Biodegradable alternate poly tetraamide diester preparation method
A polytetramide diester, biodegradable technology, applied in the field of preparation of biodegradable alternating polytetramide diester, can solve the problems of poor crystallinity, thermal properties and mechanical properties, and achieve excellent mechanical properties and good thermal properties Effect
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Embodiment 1
[0049] 1) Preparation of diamide diester: 50 parts by weight of dimethyl adipate and 3.3 parts of hexamethylenediamine, gradually from 120°C to 180°C within 5 hours under nitrogen protection, cooling, filtering, Purified by recrystallization from DMF to obtain diamide diester.
[0050] 2) Weigh 41 parts of diamide diester and 50 parts of ethanolamine in step 1) in parts by weight, gradually increase from 140°C to 180°C within 3 hours under the protection of nitrogen until the end of the reaction, recrystallize and purify with DMF to obtain Tetraamide diol—bis(ethanolamine adipyl)hexamethylenediamine, its melting point is 205~207°C.
[0051] 3) Preparation of alternating polytetraamide diester prepolymer [PreP(4A-alt-2E)-1]: Weigh 50 parts of tetraamide diol, 17.5 parts of adipic acid, 0.05 % tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 160 ℃, after collecting 80% of the generated water, use a decompression device, first use a wate...
Embodiment 2
[0054] Preparation of alternating polytetraamide diester prepolymer [PreP(4A-alt-2E)-2]: Weigh 50 parts of tetraamide diol, 21.4 parts of sebacic acid, 0.05% tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 160 °C, collect 80% of the generated water, then use a decompression device, first use a water pump to gradually depressurize the reaction for 2 hours, and then use an oil pump to depressurize to 7mmHg, Continue to react in the temperature range of 160-180°C for 3-4 hours until the acid value is basically unchanged, and the PreP(4A-alt -2E)-2 prepolymer.
[0055] Weigh 10 parts of the above-mentioned PreP(4A-alt-2E)-2 prepolymer in parts by weight, 0.13 parts of 1,4-phenyl-bis(2-oxazoline), the catalyst is 0.15% tin dichloride and 0.05% p-toluenesulfonic acid was reacted at 200°C under normal pressure for 1.5 hours under the protection of nitrogen, and the oil pump was depressurized to 5mmHg for 3 hours to prepare a biodegradable a...
Embodiment 3
[0057] Weigh 110 parts of PreP(4A-alt-2E)-110 parts in step 2) of Example 1, 0.45 parts of chain extender N,N'-adipyl biscaprolactam, 1,4-phenyl-bis( 2-oxazoline) 0.71 parts, the catalyst is 0.15% tin dichloride, reacted at 200 ° C under normal pressure for 1.5 hours under the protection of nitrogen, and reacted for 3 hours under reduced pressure (pressure 5mmHg) with an oil pump to prepare an intrinsic viscosity of 0.32dL / g of biodegradable alternating polytetramide diester.
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