Paired Electrosynthesis Of Anisaldehyde And P-aminophenol

With the rapid development of today's society,chemical industrial products have an impact on people's lives.While improving people's lives,they also inevitably exert great pressure on the society because in their production processes,they are often accompanied by environmental issues pollution.In response to this problem,people began to further study “Green Chemistry”.Electrochemistry in the production process,the electricity for the energy,produce hydrogen and oxygen,less environmental pollution,has become an important part of green chemistry.Today,electrochemistry is widely used in many fields.Currently,many popular research topics in the world are more or less closely connected with electrochemistry.Electrochemical synthesis technology compared with the traditional chemical synthesis technology,the operation easier to control the process,the production of higher purity products,fewer by-products and less environmental pollution and has a high economic advantages.As an organic chemical product,anisaldehyde and p-aminophenol play an important role in production and life.Anisaldehyde,also known as p-methoxybenzaldehyde,is a natural component of some ether oils that can be used as a perfume ingredient in soaps and other cosmetics,as well as a chemical intermediate in the pharmaceutical and perfumery industries;At the same time,as the brightener of the cyanide galvanizing DE additive can effectively improve the anodic polarization,and the applicable current range is wider,and a bright plating layer can be obtained,which effectively reduces the pollution to the environment.p-Aminophenol,also known as "p-hydroxyaniline" is widely used as a common fine chemical in a variety of industries.It is mainly used in dyes and pharmaceutical industries.Therefore,the active exploration of the preparation method of anisaldehyde and p-aminophenol is of great significance.Through literature research,it was found that the reaction conditions for the preparation of anisaldehyde and p-aminophenol by electrosynthesis are similar,that is,they can be electrolyzed under acidic conditions,and the electrolysis temperature and the cell voltage are similar,which is theoretically in line with the reaction conditions of the paired electrosynthesis.The experiment adopts the green clean paired electrosynthesis technology.In an electrolysis reaction,p-aminophenol and anisaldehyde,two kinds of products with high added value,are simultaneously prepared at the cathode and anode.The experiment content is as follows:First,graphite anode was used in this experiment,cyclic voltammetry analysis was carried out on the graphite electrode to investigate the effect of different scanning rates on the oxidation of p-methylanisole on the graphite electrode in acidic solution.The experimental results show that in acidic solution,the electrochemical reaction of p-methylanisole on the graphite electrode to form anisaldehyde is a diffusion-controlled process.Second,in the H-type membrane electrolyzer,self-made graphite electrode as anode and self-made copper electrode as cathode,anisaldehyde was electrolytically synthesized in the mixed solution of sulfuric acid and acetonitrile.Through the orthogonal experiment and supplementary experiments,the effects of the addition of p-methylphenylether,the addition of sulfuric acid,the reaction temperature,the reaction current and the addition of acetonitrile on the anode current efficiency were discussed.The experimental results showed that the optimal conditions for the electro-oxidation of p-methylphenylether to anisaldehyde were 0.015 mol of reactant,0.04 mol/L of sulfuric acid,45?of electric current,0.04 A of current and 40% of acetonitrile,The current efficiency reached 62.81%.Third,by consulting the literature,we can see that there are many methods for the detection of cathodic products of p-aminophenol and aniline.Among them,the HPLC method is simpler than other detection methods,the detection results are accurate,and the volatility of the sample to be tested is high.Thermal instability does not affect the detection results.Therefore,high performance liquid chromatography is a common detection method and is very suitable for the detection of the content of such substances.Based on the existing literature,this experiment established a high-performance liquid chromatography method for the detection of electroreduced nitrobenzene reaction products,and explored the influence of various factors on the detection results.The experimental results show that the optimal detection conditions for HPLC analysis are detection wavelength of 260 nm,mobile phase of 60% methanol solution,column temperature of 35?,flow rate of 1.0 mL/min,and detection of electroreduction nitro groups using this method.The recoveries of the benzene reaction products were between 90.8%~107.3%,93.8%~108.2%,and 92.0%~103.4%,indicating that the three components of nitrobenzene,aniline and p-aminophenol exist simultaneously.This method can be used to detect the content of 3 substances.Fourth,the electrochemical behavior of nitrobenzene on the surface of copper electrode was studied in a mixed system of sulfuric acid and ethanol using homemade graphite electrode and copper electrode as the electrolytic anode and cathode,respectively,and different scanning rates were investigated for copper in acidic solution.Effect of nitrobenzene reduction on the electrode.The experimental results show that in the acidic solution,the electrochemical reaction of nitrobenzene on the copper electrode to generate p-aminophenol is a diffusion-controlled process.Under the optimal conditions to ensure that the anion generates anisaldehyde,the process of preparing the cathodoxy from the cathode is paired with the anode.In an H-type diaphragm cell,the homemade graphite electrodes and copper electrodes were used as the electrolysis anode and cathode,respectively.The optimum electrolysis conditions of the anode were fixed.Through the orthogonal test and complementary experiments of related conditions,the reactant nitrobenzene was investigated.The effect of electrolysis conditions on the current efficiency,such as the amount,the amount of sulfuric acid added,and the volume fraction of absolute ethanol.The result showed that the optimal reaction conditions for the cathode were 0.005 mol of reactants,and the volume fraction of sulfuric acid and absolute ethanol was 20%.On this basis,the total current efficiency of the cathode and anode of the electrolysis reaction reached more than 141%,demonstrating that paired electrosynthesis of anisaldehyde and p-aminophenol is completely feasible.For the single-electrode reaction,the research results not only greatly improve the current efficiency and space-time efficiency of the electrolysis process,but also lay a good theoretical foundation for the future industrial production.