• 专利标题:   Production method of high-purity pentachlorobenzonitrile, involves stirring graphene oxide and zinc chloride, placing in impregnation tank, adding distilled water, and stirring to form graphene oxide/zinc chloride mixed solution.
  • 专利号:   CN107597091-A, CN107597091-B
  • 发明人:   MIAO J, WANG J, HUANG Y, WANG C, BAO L
  • 专利权人:   JIANGSU SULI FINE CHEM CO LTD
  • 国际专利分类:   B01J021/18, B01J023/06, B01J035/10, B01J037/02, B01J037/12, B01J037/24, C07C253/30, C07C253/34, C07C255/50
  • 专利详细信息:   CN107597091-A 19 Jan 2018 B01J-023/06 201816 Pages: 7 Chinese
  • 申请详细信息:   CN107597091-A CN10874478 25 Sep 2017
  • 优先权号:   CN10874478

▎ 摘  要

NOVELTY - The production of high-purity pentachlorobenzonitrile involves stirring graphene oxide and zinc chloride, placing in a impregnation tank, adding distilled water into the impregnation tank, and stirring to form graphene oxide/zinc chloride mixed solution, immersing in the graphene oxide/zinc chloride mixed solution to obtain modified activated carbon catalyst, filling the catalyst into a bed reactor, introducing nitrogen into the bed reactor, dehydrating, adding excess chlorine, reacting the modified activated carbon catalyst, and pumping raw material benzonitrile into a vaporizer. USE - Production method of high-purity pentachlorobenzonitrile. ADVANTAGE - The method enables production of high-purity pentachlorobenzonitrile with greatly reduced required temperature of chlorination reaction, improved product content of less than 99.6%, and prolonged service life of the catalyst. DETAILED DESCRIPTION - The production method of high-purity pentachlorobenzonitrile involves (A) preparing graphene oxide, (B) weighing 0.5-2 kg prepared graphene oxide and 8-12 kg zinc chloride, uniformly stirring, placing in a impregnation tank, adding 1500 kg distilled water into the impregnation tank, and stirring to completely dissolve zinc chloride and graphene oxide to form graphene oxide/zinc chloride mixed solution, immersing the coconut shell activated carbon in the graphene oxide/zinc chloride mixed solution to obtain modified activated carbon catalyst, where the adding amount of graphene oxide/zinc oxide composite material is 0.5-2 wt.% of the total amount of coconut shell activated carbon, (C) filling the modified activated carbon catalyst prepared in the step (B) into a composite bed reactor, where the composite bed reactor is a fluidized-bed and fixed-bed composite bed reactor, introducing nitrogen into the composite bed reactor, increasing the temperature to 100-150 degrees C, dehydrating for 0.5-2 hours, adding excess chlorine, reacting the modified activated carbon catalyst at 200-250 degrees C for 2-4 hours, when the temperature of each point of the two reactors is stable, no hydrogen chloride gas is detected in the tail gas, (D) pumping the raw material benzonitrile through a metering pump into a vaporizer, passing the pre-heated nitrogen into the vaporizer, vaporizing the benzonitrile, and heating nitrogen preheater and vaporizer by a gas furnace, (E) vaporizing the liquid chlorine, preheating to obtain chlorine gas, mixing 70 vol.% chlorine gas with benzonitrile gas containing nitrogen, adding into the fluidized bed in step (C), mixing the gas in fluidized bed with 30 vol.% remaining chlorine into fixed bed for supplementary reaction, and heating a mixer using the gas furnace, and (F) collecting the reactants by a collecting device to obtain pentachlorobenzonitrile powder, where the collecting device comprises water cooling jacket, absorbing the exhaust gas generated by reaction with water, iron chloride and calcium hydroxide, and discharging exhaust gas at zero.