WO2022111040A1 - Functional polyamide 56 filament and manufacturing method therefor - Google Patents
Functional polyamide 56 filament and manufacturing method therefor Download PDFInfo
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- WO2022111040A1 WO2022111040A1 PCT/CN2021/121258 CN2021121258W WO2022111040A1 WO 2022111040 A1 WO2022111040 A1 WO 2022111040A1 CN 2021121258 W CN2021121258 W CN 2021121258W WO 2022111040 A1 WO2022111040 A1 WO 2022111040A1
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- polyamide
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 139
- 229920002647 polyamide Polymers 0.000 title claims abstract description 139
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000009987 spinning Methods 0.000 claims abstract description 34
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 238000004804 winding Methods 0.000 claims abstract description 23
- 238000001291 vacuum drying Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 15
- 125000003277 amino group Chemical group 0.000 claims abstract description 11
- 238000009998 heat setting Methods 0.000 claims abstract description 9
- 238000007664 blowing Methods 0.000 claims abstract description 8
- 238000002074 melt spinning Methods 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000004043 dyeing Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical group N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 13
- 239000003063 flame retardant Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 241001589086 Bellapiscis medius Species 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 230000006855 networking Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000012216 screening Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 101000765308 Aspergillus niger N-(5'-phosphoribosyl)anthranilate isomerase Proteins 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 241001136494 Talaromyces funiculosus Species 0.000 description 2
- 241000223261 Trichoderma viride Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 2
- 238000010622 cold drawing Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 229920006021 bio-based polyamide Polymers 0.000 description 1
- 229920013724 bio-based polymer Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 238000010036 direct spinning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Definitions
- the invention relates to a functional polyamide 56 filament and a preparation method thereof, belonging to the field of textiles.
- Polyamide fiber is nylon, also known as polyamide in our country.
- Polyamide is the second largest synthetic fiber after polyester fiber. Due to its high breaking strength, wear resistance, fatigue resistance, light weight and softness, breathability and moisture absorption, and good elasticity, it is widely used in textiles, engineering plastics, military products, Rubber frame materials, ropes, nets, ropes, tarpaulins, industrial filter cloths and silk for high-grade sewing threads have good market prospects.
- Polyamides are prepared by condensation reactions between diamines and diacids.
- polyamide fibers are basically prepared from petroleum derivatives, such as polyamide 6 and polyamide 66, which have the largest market share.
- Their raw materials, caprolactam and adipic acid are hydrogenated by benzene homologues. It is prepared by a series of reactions such as oxidation, and hexamethylene diamine is prepared by first synthesizing adiponitrile from butadiene or acrylonitrile and then by catalytic hydrogenation. Currently, it is prepared by petrochemical methods.
- melt spinning is the most commonly used spinning method, which is divided into melt direct spinning and chip spinning. Melt spinning does not require solvent, it can be directly spun, the process is simple, the cost is low, and there is no solvent recovery problem.
- the invention relates to a functional polyamide 56 filament, which belongs to a novel bio-based polymer product.
- the raw material, pentamethylene diamine is mainly prepared by a biological fermentation method, and then synthesized with adipic acid to obtain a bio-based polyamide 56 polymer.
- the preparation method of a functional polyamide 56 filament provided by the invention comprises the following technological process:
- Filament post-processing the polyamide 56 tow is subjected to thermal drawing, heat setting and winding, or a texturing process to obtain functional polyamide 56 filaments.
- the index of described functional polyamide 56 slices is as follows:
- the slice viscosity index is 145-180 ml/g
- the slice viscosity index is 135-160 ml/g
- the amino group content index at the end of the slice is 40-70 mmol/kg
- the amino group content index at the end of the slice is 30-55 mmol/kg.
- the index of the described functional polyamide 56 slices after the segmental vacuum drying described in step 1) is as follows:
- the water content of the slices is ⁇ 600ppm; the melting point is 245 ⁇ 260°C.
- the temperature of each zone of the screw of the spinning box the temperature of each zone of the screw: 260-290 °C in the first zone, 260-290 °C in the second zone, 260-290 °C in the third zone, 260-290 °C in the fourth zone, and 5.
- the spinning speed is specifically 3000m/min ⁇ 4500m/min;
- the cooling mode of air blowing by ring blowing or side blowing is adopted, and the conditions are as follows: wind speed: 30 ⁇ 60m/min; wind temperature: 18 ⁇ 26 °C; wind pressure: 350Pa ⁇ 600Pa;
- the mass concentration of the oiling agent is 3% to 5%.
- the temperature of the cooling drafting roll is 0-20°C, and the drafting ratio is 1.05-1.45.
- the hot drawing process can be one-stage drafting, two-stage drafting or multi-stage drafting, and the process conditions: the drafting ratio is 1.01 ⁇ 5.50, and the drafting temperature is 80 ⁇ 200 °C ;
- high-strength polyamide 56 filaments are prepared with a draw ratio of 3.00 to 5.50.
