• 专利标题:   Sulfonated poly(ether ether ketone)-sulfonated graphene oxide hybrid film used for separation of carbon dioxide and methane comprises sulfonated poly(ether ether ketone) and sulfonated graphene oxide graphene oxide.
  • 专利号:   CN105694358-A, CN105694358-B
  • 发明人:   HUANG D, ZHANG Y, XIN Q, LIU H, SHUAI Y, NI Y
  • 专利权人:   UNIV TIANJIN POLYTECHNIC
  • 国际专利分类:   B01D053/22, C08J005/18, C08K003/04, C08K009/04, C08K009/06, C08L061/16
  • 专利详细信息:   CN105694358-A 22 Jun 2016 C08L-061/16 201663 Pages: 12 Chinese
  • 申请详细信息:   CN105694358-A CN10221746 08 Apr 2016
  • 优先权号:   CN10221746

▎ 摘  要

NOVELTY - Sulfonated poly(ether ether ketone)-sulfonated graphene oxide hybrid film comprises sulfonated poly(ether ether ketone) of 45-75% sulfonated degree and sulfonated graphene oxide graphene oxide in 0.92-0.98: 0.02-0.08 mass ratio. The film has thickness of 55-80 microns. USE - Sulfonated poly(ether ether ketone)-sulfonated graphene oxide hybrid film used for separation of carbon dioxide and methane (claimed). ADVANTAGE - The sulfonated poly(ether ether ketone)-sulfonated graphene oxide hybrid film has high selectivity, permeability and prepared in a simple and cost-effective manner. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is included for a method for sulfonated poly(ether ether ketone)-sulfonated graphene oxide hybrid film preparation, which involves: (A) preparing graphene oxide by using Hummers' Method which involves taking 98% concentrated sulfuric acid and placing the reaction vessel in an ice bath with vigorous stirring; (B) adding graphite sheet and sodium nitrate in the mixing process with vigorous stirring; (C) adding potassium permanganate slowly to form mixture A at not more than 20 degrees C where graphite sheet and sodium nitrate are mixed in 1-5: 1 mass ratio and graphite sheet is 2-10wt.% of concentrated sulfuric acid; (D) stirring mixture A at 1-10 degrees C for 1-5hours then placing in water bath at 20-50 degrees C and stirring for 20-60minutes; (E) adding deionized water to the mixture A slowly at temperature not more than 100 degrees C; (F) increasing water bath temperature to 70-120? for 2-8hours, pouring the reaction mixture into deionized water, followed by addition of 30% hydrogen peroxide, potassium permanganate and removing residual manganese dioxide; (G) filtering while hot, washing with 5% hydrochloric acid thoroughly and then washing with distilled water until neutral pH to obtain graphene oxide; (H) performing ultrasonic dispersion of graphene oxide in anhydrous ethanol and adding 3- (methacryloxypropyl)trimethoxysilane to graphene oxide in 1: 1-6 ratio; (I) reacting at 30-50 degrees C for 12-60 hours, washing by centrifugation and drying to yield double-modified graphene oxide; (J) performing ultrasonic dispersion of double-modified graphene oxide in acetonitrile, sodium styrene sulfonate, styrene and 2,2-azobisisobutyronitrile where sodium styrene sulfonate is monomer and 2,2'-azobisisobutyronitrile is initiator agent quality, double-modified graphene oxide and sodium styrene sulfonate are in 1: 6-18, sodium styrene sulfonate and 2,2'-azobisisobutyronitrile are in 3: 1-6 ratio, 2,2'-azobisisobutyronitrile is 1-10% by mass of sodium styrene sulfonate; (K) co-precipitating with zeolite at 80 degrees C to form polymeric sulfonic polymer layer on surface and performing distillation for 20-100 minutes; (L) centrifuging the round bottom flask by centrifugation and washing solid with deionized water; (M) drying naturally to give sulfonated graphene oxide; (N) adding sulfonated poly(ether ether ketone) of 45-75% sulfonated degree to N,N-dimethylacetamide solvent while stirring at room temperature to prepare 3-15% concentrated solution of sulfonated polyetheretherketone; (O) mixing sulfonated polyetheretherketone and sulfonated graphene oxide in 0.92-0.98: 0.02-0.08 ratio and dispersing in N-dimethylacetamide solvent for 12-36 hours; (P) stirring for 24hours, allowing to stand for 1-3hours and degassing to give sulfonated polyether ether ketone-sulfonated graphene oxide casting solution; and (Q) pouring the above solution in a glass Petri dish and drying first at 60 degrees C for 12 hours then at 80 degrees C for 12 hours to obtain a sulfonated polyether ether ketone-sulfonated graphene oxide hybrid film.