A kind of multi-level gradient porous carbon-based sulfonic acid microsphere with uniform particle size, its preparation method and application
A carbon-based sulfonic acid, gradient pore technology, applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of diffusion and transmission of unfavorable substances, high cost of catalyst preparation, and poor catalytic effect.
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[0044] The present invention provides a method for preparing the multi-stage gradient porous carbon-based sulfonic acid microspheres of the above-mentioned technical scheme, comprising the following steps:
[0045] Mix carbon source, sulfonating agent, inorganic salt and water to obtain precursor solution;
[0046] Microfluidic spray drying of the precursor solution to obtain composite microspheres;
[0047] The composite microspheres are calcined to remove inorganic salts to obtain carbon-based sulfonic acid microspheres with multi-level gradient pores.
[0048] The preparation method provided by the invention combines the precursor solution mixed with carbon source, sulfonating agent, inorganic salt and water with microfluidic spray drying technology to obtain good sphericity, uniform particle size, continuously adjustable in the micron range, and specific surface area Large multi-level gradient pore carbon-based sulfonic acid microspheres; it also has a multi-level pore st...
Embodiment 1
[0084] (1) Take 2.0 g of sulfuric acid with a mass fraction of 98%, dissolve it in 380 g of deionized water, and stir for 5 min;
[0085] (2) In the above solution, add 10.0g sucrose and 10.0g sodium chloride successively, stir continuously for 2h, and filter to obtain a clear precursor solution; the precursor solution is spray-dried in a microfluidic spray drying tower, and the inlet temperature is 195 ℃, the hot air flow rate is 255L / min, to obtain microspheres with uniform particle size, and dry for 24 hours;
[0086] (3) Roasting at 700° C. for 2 hours, with a heating rate of 2° C. / min; after that, soaking in water for 24 hours, washing and suction filtration, and vacuum drying to obtain multi-level gradient porous carbon-based sulfonic acid microspheres;
[0087](4) The porous carbon-based sulfonic acid microsphere that takes 0.6g step (3) is put into the autoclave that 10mL mass fraction is that 98% sulfuric acid is housed, and is heated at 150 ℃ for 24h; After that, was...
Embodiment 2
[0103] Steps (1)~(3) are with embodiment 1;
[0104] Step (4) Weigh 0.6 g of carbon-based solid microspheres into a reaction kettle filled with 10 ml of sulfuric acid with a mass fraction of 98%, and heat at 180° C. for 24 h. After that, it was washed with water three times, dispersed with ethanol, and dried in vacuum for 24 hours to finally obtain deeply sulfonated multi-level gradient porous carbon-based sulfonic acid microspheres with good sphericity and uniform particle size. The nitrogen analysis results show that its specific surface area is 988m 2 / g, the total acid density recorded by the acid-base back titration method is 5.88mmol / g.
[0105] Catalytic performance test of carbon-based sulfonic acid microspheres:
[0106] Take by weighing 3.204g methyl alcohol and add in the nitrogen atmosphere three-necked flask that is connected with condensed water, then add 0.056g carbon-based solid sulfonic acid microsphere catalyst, stir and disperse for 5 minutes, then add 2.8...
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