• 专利标题:   Preparing sulfonamide antibiotic composite template molecular imprinting magnetic material useful for water sample adsorption removal and magnetic solid phase extraction, comprises e.g. preparing graphene oxide adopts improved Hummer method and magnetic graphene oxide-mesoporous silicon compound.
  • 专利号:   CN113462011-A
  • 发明人:   FAN Y, MA X
  • 专利权人:   UNIV GUANGDONG TECHNOLOGY
  • 国际专利分类:   C08F222/14, C08F212/14, C08F292/00, B01J020/30, B01J020/28, B01J020/26, C08J009/26
  • 专利详细信息:   CN113462011-A 01 Oct 2021 C08J-009/26 202102 Chinese
  • 申请详细信息:   CN113462011-A CN10732740 28 Jun 2021
  • 优先权号:   CN10732740

▎ 摘  要

NOVELTY - Preparing sulfonamide antibiotic composite template molecular imprinting magnetic material comprises (i) preparing graphene oxide (GO) adopts improved Hummer method, (ii) preparing magnetic graphene oxide (MGO) by chemical coprecipitation method for preparing magnetic magnesium oxide, (iii) preparing magnetic graphene oxide-mesoporous silicon compound (MGO-mSiO2), (iv) preparing grafting double bond magnetic graphene oxide-mesoporous silicon compound (VTTSMGO-mSiO2),(v) dispersing MGO-mSiO2 dispersed in toluene, ultrasonically reacting, adding vinyl trimethoxy silane (VTTS), introducing nitrogen and removing oxygen (10 minutes), stirring and reacting for 24 hours, and washing, and (v) dissolving sulfadiazine, sulfathiazole, sulfamethazine, sulfamethazine, sulfamethoxazole, sulfadoxine in toluene, ultrasonically processing, and collecting imprinted polymer USE - The material is useful for adsorption removal and magnetic solid phase extraction of water samples containing sulfonamide antibiotics (claimed). ADVANTAGE - The material has adsorption capacity of more than 16 mg/g. DETAILED DESCRIPTION - Preparing sulfonamide antibiotic composite template molecular imprinting magnetic material comprises (i) taking 5 g graphite powder (carbon content is more than 98 wt.%) and 2.5 g sodium nitrate under the condition of ice bath, continuously stirring, mixing in 98% concentrated sulfuric acid (250 ml), slowly adding, 35 g potassium permanganate the temperature not greater than283K, low temperature reacting for 2 hours, heat preserving at greater than or equal to283K, heat preserving at 308plus minus2K, and reacting for 2 hours, cooling to room temperature, obtaining bright yellow suspension, using 500 ml deionized water to dilute, adding hydrogen peroxide (30 %) to generate without bubble, sequentially diluting 10 times concentrated hydrogen chloride and acetone to wash the product, and vacuum drying at 80degrees Celsius, (ii) preparing magnetic graphene oxide (MGO) by chemical coprecipitation method for preparing magnetic magnesium oxide, mixing the 0.5 g graphene oxide in de-ionized water, ultrasonically processing for 30 minutes, adding 8 g ferric chloride nonahydrate and 7 g ferrous sulfate heptahydrate (ferric ion: ferrous ion has molar ratio of 1.5: 1), nitrogen and oxygen, gradually adding 25% ammonia aqueous solution until the pH of 11, stirring for 1 hours at 80degrees Celsius, cooling the solution to room temperature and collecting the sample under the action of the magnet, using de-ionized water, respectively washing by anhydrous ethanol for 3 times, vacuum drying the collected MGO at 50degrees Celsius, grinding and putting into a drier, (iii) preparing the magnetic graphene oxide-mesoporous silicon compound (MGO-mSiO2): mixing 0.5 g MGO, 1.5 g hexadecyl trimethyl ammonium bromide (CTAB) and 100 ml de-ionized water, and ultrasonically processing the mixture for 30 minutes, adding 250 ml absolute ethyl alcohol and 5 ml 30% aqueous ammonia into the solution, ultrasonically processing for 10 minutes, gradually adding 4 ml tetraethoxysilane (TEOS) under the mechanical stirring condition, reacting for 24 hours under the room temperature condition, collecting the material, using absolute ethyl alcohol to wash for not less than3 times, removing cetrimonium bromide using 1% ammonium nitrate-ethanol mixed solution as solvent, condensing and refluxing for 24 hours at 60degrees Celsius, using absolute ethyl alcohol to wash for 3 times, and vacuum drying at 60degrees Celsius, (iv) dispersing 0.5 g MGO-mSiO2 dispersed in 50 ml toluene, ultrasonically reacting for 60 minutes, adding 10 ml vinyl trimethoxy silane (VTTS), introducing nitrogen and removing oxygen (10 minutes), stirring and reacting for 24 hours, washing the collected product with toluene for 3 times with magnet under the condition of 50degrees Celsius, drying for 24 hours at 50degrees Celsius under vacuum condition to obtain the modified double bond MGO-mSiO2 (VVTS-MGO-mSiO2), (v) dissolving sulfadiazine, sulfathiazole, sulfamethazine, sulfamethazine, sulfamethoxazole, sulfadoxine 21, 22, 23, 21, 26, 21 mg, respectively in 50 ml toluene, ultrasonically processing for 15 minutes, adding 221 mg 4-vinylbenzoic acid, ultrasonically processing for 15 minutes, and placing in a gas bath shaker and shaking at 200 revolutions/minute for 8 hours under 15degrees Celsius, adding 300 mg MGO-SiO2, 471 mul ethylene glycol dimethacrylate, and 50 mg 2,2'-azobisisobutyronitrile, ventilating nitrogen to remove oxygen, stirring mechanically at revolutions/minute in a 60degrees Celsius water bath for 24 hours, collecting the imprinted polymer obtained by applying an external magnetic field, washing twice with methanol, eluting the polymer with a methanol and acetic acid (9:1, V:V) mixed solution at 25degrees Celsius until no template molecules can be detected in the high-performance liquid chromatography, washing polymer for many times with methanol and drying under vacuum at 50degrees Celsius for 24 hours. An INDEPENDENT CLAIM is also included for use method of magnetic material for adsorption removal and magnetic solid phase extraction of water samples containing sulfonamide antibiotics, comprising (a) adding 20 mg material to 50 ml water sample containing a specific concentration of sulfonamide antibiotics, adjusting the pH to 7, and oscillating and absorbing in a constant temperature oscillator at 200 revolutions/minute for 15 minutes, and (b) separating the magnetic material with sulfonamide antibiotics from the solution using a magnet, adding 2 ml methanol, shakingf elution and eluting at 200 revolutions/minute in a constant-temperature oscillator for 6 minutes, performing magnetic separation, and collecting the eluate, and (c) measuring the concentration of sulfonamide antibiotics in the eluent with high performance liquid chromatography.