• 专利标题:   Solid-phase micro-extraction probe based on functionalized alkenyl-modified graphene-nanosiloxane polymer coating is a kind of modified graphene oxide containing ethylenic functional groups.
  • 专利号:   CN112870763-A, CN112870763-B
  • 发明人:   QI G
  • 专利权人:   UNIV FUZHOU
  • 国际专利分类:   B01D015/20, B01J020/26, B01J020/30
  • 专利详细信息:   CN112870763-A 01 Jun 2021 B01D-015/20 202156 Pages: 13 Chinese
  • 申请详细信息:   CN112870763-A CN10209323 25 Feb 2021
  • 优先权号:   CN10209323

▎ 摘  要

NOVELTY - Solid-phase micro-extraction probe based on functionalized alkenyl-modified graphene-nanosiloxane polymer coating is a kind of modified graphene oxide containing ethylenic functional groups and polysiloxane containing nano-cage structure as functional monomers, and binary solvent system as porogen. The one-pot method on the surface-modified sulfhydryl stainless steel wire realizes photo-initiated free radical polymerization. The thiol-ene bond is synchronized with the sulfhydryl group modified on the surface of the stainless steel wire, and the resulting polymer is immobilized by ''mercapto-ene'' click chemistry. USE - Solid-phase micro-extraction probe based on functionalized alkenyl-modified graphene-nanosiloxane polymer coating. ADVANTAGE - The prepared micro-extraction probe supports the modified graphene through the rigid skeleton of polysiloxane monomer, which effectively prevents the aggregation of graphene and realizes the stable distribution of graphene. The prepared polymer coating has a large specific surface, delocalized pi-pi bond and strong hydrophobicity. The preparation operation is simple, the cycle time is short (5 minutes), the probe has good adsorption performance for volatile aromatic organic pollutants in environmental water, and can provide good pretreatment materials and technical support for environmental analysis. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is included for a method for preparing a solid-phase microextraction probe functionalized based on alkenyl-modified graphene-nanosiloxane polymer coating, which involves: (A) dispersing graphene oxide in deionized water under ultrasonic action, and ultrasonically treating for 1 hour, and adding methacryloxypropyltrimethoxysilane dropwise to the above graphene oxide solution within 0.5 hours under ultrasonic conditions, and continue to mechanically stirring at 25 degrees C for 24 hours to obtain graphene oxide functionalized with alkenyl groups on the surface; (B) treating the stainless steel wire with hydrofluoric acid at 70 degrees C for 5 minutes to form a rough surface, then using deionized water, ethanol, and deionized water in an ultrasonic machine for 15 minutes and drying naturally; (C) dissolving silver nitrate (AgNO3) and glucose in distilled water respectively, slowly dropping 28% ammonia in the AgNO3 solution to form silver oxide (Ag2O) precipitation, continue to dripping 2.8% ammonia until the precipitate is just completely dissolved, and pouring into the prepared glucose solution; (D) inserting the stainless steel wire into the above solution and react for 3 hours to form a silver-plated stainless steel wire; (E) immersing the silver-plated stainless steel wire in 1,6 hexanedithiol ethanol solution for 24 hours to prepare the silver-plated stainless steel wire with surface modified mercapto group; (F) weighing the modified graphene oxide containing ethylenic functional groups, methyl methacrylate-based cage oligomeric silsesquioxane, n-propanol and polyethylene glycol PEG400, 2,2 dimethoxy 2 Phenylacetophenone in a centrifuge tube, and ultrasonic mixing for 2 minutes to form a uniform polymerization reactant solution; (G) immersing the stainless steel wire into the solution, then pulling it out and putting it into the ultraviolet (UV) crosslinker steadily, and synthesizing modified graphene-polysiloxane coating by ''one-pot method'' in-situ photopolymerization at 365 nanometer wavelength for 5 minutes; and (H) washing the coating with ethanol and dried in the GC injection port under 250 degrees C dinitrogen (N2) atmosphere for 12 hours.