• 专利标题:   Preparing nitrogen trifluoride by electrolysis of ammonium bifluoride comprises adding conductive graphene into methanol, adding 1-hexyl-3-methylpyridinium bromide, mixing to obtain suspension.
  • 专利号:   CN106222688-A, CN106222688-B
  • 发明人:   CHEN G, LI J, ZHANG G, WANG N, ZHOU J, CHEN L, SUN L, QIAN H, HUA Y, XUN Y
  • 专利权人:   ZHEJIANG BORUI ELECTRONIC TECHNOLOGY CO
  • 国际专利分类:   C25B001/24
  • 专利详细信息:   CN106222688-A 14 Dec 2016 C25B-001/24 201716 Pages: 6 Chinese
  • 申请详细信息:   CN106222688-A CN10567035 19 Jul 2016
  • 优先权号:   CN10567035

▎ 摘  要

NOVELTY - Preparing nitrogen trifluoride by electrolysis of ammonium bifluoride comprises adding conductive graphene into methanol, adding 1-hexyl-3-methylpyridinium bromide, mixing to obtain suspension, soaking carbon electrode in suspension, adding ammonia solution, adding 1-butyl-3-methyl-imidazole, soaking, and drying to obtain graphene-modified carbon electrode, preparing nitrogen trifluoride by carrying out electrolysis to obtain mixed gas containing nitrogen trifluoride, tetrafluoromethane, nitrous oxide and many trace impurities, and purifying the mixed gas. USE - The method is useful for preparing nitrogen trifluoride by electrolysis of ammonium bifluoride (claimed). DETAILED DESCRIPTION - Preparing nitrogen trifluoride by electrolysis of ammonium bifluoride comprises (i) preparing conductive graphene-modified carbon electrode: adding conductive graphene into 10-15 times the amount of methanol, adding 1-hexyl-3-methylpyridinium bromide (0.1-0.5% of the amount of conductive graphene), mixing for 10-50 minutes to obtain suspension, adding carbon electrode into the above obtained suspension and soaking for 20-80 hours, adding ammonia solution (10-15 times the amount of the amount of conductive graphene) having specific gravity of 10-30, adding 1-butyl-3-methyl-imidazole (0.1-0.5% of the amount of conductive graphene), and soaking for 20-80 hours, taking out and drying to obtain graphene-modified carbon electrode i.e. an anode for electrolytic reaction, and (ii) preparing nitrogen trifluoride: taking hydrogen fluoride and ammonium fluoride dubbed continuous electrolytic solution, injecting into electrolysis tank, using above obtained conductive type graphene-modified carbon electrode as anode of the electrolysis tank, carrying out electrolysis at 80-150 degrees C under a pressure of -0.01 MPa to 0.01 MPa and voltage of 5-10 V to obtain anode-forming mixed gas containing nitrogen trifluoride, tetrafluoromethane, nitrous oxide and many trace impurities, purifying the mixed gas by series of processes including removal of fluoride impurities and acidic impurities, adsorbing nitrogen trifluoride through molecular sieve to separate nitrogen trifluoride from tetrafluoromethane, and removing impurities to obtain high purity fluorine-containing organic gas products.