Method for preparing polymeric micron/nanometer spherical particle
A technology of micro-nano spheres and polymers, which is applied in the field of preparing micro-nano spheres, can solve the problems of wide distribution of micellar particle size and complicated process, and achieves the effects of low cost, simple steps and good prospects for large-scale production.
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Embodiment 1
[0027] (1) get the block copolymer of 5g polystyrene and polybutadiene (polybutadiene volume ratio is 30%) and dissolve in 45g toluene, obtain the solution that polymer weight ratio is 10%;
[0028] (2) Add 1 mol of formic acid and hydrogen peroxide in a three-necked flask, and react for half an hour at 70° C. to make peroxyformic acid; Add 2mol formic acid to continue the reaction for 3h after the end of the reaction;
[0029] (3) Add methanol to the obtained hydroxylated product for precipitation, then filter, and repeat the operation 3 times. Take out the final polymer and dry it in a vacuum oven at 70°C for 12 hours;
[0030] (4) Take 0.05 g of the dried hydroxylated product in a hydrothermal reaction kettle, and add 9.95 g of acetic acid, so that the polymer mass ratio is 0.5%;
[0031] (5) The obtained sample was heat-treated at 150° C. for 15 hours to obtain polymer micro-nano spheres with narrow particle size distribution. The scanning electron micrographs of the ob...
Embodiment 2
[0033] (1) get the block copolymer of 5g polystyrene and polybutadiene (polybutadiene volume ratio is 30%) and dissolve in 45g toluene, obtain the solution that polymer weight ratio is 10%;
[0034] (2) Add 1 mol of formic acid and hydrogen peroxide in a three-necked flask, and react for half an hour at 70° C. to make peroxyformic acid; Add 2mol formic acid to continue the reaction for 3h after the end of the reaction;
[0035] (3) Add methanol to the obtained hydroxylated product for precipitation, then filter, and repeat the operation 3 times. Take out the final polymer and dry it in a vacuum oven at 70°C for 12 hours;
[0036] (4) Take 0.05 g of the dried hydroxylated product in a hydrothermal reaction kettle, and add 9.95 g of acetic acid, so that the polymer mass ratio is 0.5%;
[0037] (5) Heat the obtained sample at 100° C. for 15 hours to obtain polymer micro-nano spheres with narrow particle size distribution. The scanning electron micrographs of the obtained spher...
Embodiment 3
[0039] (1) get 5g polystyrene-butadiene-styrene triblock copolymer (polybutadiene volume is 35%) and dissolve in 25g tetrahydrofuran, obtain the solution that polymer weight ratio is 16.7%;
[0040] (2) Add 10g potassium permanganate and 20g polymer solution to react for 4h in a three-necked flask;
[0041] (3) Add ethanol to the obtained hydroxylated product for precipitation, then filter, and repeat the operation 3 times. Remove the final polymer and dry it in a vacuum oven at 60°C for 15 hours;
[0042] (4) Take 0.1 g of the dried hydroxylated product in a hydrothermal reaction kettle, and add 29.9 g of formic acid, so that the weight ratio of the polymer is 0.33%;
[0043] (5) Heat the obtained sample at 100° C. for 4 hours to obtain polymer micro-nano spheres with narrow particle size distribution.
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Abstract
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