Method for preparing PET copolymer ester/clay nano composite material
A technology of nanocomposite materials and copolyester, which is applied in the field of preparation of PET copolyester/clay nanocomposite materials, can solve the problem of uneven dispersion of montmorillonite, and achieve the effect of improving compatibility and uniformity of dispersion
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Embodiment 1
[0024] (1) Add 50.0 g of montmorillonite with a cation exchange capacity of 100 meq / 100 g, a particle size of 200 mesh, and 4 g of trimethyl phosphate into 2000 g of deionized water, and stir at high speed for 0.5 hours to obtain an aqueous suspension A of montmorillonite. (2) 10.0 g of aminocaproic acid and 10.2 g of phosphoric acid were dissolved in 500 g of deionized water to obtain organic solution B. (3) Add B dropwise to A under stirring, keep the temperature at 80° C. for 4 hours, cool to room temperature naturally, centrifuge and wash to obtain 110 g of filter cake (solid content 48%). (4) Then, mix 110g of filter cake, 435g of caprolactam, 43.5g of aminocaproic acid, and 0.44g of adipic acid and stir at 90°C for 3 hours, continue to heat up to 260°C to start distillation and continue to react for 4 hours, pressurize and discharge, cast Belt cutting, hot water extraction, and vacuum drying to obtain nylon 6 / clay master batches with a clay content of 10%.
[0025] Add ...
Embodiment 2
[0029] Add 106g of BHET and 20g of the nylon 6 / clay nano-masterbatch prepared in Example 1 into a polycondensation reaction vessel with high-purity nitrogen, heat to 200°C, and stir for 2 hours until the nylon 6 / clay masterbatch is completely melted. Dissolve, add 0.032g of antimony trioxide, gradually raise the temperature, when the temperature rises above 240°C, start vacuuming, depressurize twice to 10-15Pa, after the temperature rises to 280°C, keep constant temperature. After continuing to react for 4 hours, the PET copolyester / clay nanocomposite material was obtained, with an intrinsic viscosity of 0.65dl / g. After XRD testing, it was found that there were no diffraction peaks below 10°, indicating that the montmorillonite sheet had been completely peeled off.
Embodiment 3
[0031] (1) Add 50.0 g of montmorillonite with a cation exchange capacity of 90 meq / 100 g, a particle size of 200 mesh, and 4 g of trimethyl phosphate into 1000 g of deionized water, and stir at high speed for 0.5 hour to obtain an aqueous suspension A of montmorillonite. (2) 25.0 g of polyvinylpyrrolidone was dissolved in 500 g of deionized water to obtain organic solution B. (3) Add B dropwise to A under stirring, keep the temperature at 90° C. for 4 hours, cool to room temperature naturally, centrifuge and wash to obtain 90 g of filter cake (solid content 51%). (4) Then, mix 90g of filter cake, 370g of caprolactam, and 37.0g of aminocaproic acid, stir at 90°C for 3 hours, raise the temperature to 260°C, start distillation and continue the reaction for 6 hours, pressurize and discharge, cast strips, cut pellets, and extract with hot water , vacuum-dried to obtain a nylon 6 / clay masterbatch with a clay content of 10%.
[0032]Add 120g of BHET and 10g of the above-mentioned ny...
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