Preparation method of solid mint type spice
A kind of mint type, spice technology, is applied in the preparation field of polylactate menthyl ester, achieves the effect of reducing synthesis cost
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Embodiment 1
[0022] Use D, L-LA and menthol as raw materials, mix them evenly according to the ratio of substances n(D, L-LA):n(menthol)=200:1, and pre-polymerize to remove water at 120°C, 4000Pa, 5h Intermediate I was obtained after treatment, and a catalyst zinc oxide (0.5% by mass of Intermediate I) was added, and melt polycondensation was performed at a temperature of 160° C. and a pressure of 70 Pa for 5 hours. After the reaction, the product was purified by dissolving in chloroform at room temperature, precipitated by methanol, and dried in vacuum to obtain white powdered polymenthyl lactate. The structure of the polymer was confirmed by polymer characterization methods such as infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and gel permeation chromatography. , intrinsic viscosity [η] 0.5940dL / g, the polymenthyl lactic acid ester that this method synthesizes both can be used in industries such as food, daily chemical, tobacco as solid mint type spices, also ca...
Embodiment 2
[0024] Use D, L-LA and menthol as raw materials, mix them evenly according to the ratio of substances n(D, L-LA):n(menthol)=64:1, and pre-polymerize to remove water at 130°C, 4000Pa, and 10h Intermediate I was obtained after treatment, adding catalyst zinc lactate (0.1% by mass of Intermediate I), controlled temperature 160°C and pressure 80Pa, and reacted for 10h. After the reaction, the product was dissolved in chloroform, purified by methanol precipitation, and vacuum-dried to obtain white powdered polymenthyl lactate. The structure of the polymer was confirmed by polymer characterization methods such as infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and gel permeation chromatography. The characteristics Viscosity [η] 0.4477dL / g, the polymenthyl lactate that this method synthesizes both can be used in industries such as food, daily chemical, tobacco as solid mint type spices, also can successfully prepare 5-fluorouracil sustained-release microsphere...
Embodiment 3
[0026] Using L-LA and menthol as raw materials, mix them evenly according to the amount ratio of substances n(L-LA):n(menthol)=50:1, and obtain intermediate Body I, add catalyst ferrous lactate (mass percentage is 0.5% of Intermediate I) at a temperature of 165 ° C and a pressure of 90 Pa, melt polycondensation for 3 hours. After the reaction, the product was dissolved, precipitated and purified, and vacuum-dried to obtain white powdered polymenthyl lactate. The structure of the polymer was confirmed by polymer characterization methods such as infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and gel permeation chromatography. The intrinsic viscosity [ η] 0.8462dL / g, the polymenthyl lactate that this method synthesizes both can be used in industries such as food, daily chemical, tobacco as solid mint type spices, also can be applied to ciprofloxacin drug microsphere (drug-loaded microsphere The half-life of external sustained release is 40h, and the cumu...
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