Method for preparing acetosyringone from alkali lignin at low temperatures under ethanol conditions
A technology for acetosyringone and alkali lignin, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as expensive raw materials, reduce environmental pollution, improve utilization, and expand preparation effect of source
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Embodiment 1
[0012] First, add 0.6 g of alkali lignin sample and 30 mL of absolute ethanol into the SLP miniature high-temperature and high-pressure reactor. Secondly, set the reaction temperature to 135 °C, the reaction time to 4 h, and the pressure when reaching the reaction temperature to 0 MPa. After the reaction was over, the reactor was rapidly cooled to room temperature. Next, a G5 sand core funnel was used for solid-liquid separation, and the solid-phase product was washed with high-performance liquid chromatography-grade isopropanol and tetrahydrofuran until it was colorless. Then, put the solid phase product in a constant temperature drying oven at 50°C and dry it to a constant weight, and weigh it to determine the yield of solid phase residual coke. Finally, the liquid phase product was adjusted to 100 mL with isopropanol, and 40 mL was poured into a disposable plastic petri dish, and dried in a constant temperature drying oven at 50 °C to constant weight.
Embodiment 2
[0014] First, add 0.6 g of alkali lignin sample and 30 mL of absolute ethanol into the SLP miniature high-temperature and high-pressure reactor. Secondly, set the reaction temperature at 150 °C, the reaction time at 4 h, and the pressure at the reaction temperature at 0.8 MPa. After the reaction was over, the reactor was rapidly cooled to room temperature. Next, a G5 sand core funnel was used for solid-liquid separation, and the solid-phase product was washed with high-performance liquid chromatography-grade isopropanol and tetrahydrofuran until it was colorless. Then, put the solid phase product in a constant temperature drying oven at 50°C and dry it to a constant weight, and weigh it to determine the yield of solid phase residual coke. Finally, the liquid phase product was adjusted to 100 mL with isopropanol, and 40 mL was poured into a disposable plastic petri dish, and dried in a constant temperature drying oven at 50 °C to constant weight.
Embodiment 3
[0016] First, add 0.6 g of alkali lignin sample and 30 mL of absolute ethanol into the SLP miniature high-temperature and high-pressure reactor. Secondly, set the reaction temperature at 180 °C, the reaction time at 4 h, and the pressure at the reaction temperature at 3.2 MPa. After the reaction was over, the reactor was rapidly cooled to room temperature. Next, a G5 sand core funnel was used for solid-liquid separation, and the solid-phase product was washed with high-performance liquid chromatography-grade isopropanol and tetrahydrofuran until it was colorless. Then, put the solid phase product in a constant temperature drying oven at 50°C and dry it to a constant weight, and weigh it to determine the yield of solid phase residual coke. Finally, the liquid phase product was adjusted to 100 mL with isopropanol, and 40 mL was poured into a disposable plastic petri dish, and dried in a constant temperature drying oven at 50 °C to constant weight.
[0017] It can be seen from ...
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