluid in the subterranean formation. ### Claim 2 (depends on 1) The method of claim 1, wherein the at least one hydrophilic, pulp cellulose-based fiber comprises a pulp cellulose fiber, a powdered cellulose fiber, a microfibrillated cellulose fiber, a nanofibrillated cellulose fiber, a nanocrystalline cellulose fiber, or a combination thereof. ### Claim 3 (depends on 1) The method of claim 1, wherein a ratio between a length of the at least one hydrophilic, pulp cellulose-based fiber and a width of the at least one hydrophilic, pulp cellulose-based fiber is between about 5 and about 1000. ### Claim 4 (depends on 1) The method of claim 1, wherein the water soluble polymer comprises a polysaccharide, a polyelectrolyte, a non-charged polymer, or a combination thereof. ### Claim 5 (depends on 1) The method of claim 1, wherein the amount of the water soluble polymer used in the treatment fluid is from about 0.6 mg per gram of the at least one hydrophilic, pulp cellulose-based fiber added to 120 mg per gram of the at least one hydrophilic, pulp cellulose-based fiber added. ### Claim 6 (depends on 1) The method of claim 1, wherein the water soluble polymer comprises a resin. ### Claim 7 (depends on 6) The method of claim 6, wherein the resin comprises a polyamideamine-epichlorohydrin (PAE) resin, a formaldehyde resin, an epoxide resin, an aldehyde resin, or a combination thereof. ### Claim 8 (depends on 1) The method of claim 1, wherein the water soluble polymer is modified or functionalized. ### Claim 9 A treatment fluid comprising: at least one hydrophilic, pulp cellulose-based fiber, wherein an outer wall of the at least one hydrophilic, pulp cellulose-based fiber is coated with a water soluble polymer comprising carboxymethylcellulose, and the at least one hydrophilic, pulp cellulose-based fiber is dried after being coated with the water soluble polymer; and at least one crosslinking agent comprising tetraethylenepentamine. ### Claim 10 (depends on 9) The treatment fluid of claim 9, further comprising a powdered cellulose fiber, a microfibrillated cellulose fiber, a nanofibrillated cellulose fiber, a nanocrystalline cellulose fiber, or a combination thereof. ### Claim 11 (depends on 9) The treatment fluid of claim 9, wherein a ratio between a length of the at least one hydrophilic, pulp cellulose-based fiber and a width of the at least one hydrophilic, pulp cellulose-based fiber is between about 5 and about 1000. ### Claim 12 (depends on 9) The treatment fluid of claim 9, wherein an amount of the water soluble polymer in the treatment fluid is from about 0.6 mg per gram of the hydrophilic, pulp cellulose-based fiber added to 120 mg per gram of the hydrophilic, pulp cellulose-based fiber added. ### Claim 13 (depends on 9) The treatment fluid of claim 9, wherein the at least one crosslinking agent further comprises glutaraldehyde, glyoxal, a zinc-based compound, a zirconium-based compound, or a combination thereof. ### Claim 14 (depends on 9) The treatment fluid of claim 9, wherein the at least one hydrophilic, pulp cellulose-based fiber is dried before being coated with the water soluble polymer. ### Claim 15 (depends on 9) The treatment fluid of claim 9, wherein the at least one crosslinking agent comprises a delay agent. ### Claim 16 (depends on 9) The treatment fluid of claim 9, wherein the at least one hydrophilic, pulp cellulose-based fiber is dried into one or more sheets, one or more pellets, or both, and subsequently added to an aqueous medium. ### Claim 17 (depends on 9) The treatment fluid of claim 9, comprising a three-dimensional polymerized structure having a plurality of coated fibers cross-linked via the at least one crosslinking agent, wherein each of the plurality of coated fibers comprises: the hydrophilic, pulp cellulose-based fiber; and a dried coating disposed on the outer wall of the hydrophilic, pulp cellulose-based fiber, wherein the dried coating comprises the water soluble polymer comprising the carboxymethylcellulose. ### Claim 18 A treatment fluid comprising: a hydrophilic fiber network comprising a plurality of coated fibers cross-linked via at least one crosslinking agent comprising tetraethylenepentamine, wherein each of the plurality of coated fibers comprises: a hydrophilic, pulp cellulose-based fiber; and a dried coating disposed on an outer wall of the hydrophilic, pulp cellulose-based fiber, wherein the dried coating comprises a water soluble polymer comprising carboxymethylcellulose. ### Claim 19 (depends on 18) The treatment fluid of claim 18, comprising a carboxyl activating agent including N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC). ### Claim 20 (depends on 18) The treatment fluid of claim 18, wherein the hydrophilic fiber network is configured to bridge fractures within a subterranean formation.