Add 0.1 g of catalyst and also 60 mmol of benzene in turn to a three-necked flask (50 mL) outfitted with a reflux condenser, and pass nitrogen gas to obtain the air in the three-necked flask and also the hydrogen chloride gas produced after the response. Soak up in sodium hydroxide option, heat to 80 ° C under magnetic stirring, then add 10 mmol of benzyl chloride, quit the response after 1 h of reaction, cool the response remedy to space temperature, filter as well as separate the stimulant, as well as take the filtrate for gas chromatography evaluation.
The preparation of the stimulant is as follows: under the surveillance of magnetic mixing and also pH meter, initial add 25 mL of sodium dihydrogen phosphate (0.01 mol) liquid option to 75 mL of salt metavanadate (0.01 mol) aqueous solution, add dropwise V( H2SO4 ): V( WATER) = 1:1 sulfuric acid to change the pH of the remedy to 4.00, after that include 50 mL of salt molybdate (0.08 mol) liquid solution, include the above sulfuric acid remedy dropwise once more to readjust the pH to 3.8, as well as reflux at 99 ° C for 8 h.
After cooling, move the option right into a separatory funnel, include 80 mL of anhydrous ether, add V( H2SO4): V( WATER) = 1:1 sulfuric acid in small portions, shake, as well as after standing still, the red oily material in the lower layer is heteropolyacid ether substances. Place the oil in the fume hood for 1-2 days till the crystalline fragments are precipitated, then include a percentage of distilled water and also recrystallize to get a noticeable crystal form. After drying out in a vacuum cleaner stove at 60 ℃, an orange-red powdery substance is acquired, which is H8P2Mo16 V2O62 · 41H2O stimulant, denoted as HPA, ready for use.
Preparation of Fe2H2P2Mo16V2O62 · 41H2O: According to the stoichiometric proportion, consider 2 mmol of HPA as well as liquify it in a three-necked flask full of 20 mL of pure water, then replace the air in the three-necked flask with nitrogen, and also placed the Add 4 mmol of ferric chloride right into the option of HPA. At this time, ferric chloride dissolves swiftly in the heteropoly acid option and reacts. After mixing for 2 hrs, it is dried out by suction filtering as well as vacuum cleaner purification, and also orange yellow is obtained after grinding. Powdered molybdenum vanadium iron salt is Fe2H2P2Mo16V2O62 · 41H2O, which is recorded as FeHPA.