• 专利标题:   Preparing fluorescence magnetic oxidized graphene 4-chlorophenol molecularly imprinted polymer comprises e.g. preparing oxidized graphene, preparing magnetic graphene oxide, and preparing cadmium telluride quantum dot, and post-processing.
  • 专利号:   CN106084232-A, CN106084232-B
  • 发明人:   HAN S, JIANG H, CHENG H, YUAN X, WANG Y
  • 专利权人:   UNIV QIQIHAR, UNIV QIQIHAR
  • 国际专利分类:   B01J020/26, B01J020/28, B01J020/30, C02F001/28, C02F101/36, C08G077/26, C08J009/26, C08K003/04, C08K003/30, C08K009/02, C09K011/88, G01N021/64, G01N030/02, H01F001/42
  • 专利详细信息:   CN106084232-A 09 Nov 2016 C08G-077/26 201715 Pages: 11 Chinese
  • 申请详细信息:   CN106084232-A CN10597454 27 Jul 2016
  • 优先权号:   CN10597454

▎ 摘  要

NOVELTY - Preparing fluorescence magnetic oxidized graphene 4-chlorophenol molecularly imprinted polymer comprises e.g. (i) preparing oxidized graphene, (ii) preparing magnetic graphene oxide, (iii) preparing cadmium telluride quantum dot, and then purifying, (iv) dispersing step (iii) obtained product ultrasonically in polyethylene glycol solution, reacting, then adding step (ii) obtained product and ethanol, stirring, and adding 3-aminopropyltriethoxysilane and 4-chlorophenol dissolved in ethanol, adding tetraethyl orthosilicate and aqueous ammonia, mechanical stirring, ultrasonicating, and washing. USE - Fluorescence magnetic oxidized graphene 4-chlorophenol molecularly imprinted polymer is useful in fluorescence detection of 4-chlorophenol (claimed). ADVANTAGE - Fluorescence magnetic oxidized graphene 4-chlorophenol molecularly imprinted polymer has low detection limit, and high extraction capacity. DETAILED DESCRIPTION - Preparing fluorescence magnetic oxidized graphene 4-chlorophenol molecularly imprinted polymer comprises (i) adding 23 ml 98% sulfuric acid into three necked flask, cooling to 4 degrees C or lower in ice bath, mechanical stirring, adding 1 g natural graphite flake and 0.5 g sodium nitrate, stirring for 1 hour, and adding 3 g potassium permanganate, controlling temperature of reaction solution at 10-15 degrees C, stirring for 2 hours, raising temperature of reaction solution to 35 degrees C, and reacting for 30 minutes, adding 80 ml deionized water, raising temperature to 95 degrees C, and reacting for 30 minutes, color of reaction solution becomes golden yellow, then adding 60 ml deionized water, 30% hydrogen peroxide with stirring, filtering, washing the filtrate using 5% hydrochloric acid and deionized water until no sulfate ions are present, and then washing with distilled water to neutral, after 40 minutes, carrying out ultrasonic stripping, and drying yellow precipitate for 48 hours to obtain oxidized graphene, (ii) dispersing step (i) obtained 0.5 g oxidized graphene powder in 120 ml ethylene glycol, ultrasonicating for 2 hours to obtain oxidized graphene dispersion, adding 0.25 g iron(III) chloride hexahydrate and 0.5 g anhydrous sodium acetate, mechanical stirring for 30 minutes, adding solution into stainless steel reactor, then crystallizing at 200 degrees C for 48 hours, washing obtained product with ethanol many times, drying under vacuum at 60 degrees C for 24 hours to obtain magnetic graphene oxide, (iii) mixing 25.5 mg tellurium powder and 30.3 mg sodium borohydride, and adding into reagent bottle containing 2 ml water under nitrogen atmosphere, and then ultrasonicating for 30 minutes to obtain aqueous sodium hydrogen telluride, then dissolving 0.2 mmol cadmium chloride in 100 ml water, carrying out ultrasonic dissolution, and adding 40 mu l thioglycolic acid and adding 0.5 mol/l sodium hydroxide solution to adjust pH value of solution to 9, adding 2 ml sodium hydrogen telluride dissolved in water under nitrogen atmosphere, magnetic stirring, and heating to reflux at 90 degrees C for 30 minutes to obtain cadmium telluride quantum dot solution, adding isopropanol, when there is a small particle suspension stop adding isopropanol, stirring for 15 minutes, placing resulting turbid liquid in ice water bath, until small particles and upper liquid separate, removing supernatant, and releasing lower turbidity liquid, and drying in oven, until all liquid evaporates to obtain purified cadmium telluride quantum dots, (iv) dispersing 0.2-2 g step (iii) obtained product ultrasonically in 0.05 mol/l polyethylene glycol (mPEG-SH) solution, reacting at room temperature for 12-24 hours, then adding step (ii) obtained 0.05-0.50 g graphene oxide-magnetic and 20-100 ml ethanol, mechanical stirring for 30 minutes, and adding 0.5-5 mmol 3-aminopropyltriethoxysilane and 0.2-2 mmol 4-chlorophenol dissolved in 10-80 ml ethanol solvent, then adding 0.5-5 ml tetraethyl orthosilicate, mechanical stirring, and adding 0.2-2.0 ml aqueous ammonia solution having a volume concentration of 25% and mechanical stirring for 24-48 hours, ultrasonicating reaction, and washing using methanol until no 4-chlorophenol is detected in eluate, and then drying to obtain final product. An INDEPENDENT CLAIM is also included for use method of molecularly imprinted polymers as solid phase extraction agent in removal and trace detection of 4-chlorophenol in water.