• 专利标题:   Preparation of sulfonated carbon nanotube/graphene oxide composite catalyst for esterification of long-chain carboxylic acid and fatty alcohol, involves mixing sulfonated modified carbon nanotubes and graphite oxide and baking mixture.
  • 专利号:   CN105148990-A, CN105148990-B
  • 发明人:   DONG Y, JIANG P, ZHANG W, BIAN G, ZHENG J
  • 专利权人:   UNIV JIANGNAN
  • 国际专利分类:   B01J031/02, C07C067/08, C07C069/24
  • 专利详细信息:   CN105148990-A 16 Dec 2015 B01J-031/02 201637 Pages: 7 English
  • 申请详细信息:   CN105148990-A CN10473014 05 Aug 2015
  • 优先权号:   CN10473014

▎ 摘  要

NOVELTY - Styrene sulfonate is dissolved in distilled water. Multi-walled carbon nanotubes are added to mixture, ultrasonically processed, and potassium persulfate is added, heated, mixed, centrifuged, washed and filtered. Solid is added to concentrated hydrochloric acid, and reflux condensed, washed, and obtained solid material is baked, to obtain sulfonated modified carbon nanotubes. Sulfonated modified carbon nanotubes and graphite oxide are mixed, heated, membrane filtered and baked, to obtain black solid product containing sulfonated carbon nanotube/graphene oxide composite catalyst. USE - Preparation of sulfonated carbon nanotube/graphene oxide composite catalyst used for esterification of long-chain carboxylic acid and fatty alcohol (claimed). ADVANTAGE - The method enables preparation of sulfonated carbon nanotube/graphene oxide composite catalyst having excellent catalytic characteristics by simple and economical method. DETAILED DESCRIPTION - 1-5 g Styrene sulfonate is dissolved in 100 mL distilled water. 20-100 mg Multi-walled carbon nanotubes are added to mixture, ultrasonically processed at 50 KHz using ultrasonic cleaning machine for 1-2 hours and uniformly stirred at 300-500 rpm for 3-5 hours. The stirred mixture is transferred to three-necked flask, and 0.2-1 g potassium persulfate is added and nitrogen is bubbled to remove oxygen, and the mixture is maintained for 30-60 minutes. The reaction mixture is slowly heated at 90 degrees C, uniformly stirred at 500-800 rpm for 4-6 hours, mixed, filtered in membrane filter, centrifuged, washed with deionized water for 5-8 times and filtered. Solid is added to 50 mL concentrated hydrochloric acid with concentration of 35-37.5 %mass, and reflux condensed at 70-100 degrees C for 8 hours. The resulting solution is mixed, provided to membrane filter, washed with deionized water for 5-10 times, and obtained solid material is placed in vacuum oven, baked at -0.1 MPa and 50-70 degrees C for 10 hours, to obtain sulfonated modified carbon nanotubes. 40 mg Sulfonated modified carbon nanotubes and 20-100 mg graphite oxide are mixed, and added to 100 mL ethanol, ultrasonically cleaned at 50 KHz using ultrasonic machine for 10-30 minutes, heated at 90-130 degrees C for 1-2 hours, membrane filtered and washed with deionized water for 5-10 times. The resulting solid material is placed in vacuum oven and baked at -0.1 MPa and 50-70 degrees C for 10 hours, to obtain black solid product containing sulfonated carbon nanotube/graphene oxide composite catalyst. An INDEPENDENT CLAIM is included for application of sulfonated carbon nanotube/graphene oxide composite catalyst for esterification reaction which involves esterifying long-chain carboxylic acid of formula: R1-C(=O)-OH and fatty alcohol of formula: R2-OH and dehydrating mixture, to obtain carbonyl group-containing compound of formula: R1-C(=O)-OR2 and water. R1=10C or more alkyl, double bond-containing group, benzene or substituted benzene ring;and R2=8C or more alkyl or hydroxy.