Polymeric material
A polymer material, polycondensation technology, applied in the field of manufacturing polyether ether ketone, can solve the problem of large waste water and so on
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Embodiment 1
[0089] Example 1 - General method for the preparation of PEEK using a single monomer
[0090] DPS (132.0 g, 0.616 mol), FHPB (92.49 g, 0.300 mol) and BDF (0.87 g, 0.004 mol) were charged into a 500 ml flange flask equipped with anchor stirrer, overhead stirrer, Air intake and air condenser. After inerting with nitrogen, (this step was not essential but included here for comparison with Example 3), the mixture was heated to 160° C. and stirred at 70 rpm. Sodium carbonate (15.98 g, 0.151 mol) and potassium carbonate (0.42 g, 0.003 mol) were added slowly, and the resulting mixture was heated to 310 °C at 1 °C / min. The polymerization mixture was maintained at 310°C until the desired torque rise was achieved. At this point, the molten mixture was poured into a foil pan, allowed to cool, crushed and washed with 2 liters of acetone and then with warm water at a temperature of 40-50 °C until the conductivity of the wastewater was less than 2 μS. The resulting polymer powder was d...
Embodiment 2
[0091] Example 2 (Comparative Example) - General Procedure for Preparation of PEEK Using Sodium Salts of Single Monomers
[0092] In this comparative example, the sodium salt of FHPB was used to prepare PEEK as shown in the scheme below.
[0093]
[0094] FHPB was reacted with an equimolar amount of sodium hydroxide to produce the sodium salt, which was then polymerized in DPS without any additional sodium carbonate.
[0095] In this method, DPS (132.0 g, 0.616 mol) was charged into a 500 ml flanged flask equipped with an anchor stirrer, overhead stirrer, gas inlet and air condenser. After inerting with nitrogen, the mixture was heated to 290°C and stirred at 70 rpm. FHPB sodium salt (99.08 g, 0.300 mol) was added over 10 minutes while maintaining the temperature of the contents at 290-300°C. When the addition was complete, potassium carbonate (0.42 g, 0.003 mol) and BDF (0.87 g, 0.004 mol) were added. The resulting mixture was heated to 310°C and held at this temperatur...
Embodiment 3
[0096] Example 3 (comparative example) - General procedure for the preparation of PEEK using BDF and HQ as described in EP1879.
[0097] DPS (132.0 g, 0.616 mol), HQ (33.03 g, 0.300 mol) and BDF (66.33 g, 0.304 mol) were charged into a 500 ml flanged flask equipped with anchor stirrer, overhead stirrer, Air intake and air condenser. After inerting with nitrogen, the mixture was heated to 160 °C and stirred at 70 rpm. When the mixture melted, sodium carbonate (31.96 g, 0.302 mol) and potassium carbonate (0.83 g, 0.006 mol) were added slowly, and the resulting mixture was heated to 310 °C at 1 °C / min. The polymerization mixture was maintained at 310°C until the desired torque rise was achieved. Next, the reaction mixture was poured into foil pans, allowed to cool, crushed and washed with 2 liters of acetone and then with warm water at a temperature of 60-70 °C until the conductivity of the wastewater was less than 2 μS. The resulting polymer powder was dried at 120°C in an ai...
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