糠醇催化加氢.docVIP

Section 7 Liquid phase hydrogenation of furfural to furfuryl alcohol over Raney Ni 实验目的： 掌握糠醛加氢反应过程及反应机理、特点，了解副反应和生成副产物的过程。 掌握高压釜的构造、原理和学习方法，学习反应器正常操作和安装，掌握催化剂的评价的一般的方法和获得适宜工艺条件的研究步骤和方法。 学习自动控制仪表的使用，如何设定温度和加热电流的大小。怎样控制床层温度分布。 了解气相色谱的原理和构造。掌握色谱的正常使用和定性、定量分析。 了解Raney Ni的制备原理和使用方法。 实验原理： 糠醇是一种应用广泛的化工产品。目前在国内工业生产中主要采用Raney Ni催化剂对液相糠醛加氢的方法制备。 本实验采用自制Raney Ni作为催化剂，在100oC，1.0MPa的条件下进行液相加氢反应。 实验仪器和药品： 仪器：高压釜，气相色谱和色谱工作站 药品：Ni-Al合金，糠醛，蒸馏水，NaOH，无水乙醇 实验步骤： Preparation of Raney Ni: In a 200 ml Erlenmeyer flask equipped with a thermometer and a Magnetic Stirrer are placed 60 ml of distilled water and 16 g of HYPERLINK /orgsyn/chemname.asp?nameID=32818 sodium hydroxide pellets. The solution is stirred rapidly and allowed to cool to 323 K in an ice bath. 12.5 g of Raney nickel-aluminum alloy powder is added in small portions during a period of 25–30 minutes. The temperature is maintained at 323±2 K by controlling the rate of addition of the alloy to the HYPERLINK /orgsyn/chemname.asp?nameID=32818 sodium hydroxide solution and the addition of ice to the cooling bath. When the entire alloy has been added, the suspension is digested at 323±2 K for 50 minutes with gentle stirring. It is usually necessary to remove the ice bath and replace it with a hot-water bath to keep the temperature constant. After this period of digestion the catalyst is washed with three 100 ml portions of distilled water by decantation. Liquid phase hydrogenation of furfural: 10 ml furfural (FFR), 90 ml EtOH and 2.0 g Raney Ni catalyst were mixed in a 500 ml steel autoclave equipped with a mechanical stirrer and an electric heating system. The reactor was filled with H2 five times in succession to exclude the inside air. Then it was filled with H2 up to 1.0MPa, followed by heating slowly (80 K/h) until 373 K. Once the pressure reached a steady state, the hydrogenation reaction was initiated immediately by stirring the reaction mixture vigorously. According to the drop of H2 pressure with the time, the hydroge