Catalyst for synthesizing sclareolide by oxidizing sclareol
A technology of sclareolactone and sclareol, which is applied in the field of heterocyclic compounds containing five-membered rings, can solve problems such as low reaction selectivity, potential safety hazards, and environmental pollution, and achieve the goal of avoiding environmental pollution and shortening the reaction time. Short, high catalytic activity
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Embodiment 1
[0033] The following manganese dioxide loading and tricobalt tetroxide loading were sent to the Testing Center of Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences for testing;
[0034] The detection method of following sclareol conversion rate is: adopt gas chromatography to detect and determine the quality of sclareol, the detector that adopts is hydrogen flame ionization detector, and chromatographic condition is 200 ℃ of inlet port, and detector 200 ℃, enters The sample volume is 0.5ul, the chromatographic column is HP-5 column, the initial temperature of the column is 80°C, the temperature is programmed to rise to 200°C at 10°C / min, and kept for 10min; , 0.1mol / L, 0.2mol / L, 0.2mol / L and 1.0mol / L sclareol-methyl ethyl ketone solution to make an external standard curve (external standard method), the standard curve made is a straight line (with sclareol The concentration is the abscissa, and the area of the chromatographic peak is the ordinate); the react...
Embodiment 2
[0044] The synthesis of sclareolactone, concrete steps are:
[0045] 1g of catalyst A obtained in Example 1, 100g of sclareol, 400ml of methyl ethyl ketone-water (volume ratio 1:1), 4g of sodium carbonate, and 3g of potassium bromide were successively added to a 1L glass kettle, and the stirring was started at a stirring speed of 15 rpm, adjust the heating temperature to 40 degrees, continuously feed ozone into the reactor at 40ml / min, and react for 0.5 hours to obtain sclareolactone, and the conversion rate of sclareol is over 99%. , The selectivity of sclareolide is 99%.
Embodiment 3
[0047] The preparation of the manganese dioxide-cobalt tetroxide catalyst supported by inorganic oxides comprises the following steps:
[0048] A. Put 100g of alumina in a muffle furnace, roast at 600°C for 6h under a nitrogen atmosphere, and cool to room temperature to obtain a carrier;
[0049] B. Dissolve 0.6g of manganese nitrate and 2.2g of cobalt nitrate in 10g of distilled water to obtain a mixed solution; add 10g of carrier to the mixed solution, let stand at room temperature for 6 hours, then dry at 100°C for 4 hours, and then bake at 400°C 6h, then reduced at 600°C for 3h in a carbon monoxide atmosphere;
[0050] C. Calcining the solid obtained in step B at 600°C for 3 hours in an air atmosphere; then reducing the solid obtained in step C at 400°C for 6 hours in a hydrogen atmosphere;
[0051] D. Calcining the solid obtained in step C at 600°C for 3 hours in an air atmosphere; then reducing the solid obtained in step E at 400°C for 6 hours in a carbon monoxide atmos...
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