Microspheric ionomer having crosslinking structure, and preparation method and application thereof
A technology of cross-linked structure and ionomer is applied in the field of microspherical ionomer and its preparation, and achieves the effect of simple preparation process and better nucleation effect
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[0031] The method for preparing ionomer provided by the invention comprises:
[0032] (1) In an organic solvent, in the presence of an initiator, maleic anhydride, monomer B and a crosslinking agent that provide structural unit B shown in formula (2) are contacted to react;
[0033] (2) In the presence of water, the product obtained in step (1) is reacted with an alkali to carry out salification (or hydrolysis).
[0034] In step (1) of the present invention, there is no special requirement to the consumption of each raw material used, preferably, relative to the maleic anhydride of 100mol, the consumption of monomer B is 50-150mol, more preferably 75-100mol. Those skilled in the art can understand that maleic anhydride is a substance that provides the structural unit A represented by formula (1). Monomer B is a substance that provides structural unit B represented by formula (2), and may be α-methylstyrene or styrene.
[0035] Preferably, relative to 100 mol of maleic anhydr...
Embodiment 1
[0051] This example is used to illustrate the microspherical ionomer (or ionomer microsphere) with a cross-linked structure of the present invention and its preparation method.
[0052] (1) Dissolve 100g of maleic anhydride, 118g of α-methylstyrene, 26g of divinylbenzene, and 2g of azobisisobutyronitrile in 1000mL of isoamyl acetate, and react at 70°C for 5 hours under a nitrogen atmosphere . The reacted system was centrifuged by a centrifuge at 5000 rad / min for 30 minutes to obtain cross-linked α-methylstyrene / maleic anhydride polymer microspheres, which were washed and purified with n-hexane and dried in vacuum.
[0053] At the same time, the supernatant after centrifugation is analyzed by LC-MC to measure the amount of remaining monomer, which is obtained by subtracting the amount of monomer (or cross-linking dose) from the input monomer amount (or cross-linking dose). The amount of monomer (or cross-linking dose) that actually participates in the reaction, thereby obtaini...
Embodiment 2
[0056] This example is used to illustrate the ionomer microspheres of the present invention and its preparation method.
[0057] (1) Dissolve 100g of maleic anhydride, 118g of α-methylstyrene, 26g of divinylbenzene, and 2g of azobisisobutyronitrile in 1000mL of isoamyl acetate, and react at 70°C for 5 hours under a nitrogen atmosphere . The reacted system was centrifuged by a centrifuge at 5000 rad / min for 30 minutes to obtain cross-linked α-methylstyrene / maleic anhydride polymer microspheres, washed with methanol, purified, and dried in vacuum.
[0058] (2) 20.5 g of sodium acetate is dissolved in 300 mL of water, and 50 g of cross-linked α-methylstyrene / maleic anhydride polymer microspheres are added to aqueous sodium acetate (relative to the maleic anhydride per mole, the amount of alkali is 1.2 mol) at 100°C for 4 hours. The reacted system was centrifuged under the condition of 5000rad / min for 30 minutes, the solid was stirred and washed with 400mL water, centrifuged und...
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