Diphenyl Methane CAS 101-81-5

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.

The details technological plan is as adheres to: Benzene and formaldehyde are utilized as raw materials, the weight proportion of the amount utilized is 20/1 2/1, the reaction problems are: at a temperature of 100-200 ° C, the reaction time is 18 hours, under the action of the driver The following set type one-step condensation reaction is used for synthesis, and also the weight ratio of driver and also reactant is 1/50 1/5.

The response actions are: 1) Add benzene and also formaldehyde right into the activator, the molar ratio of benzene and formaldehyde is 20/1 2/1; 2) Add driver, the ratio of catalyst to formaldehyde is 1/50 1/ 5. Use high-purity nitrogen as a safety ambience, stir, as well as respond at a temperature level of 100-200 ° C for 18 hours, add nitrobenzene as an interior standard to the obtained product, and do conversion evaluation on GC; after the response, the stimulant is centrifuged 3) The response item is remedied, as well as the unreacted benzene can be recovered and also recycled; 4) Include absolute ethanol to dissolve the solid product after rectification, and after that continuously correct under minimized pressure to obtain Item Diphenyl Methane.

It is identified by adding HCl with a focus of 10% to 16% to Hangjin 2 # clay mine at a solid-liquid proportion of 1:2.5 -3, home heating and also activating at 90-100 ° C for 3.5-4 hrs, washing with water until pH=6, and also suction purification. The filter cake is dried at 100 ° C-105 ° C, baked at 250-300 ° C for 2-3 hours, and also cooled down to area temperature to obtain clay-SA01 for later usage. Utilizing clay-SA01 as a provider, first liquify ZnCl2 in a ratio of 0.135-0.27 g: 1ml-2ml Acquire a ZnCl2 methanol combination in methanol, after that mix and impregnate the blend with the provider clay-SA01 at a proportion of 0.135-0.27 g of energetic component ZnCl2 per gram of clay-SA01 for 24-36 hrs to create a paste example.

Dry the sample in vacuum at 70-80 ° C for 3-4 hrs, recuperate methanol, and also prepare a strong sample of ZnCl2/clay-SA 01, and roast the strong example of clay-SA01 at 250-300 ° C for 3-4 hrs under the protection of N2 gas. Get ZnCl2/clay-SA 01 catalyst, after that cool down the catalyst to area temperature level in N2 atmosphere, include stimulant as well as benzene in the activator geared up with calcium chloride drying out gadget as well as HCl gas absorption gadget, slowly warmth to 40-50 ° C, After mixing for 10-15 minutes, slowly add benzyl chloride, the proportion of benzene: benzyl chloride: driver is 25ml:2.6 ml:1 g, after that elevate the response temperature level to 65-70 ° C, after 3-4 hrs of response, stop home heating, After cooling down to area temperature level, solid-liquid separation is performed, the catalyst is recuperated, the mixed fluid is distilled to divide benzene as well as Diphenyl Methane, and also the solvent benzene is recovered.