• 专利标题:   Hybrid material used for drinking water, prepared by preparing carboxyl functional ferric oxide magnetic nanoparticle microsphere, graphene oxide acyl chloride, and magnetic functionalized graphene oxide, and ultrasonic dispersing.
  • 专利号:   CN102977247-A, CN102977247-B
  • 发明人:   LI P, LI Y, HUANG Y, XU Y, ZHANG J
  • 专利权人:   UNIV TIANJIN POLYTECHNIC
  • 国际专利分类:   B01J020/26, B01J020/28, B01J020/30, C08F002/44, C08F212/36, C08F220/06, C08J009/26, C08K003/04, C08K003/22, C08K009/12
  • 专利详细信息:   CN102977247-A 20 Mar 2013 C08F-212/36 201376 Pages: 9 Chinese
  • 申请详细信息:   CN102977247-A CN10541368 12 Dec 2012
  • 优先权号:   CN10541368

▎ 摘  要

NOVELTY - A hybrid material is prepared by using pyrolysis method to obtain carboxyl functional ferric oxide (Fe3O4) magnetic nanoparticle microsphere; preparing graphene oxide acyl chloride; preparing magnetic functionalized graphene oxide; and adding vacuum dried magnetic functionalized graphene oxide, acetonitrile, estrogen, methacrylic acid, and divinylbenzene, sealing, ultrasonic dispersing, polymerizing, reacting with azobisisobutyronitrile, washing with ethanol, modifying with mixed solution of glacial acetic acid and ethanol, washing estrogen extract, and vacuum drying. USE - Hybrid material used for drinking water in removal of estrogen (claimed). ADVANTAGE - The method is reasonable and easy to implement, has strong magnetic response scheduling, identifying, and practicability, greatly improves efficiency of molecular imprinting technique, and widens the range of molecular imprinting. The material for removal of endocrine disruptors has good chemical stability, repetition, and identification, and is easy for active adsorption. DETAILED DESCRIPTION - A hybrid material is prepared by dissolving 125 millimole sodium hydroxide (NaOH) in 50 ml diethylene glycol at 120 degrees C for 1 hour under nitrogen pressure to obtain mixed solution, incubating mixed solution at 70 degrees C, dissolving 20-50 millimole polyacrylic acid and 20-50 millimole iron (III) chloride hexahydrate into 40-80 diethylene glycol at 220 degrees C for 45 minutes under nitrogen pressure, adding 20-40 ml incubated solution, continuously reacting at 220 degrees C for 2 hours, washing 3 times with ethanol, and vacuum drying to obtain carboxyl functional Fe3O4 magnetic nanoparticle microsphere; mixing 1-3 g graphite and 1.5 g sodium nitrate in an ice water bath at less than 4 degrees C, adding 40-70 ml 98% sulfuric acid, slowly adding 6-12 g potassium permanganate, heating at 35 degrees C, stirring for 2-4 hours, adding 138 ml distilled water, cooling for 15 minutes, adding 200-600 ml water for two times, adding 3-5 ml 30% hydrogen peroxide, standing for 10 minutes, adding with 10% hydrochloric acid, centrifuging, washing with distilled water, vacuum drying for 12 hours to obtain oxidized graphite alkene, adding 0.1-0.3 g vacuum dried oxidized graphite alkene, adding 5 g NaOH and 5 g sodium chlorate in 200 ml beaker, ultrasonic dispersing for 1-2 hours, standing to precipitate, washing three times with ethanol, vacuum drying to obtain carboxylated graphene oxide, ultrasonic dispersing 0.5-1 g vacuum dried carboxylated graphene oxide with mixed solution of 50 ml thionyl chloride and 10 ml benzene at 50 degrees C under nitrogen pressure, refluxing for 12-24 hours, reacting product with tetrahydrofuran, washing three times with ethanol, and vacuum drying to obtain graphene oxide acyl chloride; ultrasonic dispersing 15-50 mg graphene oxide acyl chloride into 50 ml dimethyl formamide (DMF), deoxygenating, adding 5 ml 5-25 mg/L carboxyl functional Fe3O4 magnetic nanoparticle microsphere and 2-5 ml triethylamine, reacting at room temperature for 24 hours, washing product with DMF, washing 3 times with ethanol, and vacuum drying at 60 degrees C to obtain magnetic functionalized graphene oxide; and adding 100-300 mg magnetic functionalized graphene oxide, 45 ml acetonitrile, 1-4 millimole estrogen, 6-10 millimole methacrylic acid, and 20-40 millimole divinylbenzene into 250 ml three-necked flask, sealing, ultrasonic dispersing with nitrogen gas except for oxygen gas for 10 minutes, placing in water bath at constant temperature, polymerizing at 50-70 degrees C, adding 5 ml 5 mg/ml azobisisobutyronitrile into sealed system, reacting for 24 hours with acetonitrile, washing three times with ethanol, modifying with 200 ml mixed solution of glacial acetic acid and ethanol with volume ratio of 2:8, washing estrogen extract, and vacuum drying.