• 专利标题:   Removing endocrine disrupters in water by activating persulfate under synergic catalytic actions of metal cerium and magnetic reduced graphene oxide comprises e.g. mixing persulfate with pretreated water, and adjusting pH of the reaction.
  • 专利号:   CN104628211-A, CN104628211-B
  • 发明人:   CHENG X, GUO H, SHI B, ZHANG Y, LIANG D
  • 专利权人:   UNIV SICHUAN
  • 国际专利分类:   B01J023/10, C02F009/12
  • 专利详细信息:   CN104628211-A 20 May 2015 C02F-009/12 201603 Pages: 11 Chinese
  • 申请详细信息:   CN104628211-A CN10073688 11 Feb 2015
  • 优先权号:   CN10073688

▎ 摘  要

NOVELTY - Removing endocrine disrupters in water by activating persulfate under synergic catalytic actions of metal cerium and magnetic reduced graphene oxide comprises (i) mixing persulfate with pretreated water, (ii) adjusting the pH of the reaction, (iii) preparing metallic cerium/magnetic reduced graphene oxide composite material, (iv) adjusting the pH of the metallic cerium/magnetic reduced graphene oxide composite material, and (v) separating the metal cerium/magnetic reduced graphene oxide composite material by using an external field, recycling, filtering, and drying. USE - The method is useful for removing endocrine disrupters in water by activating persulfate under synergic catalytic actions of metal cerium and magnetic reduced graphene oxide (claimed). ADVANTAGE - The method achieves 89-9% removal rate of endocrine disrupters in water. DETAILED DESCRIPTION - Removing endocrine disrupters in water by activating persulfate under synergic catalytic actions of metal cerium and magnetic reduced graphene oxide comprises (i) mixing persulfate with pretreated water, stirring at room temperature at a speed of 160-250 rotations/minute for 20-45 minutes to obtain a mixed solution of persulfate and pretreated water, where the concentration of endocrine disruptors in pretreated water is 0.02-100 mg/l, and the mass ratio of persulfate and pretreated water is 1:(1000-10000), (ii) adjusting the pH of the reaction: using 0.1-100 mol/l perchloric acid and 0.1-100 mol/l sodium hydroxide solution and stirring at stirring speed of 150-200 rpm to adjust the pH of the mixed solution to obtain pH adjusted mixed solution containing persulfate and pretreated water, (iii) preparation of metallic cerium/magnetic redox graphene composite material by (a) adding graphene oxide to 97-99% ethylene glycol solution, using an ultrasonic vibration analyzer for vibrating and dispersing for 3-4 hours to give mixed solution of graphene oxide and ethylene glycol, where the volume ratio of the graphene oxide and 97-99 wt.% ethylene glycol solution is (0.001-10 g):1 ml, (b) heating a mixed solution of sodium citrate and ethylene glycol at a temperature of 60-75 degrees C for 20-45 minutes to obtain heated mixed solution of sodium citrate and ethylene glycol, adding iron(iii) chloride hexahydrate, urea and cerium chloride hexahydrate to the resulting heated mixed solution, magnetically stirring at room temperature at the speed of 100-250 rpm for 2-4 hours to obtain mixed solution containing iron-cerium of sodium citrate and ethylene glycol, where the concentration of the sodium citrate in the mixed solution of sodium citrate and ethylene glycol is 60-200 mg/ml, the volume mass ratio of the mixed solution of sodium citrate and ethylene glycol and iron(iii) chloride hexahydrate is 1-1000 ml:1 g, the mass ratio of iron(iii) chloride hexahydrate and urea is (0.01-100):1, and the mass ratio of iron(iii) chloride hexahydrate and cerium chloride hexahydrate is (0.01-1000):1, (c) mixing the mixed solution of graphene oxide and ethylene glycol and mixed solution containing iron-cerium of sodium citrate and ethylene glycol, adding to a stainless steel high-pressure reaction kettle with polytetrafluoroethylene liner, sealing the high-pressure reaction kettle, reacting in the high-pressure reaction kettle at temperature of 200-230 degrees C for 12 h-48 hours, cooling to room temperature to obtain black suspension, where the volume ratio of the mixed solution of graphene oxide and ethylene glycol and mixed solution containing iron-cerium of sodium citrate and ethylene glycol is (0.1-50):1, and (d) centrifuging the black suspension at a speed of 6500-8000 rpm for 10-30 minutes, taking the precipitate after centrifugation, respectively, washing the precipitate with methanol and deionized water for 5-10 times, placing at -18 degrees C to -15 degrees C and then drying at temperature of 24-48 hours to obtain the metallic cerium/ magnetic redox graphene composite material, (iv) adjusting the pH of the metallic cerium/magnetic reduced graphene oxide composite material by adding mixed solution of persulfate and pre-treated water, and reacting for 15-240 minutes to obtain aqueous metallic cerium/ magnetic redox graphene composite material, where the content of the metallic cerium/magnetic reduced graphene oxide composite material is 1-200 mg/l, and (v) separating the metal cerium/magnetic reduced graphene oxide composite material by using an external field, recycling the metallic cerium/magnetic redox graphene composite material, filtering the recycled composite material using glass fiber membrane with pore size of 0.45 mu m, drying the filtered composite material at temperature of 50-75 degrees C for 12-48 hours to obtain regenerated metallic cerium/magnetic redox graphene composite material, and removing endocrine disrupters in water.