Polymer or oligomer fibers by solvent-free electrospinning
An electrospinning and polymer technology, applied in the direction of single-component synthetic polymer rayon, fiber treatment, fiber chemical characteristics, etc., can solve the problems of low productivity, high polymer, low fiber yield, etc.
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[0121] Preparation of amidodiol ethylene-N,N"-dihydroxycaproamide (C2C)
[0122] C2C monomer was prepared by reacting 1.2 kg of ethylenediamine (EDA) with 4.56 kg of ε-caprolactone in a stainless steel reactor equipped with a stirrer and cooling water jacket under a nitrogen blanket. An exothermic condensation reaction between ε-caprolactone and EDA occurred, resulting in a gradual increase in temperature up to 80 degrees Celsius (°C). A white deposit formed and the reactor contents solidified at which point stirring was stopped. The reactor contents were then cooled to 20°C and then allowed to stand for 15 hours. The reactor contents were then heated to 140°C, at which temperature the solidified reactor contents melted. The liquid product is then drained from the reactor into a collection pan. NMR studies of the resulting product showed a C2C molar concentration of over 80% in the product. The melting point of the C2C product was determined to be 140 °C.
[0123] Exp...
Embodiment A
[0146] Example A. Preparation of prepolymer from C2C, dimethyl adipate and 1,4-butanediol. Under an inert atmosphere, a 250 mL round bottom flask was charged with titanium(IV) butoxide (0.194 g, 0.571 mmol), N,N'-1,2-ethanediyl-bis[6-hydroxycaproamide] (13.62 grams, 47.22 mmol), dimethyl adipate (65.80 grams, 0.3777 mol), and 1,4-butanediol (59.57 grams, 0.6611 mol). Polymerization was performed with overhead stirring, nitrogen / vacuum, heating, and using distillation equipment. The reaction progressed as follows: from 160°C to 175°C / at 175°C, 2.0 hours, N2; 5 minutes, 450 Torr; 10 minutes, 50 Torr; 5 minutes, 40 Torr; 10 minutes, 30 Torr; 10 minutes, 20 Torr; 10 minutes, 15 Torr; 90 minutes, 10 Torr; 1.0 hour, 0.425 Torr to 0.60 Torr. Upon cooling, the waxy solid has Tm = 51°C (55J / g); intrinsic viscosity = 0.090dL / g (chloroform / methanol (1 / 1, w / w), 30.0°C, 0.5dL / g); Mn by NMR was ~1098; and C2C incorporation by 1H-NMR was ~12 mol%.
Embodiment B
[0147] Example B. Preparation of prepolymer from A4A, dimethyl adipate and 1,4-butanediol:
[0148]
[0149] Under an inert atmosphere, a 250 mL round bottom flask was charged with titanium(IV) butoxide (0.174 g, 0.512 mmol), 7,12-diaza-6,13-dioxo-1,18-octadecanedi Dimethyl adipate (31.68 grams, 85.06 mmol), dimethyl adipate (44.45 grams, 0.2552 mol), and 1,4-butanediol (61.33 grams, 0.6805 mol). Polymerization was performed with overhead stirring, nitrogen / vacuum, heating, and using distillation equipment. The reaction progressed as follows: from 160°C to 175°C / at 175°C, 2.0 hours, N2; 5 minutes, 450 Torr; 5 minutes, 100 Torr; 10 minutes, 50 Torr; 5 minutes, 40 Torr; 10 minutes, 30 Torr; 10 minutes, 20 Torr; 10 minutes, 15 Torr; 90 minutes, 10 Torr; 1.0 hour, ~0.400 Torr. Upon cooling, the waxy solid has a bimodal Tm = 47 and 95 °C; intrinsic viscosity = 0.091 dL / g (chloroform / methanol (1 / 1, w / w), 30.0 °C, 0.5 dL / g); by 1H-NMR Mn was determined to be ~1049; and A4A inco...
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