Method for lactide synthesis from lactic acid catalysized by montmorillonite
A technology for catalyzing lactic acid and lactide with montmorillonite, which is applied in the chemical field, can solve the problem of no lactide being found, and achieve the effects of high yield, wide source of raw materials, and short time consumption
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Embodiment 1
[0017] Embodiment 1: Add 50gD in the 250ml three-necked round-bottomed flask that is equipped with thermometer, and place in magnetic stirrer, temperature rises to 60 ℃, and vacuum degree is controlled at 0.001MPa decompression distillation removes free in lactic acid. Water; after about 2.5 hours, the water is basically evaporated, add D,L-lactic acid acidified montmorillonite with 0.01% acetic acid, slowly raise the temperature to 80°C, and reduce the pressure to 1.0×10 -4 The dehydration was continued for 3 hours under MPa, and polylactic acid with low molecular weight was generated; the water condenser was replaced with an air condenser, and the round bottom flask was connected twice, the temperature was raised to 170 °C, and the pressure was raised to 6.0×10 -5 MPa, the nitrogen flow rate is controlled at 1L / min, react for 2 hours to generate crude lactide; wash the crude lactide with distilled water, recrystallize 2-5 times with ethyl acetate, and then put it in a vacuum ...
Embodiment 2
[0018] Embodiment 2: Add 50gD in the 250ml three-necked round-bottomed flask that is equipped with thermometer, and place in magnetic stirrer, temperature rises to 70 ℃, and vacuum degree is controlled at 0.005MPa decompression distillation removes free in lactic acid. Water; after about 2.5 hours, the water is basically evaporated, add D,L-lactic acid acidified montmorillonite with 0.03% phosphoric acid, slowly raise the temperature to 100°C, and reduce the pressure to 5.0×10 -4 Continue dehydration for 1 hour at MPa to generate polylactic acid with low molecular weight; replace the water condenser with an air condenser, connect the round bottom flask twice, raise the temperature to 180°C, and the pressure to 1.0×10 -4 MPa, the nitrogen flow rate is controlled at 1.5L / min, react for 6 hours to generate crude lactide; wash the crude lactide with distilled water for several times, then recrystallize with ethyl acetate for 2-5 times, and put it in a vacuum at 50°C Drying in a dr...
Embodiment 3
[0019] Embodiment 3: Add 50g D, L-lactic acid in the 250ml three-necked round bottom flask that is equipped with thermometer, and place in magnetic stirrer, temperature rises to 80 ℃, and vacuum degree is controlled at 0.005MPa Reduced pressure distillation removes in lactic acid Free water; after about 2.5 hours, the water is basically evaporated, add D,L-lactic acid acidified montmorillonite with 0.05% sulfuric acid, slowly raise the temperature to 120°C, and reduce the pressure to 7.0×10 -4 Continue dehydration at MPa for 2 hours to produce polylactic acid with low molecular weight; replace the water condenser with an air condenser, connect the round bottom flask twice, raise the temperature to 200°C, and the pressure to 3.0×10 -4 MPa, the nitrogen flow rate is controlled at 2.0L / min, react for 5 hours to generate crude lactide; wash the crude lactide with distilled water, recrystallize it with ethyl acetate for 2-5 times, and put it in a vacuum oven at 50°C Drying in mediu...
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