Method of preparing polymer/montmorillonid nano-composite material by montmorillonoid in-situ organization
A nanocomposite material and montmorillonite technology, which is applied in the field of montmorillonite in-situ organic preparation of polymer/montmorillonite nanocomposite materials, can solve the problems of polymer degradation, low thermal decomposition temperature, discoloration, etc. Saturated vapor pressure, improved compatibility, low volatility effects
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Embodiment 1
[0049] Take 100 ml of xylene and 0.25 g of 1-methyl-3-tetradecyl imidazolium chloride, add it to a 250 ml three-necked flask, put in a magnetic stirrer, install a reflux condenser, heat in an oil bath, and control the temperature at 40°C , stirred for 5 hours until the solution was transparent and clear, then added 0.5 g of Na-montmorillonite, and continued to stir for 24 hours to obtain a slurry of organic montmorillonite. Then, add 9.5 grams of isotactic polypropylene, heat up to 140±2°C, and stir for 24 hours. The polymer solution in the flask was poured into a large amount of ethanol while it was hot, and the precipitated floc was filtered and washed three times with deionized water and ethanol respectively, and dried in vacuum to obtain a polypropylene / montmorillonite composite material, XRD and The TEM characterization results show that the composite material is a polypropylene / montmorillonite nanocomposite material, as shown in Figures 1a and 1b.
Embodiment 2
[0055] 0.25 g of 1-methyl-3-hexadecyl tetrafluoroborate imidazolium salt was vacuum-dried at 80°C for 6 hours, 0.5 g of synthetic montmorillonite was vacuum-dried at 100°C for 6 hours, and 250 ml of dried In the three-necked flask, add a dry magnetic stirrer, add 100 ml of dry and refluxed toluene with a syringe, install a reflux condenser, and heat in a water bath under nitrogen protection to control the temperature at 50 ± 2 ° C. Stir for 24 hours to obtain Slurry of organomontmorillonite. Get a clean, dry 250 ml two-necked flask in addition, put into a dry magnetic stirrer, seal the bottle mouth with a reverse rubber stopper, after pumping three times, extract 50 ml of organic montmorillonite colloidal solution into the flask, Feed propylene gas to a pressure of 770mmHg, add 3 milliliters of MAO (1.4mol / l), 2 milliliters of Me 2 Si(Ind) 2 ZrCl 2 (1.5 μm / l), after polymerization at 40°C for about 30 minutes, acidified ethanol was added to terminate the reaction, the polym...
Embodiment 3
[0057] 0.35 g of 1-methyl-3-(4-ethyl-hexadecyl) imidazolium tetrafluoroborate was vacuum-dried at 80°C for 6 hours, and 0.5 g of mixed montmorillonite (Na-montmorillonite and Ca- The mass percentage of montmorillonite is 80 / 20) under 100 ℃, after vacuum drying for 6 hours, add in the dry three-necked flask of 250 milliliters, then add and put into dry magnetic stirrer, add 100 milliliters of dry refluxed For toluene, install a reflux condenser, under nitrogen protection, heat in a water bath, control the temperature at 50±2°C, and stir for 24 hours to obtain a slurry of organic montmorillonite. Get a clean, dry 250 ml two-necked flask in addition, put into a dry magnetic stirrer, seal the bottle mouth with a reverse rubber stopper, after pumping three times, extract the slurry liquid of 50 ml of organic montmorillonite and inject it into the flask. Introduce ethylene gas to a pressure of 770mmHg, add 2 mmol of AlEt 3 , 3 mmol of MAO (1.4 mol / l), 2 ml of Et(Ind) 2 ZrCl 2 (1....
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