A kind of catalyst for preparing γ-valerolactone from furfural, its preparation method and preparation method of γ-valerolactone
A catalyst, valerolactone technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high price, easy deactivation, high price, etc., and achieve the effect of wide sources and cost reduction
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[0040] The present invention also provides a kind of preparation method of the catalyst that furfural prepares gamma-valerolactone, comprises the following steps:
[0041] A) dispersing the zirconium source compound and the carbon nitrogen source compound in deionized water, heating and stirring to obtain a transparent liquid;
[0042] B) dispersing the Hβ molecular sieve in the above transparent liquid to obtain a suspension;
[0043] The mass ratio of the zirconium source compound, carbon nitrogen source compound and Hβ molecular sieve is 3:10:50~1:10:50;
[0044] C) continuously heating and stirring, and evaporating the suspension to dryness to obtain a suspension;
[0045] D) drying and grinding the obtained suspension, and calcining it under a nitrogen atmosphere to obtain a catalyst.
[0046] First, the zirconium source compound and the carbon nitrogen source compound are dispersed in an appropriate amount of water, heated and stirred to obtain a transparent liquid.
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Embodiment 1
[0075] Zr-C 3 N 4 The preparation method of -Hβ:
[0076] Add 0.02g of zirconium oxychloride octahydrate and 0.2g of dicyandiamide into 15mL of deionized water, heat and stir at 100°C, add 1.0g of Hβ after the solid is completely dissolved, continue heating and stirring at 100°C until the liquid is completely evaporated to dryness. The resulting solid was transferred to a mortar for grinding, and then dried overnight in a vacuum oven at 25°C. The obtained powder samples were calcined at 600 °C for 4 h under a flowing nitrogen atmosphere, and the temperature was raised at a rate of 5 °C / min. Zr-C 3 N 4 The scanning electron microscope image of -Hβ is as follows figure 1 shown.
Embodiment 2
[0081] The Zr-C prepared by 0.1g embodiment 1 3 N 4 -Hβ catalyst was added to a 15mL thick-walled pressure-resistant tube, then 0.2g of furfural was added, and finally 5mL of isopropanol was added, and the thick-walled pressure-resistant tube with the cap tightly tightened was placed in an oil bath at a set temperature of 160°C , adjust the stirring rate to 600rpm, and start timing when the temperature reaches 160°C again. After 18 hours, the thick-walled pressure-resistant tube was removed from the oil bath and rapidly cooled to room temperature. Add 50 microliters of internal standard substance to the mixed solution, mix well, filter, and detect the product content by gas chromatography.
[0082] The detection conditions are: Agilent 7820A, Agilent HP-5 capillary column, detector is FID, furnace temperature is 50°C for 3 minutes, the temperature is raised to 280°C at 10°C / min and kept for 10 minutes, nitrogen is used as the carrier gas.
[0083] The results showed that un...
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