Synthesis method of 2-tert-butoxymethyltetrahydrofuran
A technology of tert-butoxymethyl tetrahydrofuran and its synthesis method, which is applied to the synthesis of 2-tert-butoxymethyl tetrahydrofuran and the field of synthesizing 2-tert-butoxymethyl tetrahydrofuran, which can solve the problem of waste acid treatment being unfriendly to the environment, Response selectivity is not high, to achieve high economic value and social value, increase the reaction rate, improve the effect of conversion rate
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[0030] The synthesis method includes the following steps: first, the catalyst and tetrahydrofurfuryl alcohol are put into a reactor for stirring, and then isobutene is passed into the reaction system for reaction; preferably, the stirring speed is 30-400 RPM.
[0031] The synthesis method comprises the following steps: loading a catalyst into a fixed-bed reactor, mixing feedstock of tetrahydrofurfuryl alcohol and isobutylene gas, and reacting to obtain 2-tert-butoxymethyltetrahydrofuran.
[0032] The etherification reaction temperature is 40-70°C, the reaction pressure is 0.05-0.8Mpa, and the reaction time is 2-4 hours;
[0033] Preferably, the etherification reaction temperature is 50-55° C., the reaction pressure is 0.1-0.45 Mpa, and the reaction time is 3 hours.
[0034] The molar ratio of tetrahydrofurfuryl alcohol and isobutene is 1:1-1.3, preferably 1:1.08.
[0035] The weight ratio of tetrahydrofurfuryl alcohol and the catalyst amount of the large pore size strong acid...
Embodiment approach
[0037] The present invention has no particular limitation on the method for purifying the reaction product mixture, for example, filtration, extraction, distillation, azeotropic distillation, rectification and other methods can be independently used for purification. According to a specific embodiment of the present invention, the purification is performed according to the following method: filter the mixture with filter paper, add 0.3-1.2 times the mass of pure water to the filtered material, carry out azeotropic distillation and purification, and then use a separatory funnel Dispense. The organic phase obtained by liquid separation is dried with alumina small spherical molecular sieves, and then the product is distilled out at atmospheric pressure, and the components after pulling are collected to obtain fractions with a purity greater than 98%.
[0038] In the embodiment of the present invention, tetrahydrofurfuryl alcohol was purchased from Shanghai Merrell Chemical Techno...
Embodiment 1
[0041] The present embodiment discloses the synthetic method of 2-tert-butoxymethyltetrahydrofuran of the present invention, specifically:
[0042] Add 3g macroporous acidic cationic resin catalyst and 1.5mol tetrahydrofurfuryl alcohol to the 1L high pressure reaction kettle, replace the air with nitrogen after the closed reaction kettle, discharge to slightly positive pressure, then fill with 1.5mol isobutene, and the reactor pressure reaches 0.2MPa (G ). Start stirring at 200rpm, adjust the reaction temperature to rise to 50°C, the pressure in the kettle is 0.45MPa (G), the reaction time is 3.0 hours, until the pressure in the kettle drops below 0.15MPa, the reaction ends.
[0043] The material was discharged, and the catalyst was filtered to obtain a transparent yellowish liquid. The obtained liquid material was added with the same amount of water as the liquid material, and the product was purified by azeotropic distillation at 120°C.
[0044] The 2-tert-butoxymethyltetr...
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