- the texturing process includes a process for preparing functionalized polyamide 56 drawn textured yarn and a process for preparing functionalized polyamide 56 air-textured yarn.
- the process for preparing the functionalized polyamide 56 stretched textured yarn includes the steps of hot drawing, twisting, networking, heat setting and winding, and the conditions are as follows:
- the hot drafting temperature is 100 ⁇ 200°C, the drafting ratio is 1.10 ⁇ 2.50, the speed of the drafting roller is 300 ⁇ 1000m/min; the twisting is divided into S twist or Z twist, the twisting tension is 20 ⁇ 60cN, and the untwisting tension is 25 ⁇ 65cN, D/Y is the ratio of the surface speed of the friction disc and the speed of the thread leaving the false twister, specifically 1.5 ⁇ 2.0; in the network step, the wind pressure is 1.0 ⁇ 1.6bar; the diameter of the nozzle is 1.2 ⁇ 1.6mm, The heat setting temperature is 180 ⁇ 220°C, and the winding speed is 600 ⁇ 1200m/min.
- the process for preparing the functionalized polyamide 56 air-textured yarn includes the steps of thermal drawing, thermal jet texturing, cooling stabilization and winding.
- the conditions are as follows:
- the hot drawing temperature is 100 ⁇ 190°C, the drawing ratio is 1.05 ⁇ 3.50, the speed of the drafting roller is 1500 ⁇ 2500m/min; The rate is 15-30%, the cooling air temperature is 15-30°C, and the winding speed is 1500-2800 m/min.
- Breaking strength and breaking elongation GB/T 14344-2008 Test method for tensile properties of chemical fiber filaments
- Anti-mildew properties GB/T 24346-2009 Evaluation of anti-mildew properties of textiles;
- R2071 network degree meter is used, according to FZ/T 50001 synthetic fiber filament network degree test method
- the viscosity index of functional slices is 163ml/g, and the amino group content is 36.4mmol/kg.
- the vacuum drying process of slices is as follows: first dry at 50°C for 12h, then heat up to 85°C for 8h, and then heat up to 110°C It was dried for 6h under the condition of 130°C and kept at 130°C for 5h. After drying, the functional chips contained 427 ppm of water and a melting point of 256°C.
- the spinning speed 4250m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder.
- the fourth zone is 288°C
- the fifth zone is 288°C
- the temperature of the box is 288°C
- the temperature of the metering pump is 288°C
- the speed of the metering pump is 14rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 21°C, and the wind pressure is 430Pa, and then the strands are oiled with a concentration of 3% oil, and then cold-drawn at 5°C for 1.23 times to obtain polyamide 56 strands bundle.
- the polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 4.53, the second-drawing multiple is 1.12, the first-drawing temperature is 110 °C, the second-drawing temperature is 175 °C, and then heat-set at 185 °C, 3800m/min winding, High-strength polyamide 56 filaments were obtained.
- the breaking strength of the high-strength polyamide filament is 8.45cN/dtex, the elongation at break is 33.7%, the moisture regain is 4.36%, and the limiting oxygen index is 35.5%.
- the viscosity index of the functional chips is 148ml/g, and the amino group content is 36.4mmol/kg.
- the vacuum drying process is as follows: first dry at 60°C for 10h, then heat up to 95°C for 8h, and then heat up to 115°C. Condition drying for 5h, continue to keep at 140 °C for 3h. After drying, the slices have a water content of 302 ppm and a melting point of 254 °C.
- the spinning speed 3650m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder.
- the four zones are 290°C, the fifth zone is 290°C, the box temperature is 290°C, the metering pump temperature is 290°C, and the metering pump speed is 16rpm. It solidifies into strands, the cooling wind speed is 60m/min, the wind temperature is 18°C, and the wind pressure is 360Pa, and then the strands are oiled with an oil concentration of 3%, and then cold-drawn at 15°C for 1.35 times to obtain a polyamide 56 tows.
- the polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 4.13, the second-draw multiple is 1.25, the first-draw temperature is 130°C, and the second-draw temperature is 180°C, and then heat-set at 190°C and wound at 3500m/min, High-strength polyamide 56 filaments were obtained.
- the breaking strength of the high-strength polyamide filament is 7.83cN/dtex, the elongation at break is 37.7%, the moisture regain is 4.28%, and the limiting oxygen index is 34.7%.
- the viscosity index of functional slices is 142ml/g.
- the vacuum drying process is as follows: first dry at 60°C for 12h, then heat up to 90°C for 8h, then heat up to 105°C for 5h, and continue to dry at 105°C for 5 hours. Incubate at 135°C for 4h. After drying, the sliced slices have a water content of 447 ppm and a melting point of 255°C.
- the spinning speed 3100m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder.
