Furylethylene functional monomer synthesized by catalyzing furfuryl alcohol/methanol conversion two-step method and catalyst application
A technology of vinyl furan and functional monomers, applied in physical/chemical process catalysts, molecular sieve catalysts, catalyst activation/preparation, etc., can solve the problems of harsh experimental conditions, unavailable raw materials, high cost of raw materials, etc., and achieve control of reaction selectivity , Improve atom utilization, poor controllability effect
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[0106] The present invention provides a kind of synthetic method of furan vinyl functional monomer, comprises the following steps:
[0107] 1) After methanol, furfuryl alcohol compounds and acidic catalysts are subjected to liquid-phase reaction, ether compounds are obtained;
[0108] 2) The ether compound and tetrahydrofuran obtained in the above steps are subjected to a gas phase reaction under the action of a solid catalyst and a protective atmosphere to obtain a furan vinyl functional monomer;
[0109] The furfuryl alcohol compound includes furfuryl alcohol and / or furfuryl alcohol derivatives;
[0110] The acidic catalyst includes an acid, and / or, an ionic liquid and / or an ionic liquid obtained from an acid and nitrogen-containing organic matter;
[0111] The solid catalyst includes a solid molecular sieve catalyst and / or a modified solid molecular sieve catalyst.
[0112]In the present invention, the parameters, selection and composition of the required raw materials, p...
Embodiment 1
[0177] Mix methanol and furfuryl alcohol into a three-necked flask at a mass ratio of 10 / 1, add 1.2g of phosphomolybdic acid, install a distillation tube, heat up to 75°C, react for 2 hours, cool to room temperature, extract three times with ether, and obtain bran after rotary evaporation Methyl methyl ether, add methanol, control the mass ratio of furfuryl methyl methyl ether / methanol to 10 / 1, stand-by.
[0178] Characterize the furfuryl methyl ether, the product of the first step prepared in the present invention.
[0179] see figure 1 , figure 1 The mass spectrogram of the first step product furfuryl methyl ether of the synthetic method provided by the present invention.
[0180] see figure 2 , figure 2 The ether-forming reaction product composition (GC) of the synthesis method provided by the invention.
[0181] Depend on figure 1 and figure 2 It can be seen that the present invention obtains the target product furfuryl methyl ether in the first step, and there a...
Embodiment 2
[0189] Accurately weigh 5mmol of phosphotungstic acid and 15mmol of N-methylpyrrolidone, and add them to 3ml of deionized water respectively. At room temperature, add the phosphotungstic acid solution to the N-methylpyrrolidone solution drop by drop while stirring, and a white precipitate appears. Filter , after drying at 120°C, weigh 1.5g of the catalyst and add it to a three-necked flask filled with methanol and furfuryl alcohol (methanol / furfuryl alcohol=8 / 1), install a distillation tube, heat up to 105°C, react for 1.5h, and cool to At room temperature, extract three times with diethyl ether, obtain furfuryl methyl ether after rotary steaming, add methanol, control the mass ratio of furfuryl methyl ether / methanol to 8 / 1, and set aside.
[0190] Roast ZSM-5 in a muffle furnace at 500°C for 4h, weigh 5g of ZSM-5 in a beaker, add it to 8ml of silver nitrate solution (concentration: 0.4g / ml), let stand overnight, dry at 120°C for 8h, then Calcined at 500°C for 5 hours in a muf...
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Abstract
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