A method for preparing crotonic acid by using levulinic acid as solvent solid acid catalytic conversion of poly-3 hydroxybutyrate
A hydroxybutyrate, solid acid catalysis technology, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problems of difficult recovery, high vapor pressure, environmental damage, etc., and achieve the effect of simple process operation
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Embodiment 1
[0031] A method for preparing crotonic acid by using levulinic acid as a solvent solid acid catalytic conversion poly-3 hydroxybutyrate, specifically as follows:
[0032] Put 6.0 g of poly-3-hydroxybutyrate, 3 g of solid acid HND-58 catalyst and 60 mL of levulinic acid into the reaction system of a 250 mL three-necked flask with a mechanical stirring and condensation device (see figure 1 ), the mechanical stirring (300 rpm) was turned on, the reaction system was heated from room temperature to 170 °C at a rate of 8 °C / min, and reacted at 170 °C for 12 hours, and the poly-3-hydroxybutyrate was completely converted. After the reaction was completed, it was cooled to room temperature, and 3.0 g of internal standard n-butanol was added to the reaction solution, and quantitatively analyzed by GC-FID (see figure 2 ) detected that the content of crotonic acid in the product was 4.0 g, so the yield of crotonic acid was 67%. Crotonic acid can be separated from levulinic acid by salti...
Embodiment 2
[0035] A method for preparing crotonic acid by using levulinic acid as a solvent solid acid catalytic conversion poly-3 hydroxybutyrate, specifically as follows:
[0036] Put 6.0 g of poly-3-hydroxybutyrate, 3 g of solid acid HND-58 catalyst and 60 mL of levulinic acid into the reaction system of a 250 mL three-necked flask with a mechanical stirring and condensation device (see figure 1 ), the mechanical stirring (300 rpm) was turned on, the reaction system was heated from room temperature to 160 °C at a rate of 8 °C / min, and reacted at 160 °C for 12 hours, and the poly-3-hydroxybutyrate was completely converted. After the reaction was completed, it was cooled to room temperature, and 3.0 g of internal standard n-butanol was added to the reaction solution. The content of crotonic acid in the product was detected by GC-FID quantitative analysis to be 2.34 g, so that the yield of crotonic acid was 39%.
Embodiment 3
[0038] A method for preparing crotonic acid by using levulinic acid as a solvent solid acid catalytic conversion poly-3 hydroxybutyrate, specifically as follows:
[0039] Put 6.0 g poly-3 hydroxybutyrate, 3 g solid acid Nafion ® NR50 catalyst and 60 mL of levulinic acid were placed in a 250 mL three-necked flask reaction system with a mechanical stirring and condensation device (see figure 1 ), turn on the mechanical stirring (300rpm), the reaction system was heated from room temperature to 150 °C at a rate of 8 °C / min, and reacted at 150 °C for 12 hours. After the reaction was completed, it was cooled to room temperature to obtain crotonic acid.
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