# US 6,702,965 B2 · Method of forming a porous composite product, in particular with a high specific surface > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 6,702,965 B2 - Document ID: US6702965B2 - Status: Granted - Kind: B2 - Application number: 09/957,573 - Filed: 2001-09-20 - Published: 2002-09-26 - Granted: 2004-03-09 - Earliest claimed: 1997-02-06 - Assignees: Bollore - Inventors: Jean-François Penneau; François Capitaine; Philippe Le Goff - Web page: https://patentgrep.com/patent/US6702965B2 ## CPC - B01D 67/003: {by selective elimination of components, e.g. by leaching} - B01D 69/02: characterised by their properties - B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes - B01J 20/26: Synthetic macromolecular compounds - B01J 20/28014: {characterised by their form} - B01J 20/28026: {Particles within, immobilised, dispersed, entrapped in or on a matrix, e.g. a resin} - B01J 20/2803: {Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products} - B01J 20/28033: {Membrane, sheet, cloth, pad, lamellar or mat} - B01J 20/28057: {Surface area, e.g. B.E.T specific surface area} - B01J 20/28078: {Pore diameter} - B29C 48/022: {characterised by the choice of material} - C08J 9/0066: {Use of inorganic compounding ingredients} - C08J 9/26: by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out - C08L 71/02: Polyalkylene oxides - C25B 11/031: Porous electrodes - H01G 11/38: Carbon pastes or blends; Binders or additives therein - H01G 11/86: specially adapted for electrodes (carbonisation or activation of carbon for the manufacture of electrodes H01G11/34) - H01M 4/00: Electrodes - H01M 4/8605: {Porous electrodes} - H01M 4/96: Carbon-based electrodes - B01D 2323/10: Specific pressure applied - B01D 2323/12: Specific ratios of components used - B29C 48/08: flexible, e.g. films - C08J 2201/046: Elimination of a polymeric phase - Y02E 60/13: Energy storage using capacitors - Y02E 60/50: Fuel cells - Y10T 428/249953: Composite having voids in a component [e.g., porous, cellular, etc.] - Y10T 428/249978: Voids specified as micro - Y10T 428/249986: Void-containing component contains also a solid fiber or solid particle - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00) - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) - C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B) - H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10) - H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract A process for the preparation of a porous composite product. The process steps are forming a homogeneous mixture having one or more insoluble polymers, one or more soluble or calcinable polymers and one or more fillers, in particular with a high specific surface; extruding the mixture to form an extruded precursor product; removing the soluble or calcinable polymer or polymers from the extruded precursor product, in order to form pores, and recovering the porous composite product. ## Claims ### Claim 1 Process for the preparation of a porous composite product, comprising the steps of: a) forming a homogeneous mixture having one or more insoluble polymers, one or more soluble or calcinable polymers and at least 20% by weight of one or more fillers exhibiting a BET specific surface greater than 1000 m2/g, b) extruding said mixture to form an extruded precursor product, c) removing the soluble or calcinable polymer or polymers from the extruded precursor product, in order to form pores, d) recovering the porous composite product, the product exhibiting a BET specific surface greater than 10 m2/g. ### Claim 2 (depends on 1) Preparation process according to claim 1, characterized in that the removal of stage c) is carried out by bringing the extruded precursor product into contact with an appropriate solvent. ### Claim 3 (depends on 2) Preparation process according to claim 2, wherein the appropriate solvent is water. ### Claim 4 (depends on 2) Preparation process according to claim 2, wherein the removal of stage c) is carried out by subjecting the extruded precursor product to a calcination. ### Claim 5 (depends on 1) Preparation process according to claim 1, wherein step b) comprises: i) forming granules, ii) forming a film. ### Claim 6 (depends on 5) Preparation process according to claim 5, wherein step i) is carried out in a corotating twin screw extruder and step ii) is carried out in a single screw extruder. ### Claim 7 (depends on 1) Preparation process according to claim 1, characterized in that stage a) is carried out by means of a mixer of a twin-screw extruder, ensuring homogeneous mixing of the polymers and of the fillers. ### Claim 8 (depends on 1, 2, 3, 4, 5, 6, 7) Preparation process according to one of claims 1, 2, 3, 4, 5, 6 or 7, characterized in that the insoluble polymer/soluble or calcinable polymer ratio by weight is between 0.1 and 5. ### Claim 9 (depends on 8) Preparation process according to claim 8, wherein the insoluble polymer/soluble polymer or calcinable polymer ratio by weight is between 0.1 and 2. ### Claim 10 (depends on 2, 3, 4, 5, 6, 7) Preparation process according to claim 2, 3, 4, 5, 6 or 7, wherein after the recovering step d), the porous composite product is wound. ### Claim 11 (depends on 3) Preparation process according to claim 3, wherein the precursor product is immersed in water for a residence time of about 5 minutes. ### Claim 12 (depends on 2) Preparation process according to claim 2, wherein the precursor product is then dried at 40° C. for 1 hour. ### Claim 13 (depends on 1, 3) Preparation process according to claims 1 and 3, wherein step a) and i) are carried out simultaneously by means of an extruder. ### Claim 14 (depends on 5) Preparation process according to claim 5, wherein step i) is carried out with a throughput comprised between 1.8 and 34 kg/h. ### Claim 15 (depends on 5) Preparation process according to claim 5, wherein step ii) is carried out with a throughput comprised between 2 and 2.5 kg/h. ### Claim 16 (depends on 5) Preparation process according to claim 5, wherein steps i) and ii) are carried out with a die pressure comprised between 8 and 17.5 MPa. ### Claim 17 Process for the preparation of a porous composite product comprising the steps of: a) forming a homogeneous mixture having one or more insoluble polymers, one or more soluble or calcinable polymers and one or more fillers, b) extruding said mixture to form an extruded precursor product, c) removing the soluble or calcinable polymer or polymers from the extruded precursor product, in order to form pores, d) recovering the porous composite product, the product exhibiting a BET specific surface greater than 10 m2/g, wherein the removal of stage c) is carried out by subjecting the extruded precursor product to a calcination. ### Claim 18 Process for the preparation of a porous composite product comprising the steps of: a) forming a homogeneous mixture having one or more insoluble polymers, one or more soluble or calcinable polymers and one or more fillers, b) extruding said mixture to form an extruded precursor product, c) removing the soluble or calcinable polymer or polymers from the extruded precursor product, in order to form pores, d) recovering the porous composite product, the product exhibiting a BET specific surface greater than 10 m2/g, wherein step b) comprises: i) forming granules in a corotating twin screw extruder, ii) forming a film in a single screw extruder.