• 专利标题:   Perfluoropolyether end capping catalyst for forming inert perfluoropolyether, is carbon-based supported catalyst containing metal fluoride such as alkali metal fluoride as active component and carbon-based material carrier, where metal fluoride is loaded on surface and pores of carbon-based material.
  • 专利号:   CN115364875-A, CN115364875-B
  • 发明人:   GAO X, ZHANG J, LIU Z, LI J, LIU T, WANG J, WANG H
  • 专利权人:   SHANDONG HUAXIA SHENZHOU NEW MATERIAL CO
  • 国际专利分类:   B01J021/18, B01J027/12, B01J027/125, B01J032/00, B01J035/10, B01J037/02, C07C041/18, C07C043/12, C08G065/328, C10M105/50, C10M107/38, C10N030/06, C10N050/10
  • 专利详细信息:   CN115364875-A 22 Nov 2022 B01J-027/125 202308 Chinese
  • 申请详细信息:   CN115364875-A CN11306453 25 Oct 2022
  • 优先权号:   CN11306453

▎ 摘  要

NOVELTY - A perfluoropolyether end capping catalyst is a carbon-based supported catalyst. The active component of the catalyst, is metal fluoride and the carrier is carbon-based material. The metal fluoride is loaded on the surface and pores of the carbon-based material. USE - Perfluoropolyether end capping catalyst is used for preparing inert perfluoropolyether (claimed). ADVANTAGE - The catalyst, when added into the perfluoropolyether containing acid fluoride end groups, enables to cap the perfluoropolyether acid fluoride end groups, through decarbonylation reaction, under mild conditions. The catalyst after regeneration by decarbonylation reaction, is recovered, and is recycled by washing twice and re-calcining. DETAILED DESCRIPTION - INDEPENDENT CLAIMS are included for: 1) preparation of perfluoropolyether end capping catalyst which involves: (i) loading the active component metal fluoride on the carbon-based material by dipping, followed by drying the carbon-based material loaded with metal fluoride; (ii) placing the dried carbon base material in a tubular furnace, then performing heat treatment under inert gas atmosphere, at 150 - 300°C, to form the catalyst; 2) regeneration of the perfluoropolyether end capping catalyst which involves: (a) placing the used catalyst in a primary detergent, stirring at 25- 35°C, with speed 250- 350 rotations/minute (rpm) for at least 20 minutes, then removing the catalyst after washing once, the amount of primary detergent used by each gram of catalyst is 16-24 ml, the detergent used is trifluorotrichloroethane, hydrofluoroether or detetrafluoroethane; (b) placing the washed catalyst in secondary detergent for at least 15 minutes, filtering and separating filter residueafter washing once, the amount of secondary detergent used is 8-12 ml, the secondary detergent is trifluorotrichloroethane, hydrofluoroether or detetrafluoroethane; (c) continuously subjecting obtained filter residue to steps (a) and (b), repeatedly washing two times; (d) drying the washed catalyst and calcining in tubular furnace, again, then sieving the catalyst particles of size 100 meshes or more and recycling. The specific conditions for re-calcining involve passing inert gas as protective atmosphere continuously, setting initial temperature as 25 - 35°C, raising the temperature to 160- 200°C, at a heating rate 4- 6°C /minute, keeping for 1- 3 hours, then raising the temperature to 240-260°C, with heating rate 8-10°C, /minute, keeping for 0.5-2 hours, reducing the temperature to 25-35°C, at speed 10°C /minute; and 3) method for capping perfluoropolyether end group, by using end-capping catalyst which involves: (1) adding the catalyst to the perfluoropolyether containing the acyl fluoride end group; (2) under inert gas atmosphere, decarbonizing perfluoropolyether acyl fluoride end group at 150-200°C and terminating; (3) separating the terminated perfluoropolyether from the catalyst liquid by centrifuging or filtering.