Patent ID: 12215440

EXAMPLES

Five samples of polymeric structures in the form of solid mixtures were prepared via masterbatch by mixing in the solid state in a tumbler having the quantities of the raw materials stated in Table 1. The resulting solid mixtures were metered with the aid of a K-tron metering unit via the throat to a twin-screw extruder (ZE 25UTS from Berstorff), and in this extruder converted into five polymeric structures compositions (MB01-MB05). Polyamide-based masterbatches (MB01, MB02 and MB03) were made in the extruder with a throughput of 20 kg/h at a speed of 400 rpm. The feed zone, barrel, die and outlet temperature of the material are respectively 20, 240, 240 and 300° C. Polyester-based masterbatches (MB04 and MB05) were made with a throughput of 23 kg/h at an extruder speed of 300 rpm. The feed zone, barrel, die and outlet temperature of the material are respectively 20, 260, 260 and 295° C.

TABLE 1P3P1, wt. %P2, wt. %wt. %P1-1P1-2P1-3P1-4P1-5P2-1P2-2P3-1MB0130————70——MB02——30——7.5—62.5MB03———30—7.5—62.5MB04—30————961MB05————30—961

Examples 1-10 (Ex. 1-10)

Each MB01-MB05 sample was then dissolved in decalin batches (95 wt % batch and 5 wt % decalin) of about 15 liters, stirring under N2for about 1 hour at about 110° C. to form five different suspensions (suspension I-V).

Separately, a suspension of UHMWPE powder (M-1) was obtained in decalin, with a concentration of 9 wt. % (suspension VI).

Each of suspension I-V was mixed with suspension VI in a twin-screw extruder having a screw diameter of 25 mm and being equipped with a gear pump to form a mixture. Each mixture obtained was then heated in this way to a temperature of 180° C. The mixture was then pumped through a spinneret having 64 holes, each hole having a diameter of 1 millimeter. The so obtained filaments were drawn in total with a factor of 80 and dried in a hot air oven. After drying, the filaments were bundled and wound on a bobbin.

The composition and properties of fibers obtained according to the Examples 1-10 are shown in Table 2.

Comparative Experiments A-B (CE-A, CE-B)

CE-A was performed in the same way as described for Examples 1-10, with the only difference that suspensions I-V were not used, but only suspension VI was added to the extruder to form an (unfilled) UHMWPE fiber.

CE-B: was performed in the same way as described for Examples 1-10, with the only difference that, instead of using suspensions I-V, inorganic particles of zeolite (commercially available under the tradename Ultrastable Y Zeolide, from ACS Materials, particle size distribution d50 of 6 micron) were used that was mixed with suspension VI to form a zeolite-filled UHMWPE fiber.

The composition and properties of fibers obtained according to CE A-B are shown in Table 2.

TABLE 2ModulusElongationHPPEHPPEFillerHPPEat breakfiberfiberHPPEFilleramount,fiber,HPPETiter,Tenacity,fibertypewt %cN/dtexfiber, %dtexcN/dtexCE-Anonenone1085.13.344431.7CE-Bzeolite106523.244623.7Ex. 1MB0151028.23.445032.8Ex. 2MB0110972.93.344632.1Ex. 3MB0251008.93.545232.8Ex. 4MB0210904.93.444330.2Ex. 5MB0351001.93.544432.8Ex. 6MB0310972.53.444732.2Ex. 7MB0451033.83.644133.5Ex. 8MB0410915.23.545530.9Ex. 9MB0551018.83.644533.6Ex. 10MB0510962.23.544633.0

Examples 11-22

Subsequently, the HPPE fibers obtained according to Examples 1-10 and CE-A and CE-B (Dyneema® 440-SK65 fibers) were knitted on a flat knit 13 gauge Shima Seiki knitting machine into a fabric with areal density of 260 grams per square meter in a single jersey construction.

The washed and rinsed fabrics were then subjected to coloring processes with 2 wt % based on the dry fabric of Dark Red Serilene FL dye from Yorkshire.

The dye auxiliaries (2 g/l Univadine DFM, used as diffusion agent) and then the dye were added successively to water, in a dye bath, at a temperature of 50° C. The amounts of auxiliaries and the dye where each 2 wt % based on the weight of the dry fabric. The pH was set to 4.5 using acetic acid. The rinsed fabric was then submerged in the dye bath (approximately 1 liter for 100 g fabric) and then the dye bath temperature was raised (with a rate of 0.8° C./min) to a temperature of 130° C. and kept constant at this temperature for 60 min. The bath was then cooled down rapidly (with a rate of 2° C./min) to 60° C. before the liquid was drained. The dyed fabric was successively rinsed with hot (70° C.) and cold (15° C.) water. The so obtained fabrics were air dried for 24 hours at ambient conditions.

The so obtained colored fabrics have been evaluated for color intensity as reported in Table 3.

TABLE 3ΔEcmcCrockingHPPE(CMCWetDryWash,Wash,Fabricfiber2:1)WarpWeftWarpWeftSublimation40° C.60° C.Ex. 11CE-A04-54-5442-34-53-4Ex. 12CE-B4.144-54-54434.54Ex. 13Ex. 11.704-5443-434-54-5Ex. 14Ex. 21.53443-43-4444Ex. 15Ex. 31.394443344Ex. 16Ex. 42.154-53-43-43-4444Ex. 17Ex. 51.944-53-443-4343-4Ex. 18Ex. 62.604-53333-443Ex. 19Ex. 72.504443-43-44-54Ex. 20Ex. 84.684-5443-444-54Ex. 21Ex. 92.674-543-43-43-444Ex. 22Ex. 103.604-5443-4443-4

The results obtained by applying the fiber according to the invention (Examples 1-10 and 13-22) compared with the results according to prior art (CE-A, CE-B and Ex. 11-12) clearly show that the fabrics containing the polymeric structures-filled HPPE fibers according to the present invention have good colourability and colour fastness (i.e. ΔE cmc values of higher than 1, with ΔE cmc being a known parameter used in the art and showing (visual) difference in color between fabrics; crocking and wash values of at least 3-4; and sublimation values of at least 3, see Table 3) and fiber tenacity values that remain at very high level even when increasing the amount of polymeric structures in the fiber (Table 2).