• 专利标题:   Preparing bromine-doped graphene oxide by preparing graphene oxide using concentrated sulfuric acid, adding analytically pure hydrobromic acid, obtaining graphene oxide and hydrobromic acid solution and carrying out hydrothermal reaction.
  • 专利号:   CN110562970-A
  • 发明人:   TANG L, XIANG J, ZHANG Q, TIAN P
  • 专利权人:   KUNMING PHYSICS INST
  • 国际专利分类:   C01B032/198
  • 专利详细信息:   CN110562970-A 13 Dec 2019 C01B-032/198 202005 Pages: 8 Chinese
  • 申请详细信息:   CN110562970-A CN10964159 11 Oct 2019
  • 优先权号:   CN10534816

▎ 摘  要

NOVELTY - Method for preparing bromine-doped graphene oxide involves adopting graphene oxide, adding analytically pure hydrobromic acid according to a certain carbon bromine atom ratio to generate bromine-doped graphene oxide at one time through a hydrothermal reaction. The method involves carrying out three steps of (i) preparing graphene oxide, (ii) obtaining graphene oxide and hydrobromic acid solution and (iii) carrying out the hydrothermal reaction. The step (i) involves taking concentrated sulfuric acid, pouring graphite powder and sodium nitrate, stirring, adding potassium permanganate, reacting, adding hydrogen peroxide solution, centrifuging and washing, obtaining a precipitate and drying. The step (ii) involves taking graphene oxide, adding deionized water and carrying out ultrasonic treatment, stirring with analytically pure hydrobromic acid and mixing to form a homogeneous solution. The step (iii) adding the homogeneous solution into reaction kettle liner and reacting. USE - The method is useful for preparing bromine-doped graphene oxide. ADVANTAGE - The method involves less consumables and simple steps and is suitable for mass production and provides a semiconductor type bromine-doped graphene oxide preparation technology which effectively modulates the energy level of graphene oxide through doping of heterogeneous bromine atoms to optimize photoelectric performance of graphene oxide. DETAILED DESCRIPTION - Method for preparing bromine-doped graphene oxide involves adopting graphene oxide, adding analytically pure hydrobromic acid according to a certain carbon bromine atom ratio to generate bromine-doped graphene oxide at one time through a hydrothermal reaction. The method involves carrying out three steps of (i) preparing graphene oxide, (ii) obtaining graphene oxide and hydrobromic acid solution and (iii) carrying out the hydrothermal reaction. The step (i) involves taking 23 ml concentrated sulfuric acid in a beaker of an ice bath, weighing and pouring 0.5 g graphite powder and 0.25 g sodium nitrate into concentrated sulfuric acid, stirring for half an hour with a mechanical stirrer, weighing and slowly adding 3 g potassium permanganate, maintaining in the ice bath for 1 hour, transferring to 35 degrees C water bath, reacting for 1 hour, transferring to 98 degrees C water bath, adding 60 ml deionized water to obtain a solution, maintaining the solution under the stirred condition for half an hour, adding 100 ml deionized water into the solution at a time, adding 10 ml hydrogen peroxide solution to finally obtain a golden yellow solution, centrifuging and washing with 10% hydrochloric acid solution for 3-5 times until no sulfate ions in the centrifugal supernatant are detected, obtaining a golden yellow precipitate which is graphite oxide and drying at 60 degrees C. The step (ii) involves weighing and taking 0.1 g graphene oxide obtained in the step (i) in the beaker, adding 100 ml deionized water and carrying out ultrasonic treatment for 3 hours to prepare 1 mg/ml graphene oxide solution, taking 32.43 ml graphene oxide solution and 7.57 ml analytically pure hydrobromic acid according to the carbon bromine atomic molar ratio of 5:1, stirring and mixing with ultrasound to form a graphene oxide and hydrobromic acid homogeneous solution. The step (iii) adding the graphene oxide and hydrobromic acid homogeneous solution prepared in the step (ii) into 50 ml reaction kettle liner and reacting in a reaction kettle at 170 degrees C for 10 hours to obtain bromine-doped graphene oxide.