• 专利标题:   Preparing hydroxyethylidene diphosphonic acid-modified magnetic graphene oxide adsorbent comprises e.g. adding silane coupling agent, absolute ethanol and water, adding hydroxyethylidene diphosphonic acid powder and post-processing.
  • 专利号:   CN105289514-A, CN105289514-B
  • 发明人:   GE H, WU J, WANG C
  • 专利权人:   UNIV JINAN, UNIV JINAN
  • 国际专利分类:   B01J020/22, B01J020/28, B01J020/30, C02F001/28, C02F001/62
  • 专利详细信息:   CN105289514-A 03 Feb 2016 B01J-020/22 201631 Pages: 8 English
  • 申请详细信息:   CN105289514-A CN10858674 01 Dec 2015
  • 优先权号:   CN10858674

▎ 摘  要

NOVELTY - Preparing hydroxyethylidene diphosphonic acid-modified magnetic graphene oxide adsorbent comprises e.g. stirring 1-2 pts. wt. iron(III) chloride hexahydrate and ethylene glycol using a magnetic stirring to obtain graphene oxide magnetic material, and (ii) adding 1 pts. wt. silane coupling agent, 2.5-10 pts. wt. absolute ethanol and 5-20 pts. wt. water into the three-necked flask, adding 0.5-1.5 pts. wt. of hydroxyethylidene diphosphonic acid powder to the solvent, then adding 0.5-2 pts. wt. basic catalyst and 0.1-1 pts. wt. polypeptide condensing agent to solution to obtain final product. USE - The method producing product is useful in removing heavy metal ions (claimed). ADVANTAGE - The method is simple; and has high adsorption capacity, environmental protection, easy to separate and reusable. DETAILED DESCRIPTION - Preparing hydroxyethylidene diphosphonic acid-modified magnetic graphene oxide adsorbent comprises (i) stirring 1-2 pts. wt. iron(III) chloride hexahydrate and ethylene glycol using a magnetic stirring, dubbing 0.05 g/ml concentration of solution, weighing 0.05-0.2 pts. wt. graphene oxide, 10 pts ammonia, 0.05-0.3 pts polyvinylpyrrolidone, reacting mixed solution of ethylene glycol and iron(III) chloride hexahydrate, adding graphene oxide powder, stirring to obtain homogeneous mixture, then adding aqueous ammonia until the mixture stabilized, adding polyvinylpyrrolidone, placing mixture in a polytetrafluoroethylene liner autoclave, heating at 160-190 degrees C for 15-24 hours, cooling to room temperature, washing with water and ethanol 3 times, freeze-drying and grinding to obtain graphene oxide magnetic material, and (ii) adding 1 pts. wt. silane coupling agent, 2.5-10 pts. wt. absolute ethanol and 5-20 pts. wt. water into the three-necked flask, adjusting pH to 4-5 using glacial acetic acid, stirring at room temperature at speed of 300 revolution per minute for 2 hours, adding 1.5-3 pts. wt. graphene oxide magnetic material, stirring at room temperature at speed of 300 revolution per minute for 4 hours, carrying out amino modification of magnetic graphene oxide adsorbing material, washing with anhydrous ethanol 3 times, freeze-drying and grinding, adding 0.5-1.5 pts. wt. of hydroxyethylidene diphosphonic acid powder to the solvent at a concentration of 0.04 g/ml solution, then adding 0.5-2 pts. wt. basic catalyst and 0.1-1 pts. wt. polypeptide condensing agent to the above solution, stirring at room temperature, adding aminated magnetic graphene oxide powder to above solution, stirring at room temperature for 24 hours at speed of 300 revolution per minute, washing with water and ethanol 3 times, freeze-drying and grinding to obtain final product. An INDEPENDENT CLAIM is also included for use method of hydroxyethylidene diphosphonic acid-modified magnetic graphene oxide adsorbent in removing heavy metal ions comprising taking 50 ml, 80-200 mg/l solution of heavy metal ions in 250 ml erlenmeyer flask, adjusting pH to 2-8, adding 7-12 mg adsorbent, oscillating in a an oscillator under water bath for 1-3 hours at 25-45 degrees C, carrying out magnetic separation, detecting heavy metal ions in the residual concentration of supernatant, calculating based on the initial concentration C(o) and adsorption of heavy metal ions in solution, solution of heavy metal ion concentration C(e), and removing heavy metal ions.