Preparation method of p-alkyl catechol
A technology of alkyl catechol and catechol, which is applied in the field of preparation of p-alkyl catechol, can solve problems such as poor selectivity, equipment corrosion, poor product quality and yield, and achieve good product quality , Less by-products, high activity effect
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[0016] The preparation method of the supported heteropolyacid catalyst of the present invention is as follows: fully mixing the heteropolyacid solution and the carrier to form a sol, and then drying, calcining and pulverizing the sol. The heteropolyacid solution is a solution of heteropolyacid in polar solvents such as water, alcohol, aldehyde, ketone, ether, etc., and the solvent is preferably methanol, ethanol or water. The concentration of the heteropolyacid solution is preferably 0.01 to 0.5 g / ml. The drying temperature is preferably 80-120°C, the drying time is preferably 2-5 hours, the calcination temperature is preferably 250-350°C, and the calcination time is preferably 2-5 hours.
[0017] The synthesis reaction of the present invention is preferably carried out under nitrogen protection. Before the reaction, the catechol is heated and melted in a nitrogen environment, raised to the reaction temperature under stirring conditions, and an alkylating agent is added for re...
example 1
[0022] (1) Preparation of catalyst
[0023] Mix phosphotungstic acid and ethanol to make a solution with a concentration of 0.2g / ml, take 80ml of phosphotungstic acid solution and 24.0g of SiO 2 Mix evenly to form a sol, dry at 120°C for 4 hours, bake at 300°C for 4 hours, and pulverize to obtain a supported catalyst A, which contains 40% by mass of phosphotungstic acid.
[0024] (2) Preparation of p-tert-butylcatechol
[0025] Add 165.2g (1.5mol) of catechol, 33.0g of catalyst A in a four-necked flask with a mechanical stirrer, a thermometer, an air inlet conduit and a liquid-sealed condenser connected, and feed N 2 Gas, replace the air in the reaction system, then heat and melt catechol, raise the temperature to 130°C under stirring, feed isobutene gas, adjust the ventilation speed of isobutene, control the pressure of the reaction system to 0.1015MPa, and feed 84.0 MPa within 3 hours g (1.5 mol) of isobutene, after ventilation is completed, continue to react at this tempe...
example 2
[0027] Add 165.2g (1.5mol) of catechol, 25.5g of Catalyst A into a four-neck flask with mechanical stirring, thermometer, dropping funnel, water separator and a condenser connected to a liquid seal, and feed into N 2 Gas, replace the air in the reaction system, then heat and melt catechol, raise the temperature to 120°C under stirring, add methyl tert-butyl ether liquid dropwise, adjust the dropping speed, control the reaction system pressure to 0.1015MPa, within 3 hours Add 110.2 g (1.25 mol) of methyl tert-butyl ether dropwise. After the addition is complete, react at this temperature for 1.5 hours, cool down to 90° C. within 15 minutes, continue to react for 1.5 hours, and stop the reaction. The methanol by-product produced by the reaction is separated from the water separator, and the reaction mixture is directly rectified to obtain the raw material catechol, the middle distillate, the p-tert-butyl catechol product and the rectification residue including the catalyst. The ...
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