• 专利标题:   Catalyst for preparing gama-valerolactone by catalytic hydrogenation of levulinic acid, comprises copper silver zirconium graphene oxide catalyst, where catalyst is metal copper-silver, metal silver as electronic agent, zirconium oxide as carrier, and graphene oxide as structural auxiliary agent.
  • 专利号:   CN114950478-A
  • 发明人:   YIN J, LI S, MAO J, JIA Y, ZHOU J
  • 专利权人:   UNIV DALIAN
  • 国际专利分类:   B01J023/89, C07D307/33
  • 专利详细信息:   CN114950478-A 30 Aug 2022 B01J-023/89 202297 Chinese
  • 申请详细信息:   CN114950478-A CN10793856 07 Jul 2022
  • 优先权号:   CN10793856

▎ 摘  要

NOVELTY - Catalyst comprises a copper silver zirconium graphene oxide (CuAgZrGO) catalyst. The catalyst is metal copper-silver (Cu-Ag) as basic component, metal silver (Ag) as electronic agent, zirconium oxide (ZrO) as carrier, and graphene oxide (GO) as structural auxiliary agent. USE - Catalyst for preparing gama-valerolactone by catalytic hydrogenation of levulinic acid. ADVANTAGE - The catalyst does not need to undergo high temperature pre-reduction pretreatment before use, and the conversion rate of levulinic acid reaches 100% after reacting for 4 hours at 200℃ and 3MPa hydrogen pressure. The selectivity of γ-valerolactone is 100%, and the detected contents of Cu, Ag, Zr components are all below 1 mg/L. The copper uses as the main metal component is cheaper than using silver or platinum, palladium and other noble metal catalysts. The small amount of Ag promoter is added as an electron promoter, which eliminates the catalyst pre-reduction operation, and also effectively inhibits the precipitation of copper. DETAILED DESCRIPTION - INDEPENDENT CLAIMS are included for: A method for preparing catalyst for preparing γ-valerolactone by catalytic hydrogenation of levulinic acid, which involves: taking 230 mL concentrated sulfuric acid and 5.0 gram NaNO3, stirring and adding 10 g natural flake graphite powder, stir for 2.5 hours, adding KMnO4, transferring to a constant temperature water bath at 35℃ to react for 2 hours, adding 460 mL deionized water, stirring in an oil bath at 98℃ for 15 minutes, and finally adding 1.4 L deionized water, and 25 mL 30 wt.% H2O2 and cooling to room temperature, centrifuging in deionized water, then washing, until become neutral to obtain a GO carrier for use. The 0.7250 gram copper nitrate trihydrate (Cu(NO3)2.3H2O), 0.2548 gram silver nitrate (AgNO3) and 3.2200 gram zirconium nitrate pentahydrate (Zr(NO3)4.5H2O) are taken and dissolved in deionized water to make a salt solution, then weighed 12.7646 gram GO and added to a beaker medium, and ultrasonically treated for 30 minutes. The ultrasonicated salt solution is put in a beaker, shaked it up and titrated it with a prepared 0.2 molar sodium hydroxide solution to make it precipitate, until pH to 12. The sample is placed after standing in a vacuum drying oven at 80℃ to dry for 12 hours, and ground with an agate mortar until the sample becomes powder. The powdered sample is put into a quartz tube, and placed in a tube furnace in a nitrogen atmosphere with a programmed temperature of 10℃/min from room temperature to 500℃, constant temperature calcination at 500℃ for 2 hours, when the temperature dropped to room temperature, the sample is taken out and sealed and stored. A method for preparing γ-valerolactone by catalytic hydrogenation of levulinic acid, which involves using water as the reaction solvent, reacting levulinic acid (LA) with hydrogen in the reaction kettle under the action of CuAgZrGO catalyst, where hydrogenation temperature of LA is 200-210℃, the hydrogen pressure is 1-4 MPa, and the reaction is 0.5-4 hours to obtain GVL.