- the four zone is 286°C
- the fifth zone is 286°C
- the temperature of the box is 286°C
- the temperature of the metering pump is 286°C
- the speed of the metering pump is 14rpm. It solidifies into strands, the cooling wind speed is 45m/min, the wind temperature is 23°C, and the wind pressure is 450Pa, then the strands are oiled with an oil concentration of 3%, and then cold drawn at 10°C for 1.18 times to obtain a polyamide 56 tows.
- the polyamide 56 tow is subjected to two-stage drafting, the first-drawing multiple is 3.68, the second-drawing multiple is 1.02, the first-drawing temperature is 80 °C, the second-drawing temperature is 165 °C, and then heat-set at 175 °C, 2400m/min winding, A flame retardant polyamide 56 filament was obtained.
- the breaking strength of the flame-retardant polyamide filament is 5.18cN/dtex, the elongation at break is 34.2%, the moisture regain is 4.48%, and the limiting oxygen index is 37.3%.
- the viscosity index of functional slices is 137.7ml/g.
- the vacuum drying process is as follows: first dry at 40°C for 12h, then heat up to 80°C for 8h, then heat up to 105°C for 6h, and continue Incubate at 135°C for 5h.
- the sliced slices have a water content of 579 ppm and a melting point of 253°C.
- the spinning speed 2000m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder.
- the four zone is 287°C
- the fifth zone is 287°C
- the temperature of the box is 287°C
- the temperature of the metering pump is 287°C
- the speed of the metering pump is 13rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 21°C, and the wind pressure is 480Pa, then the strands are oiled with an oil concentration of 5%, and then cold-drawn at 0°C for 1.30 times to obtain a polyamide 56 tows.
- the polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 3.30, the second-drawing multiple is 1.15, the first-drawing temperature is 100 °C, the second-drawing temperature is 170 °C, and then heat-set at 180 °C, 1800m/min winding, A flame retardant polyamide 56 filament was obtained.
- the breaking strength of the flame-retardant polyamide filament is 4.99cN/dtex, the elongation at break is 40.4%, the moisture regain is 4.37%, and the limiting oxygen index is 36.4%.
- the content of terminal amino group of functional slices is 68.8mmol/kg.
- the vacuum drying process is as follows: first drying at 55°C for 10h, then heating to 90°C for 10h, and then heating to 110°C for 6h , and continue to incubate at 130 °C for 5 h. After drying, the slices have a water content of 363 ppm and a melting point of 249°C.
- the temperature of the four zone is 283°C
- the zone five is 283°C
- the temperature of the box is 283°C
- the temperature of the metering pump is 283°C
- the speed of the metering pump is 15rpm. It solidifies into strands, the cooling wind speed is 48m/min, the wind temperature is 20°C, and the wind pressure is 460Pa, and then the strands are oiled with an oil concentration of 3%, and then cold-drawn at 10°C for 1.28 times to obtain a polyamide 56 tows.
- the polyamide 56 tow is subjected to two-stage drawing, the first-drawing ratio is 3.11, the second-drawing ratio is 1.10, the first-drawing temperature is 100 °C, the second-drawing temperature is 185 °C, and then heat-set at 200 °C, 1300m/min winding, Easy-dyeing polyamide 56 filaments were obtained.
- the breaking strength of the easily dyed polyamide filament is 4.63cN/dtex, the elongation at break is 51.1%, the moisture regain is 4.51%, the limiting oxygen index is 32.1%, and the dyeing rate is 99.2%.
- the amino-terminal content of functional slices is 68.8 mmol/kg.
- the vacuum drying process is as follows: first drying at 55°C for 12h, then heating to 95°C for 10h, and then heating to 115°C for 6h , and kept at 140°C for 4h. After drying, the slices have a water content of 398 ppm and a melting point of 253°C.
- the polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 3.00, the second-drawing multiple is 1.10, the first-drawing temperature is 100 °C, the second-drawing temperature is 160 °C, and then heat-setting at 180 °C, 1000m/min winding, Easy-dyeing polyamide 56 filaments were obtained.
- the breaking strength of the easily dyeable polyamide filament is 4.60cN/dtex, the elongation at break is 51.4%, the moisture regain is 4.44%, the limiting oxygen index is 32.2%, and the dyeing rate is 99.5%.
- the amino content of functional slices is 32.4mmol/kg.
- the vacuum drying process is as follows: first dry at 55°C for 10h, then heat up to 90°C for 10h, then heat up to 110°C for 6h, and continue Incubate at 130°C for 5h. After drying, the slices had a water content of 412 ppm and a melting point of 251°C.
- the polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 2.30, the second-draw multiple is 1.15, the first-draw temperature is 80 °C, and the second-draw temperature is 155 °C, and then heat-set at 165 °C, 900m/min winding, Mildew-resistant polyamide 56 filaments were obtained.
- the anti-fungal properties of the filament were evaluated, wherein the concentration of mixed spore solution: 1.2 ⁇ 106 CFU/mL, and the molds used for detection were Aspergillus niger AS 3.4463, Penicillium funiculosum AS 3.3875, globosa ( chaetoomium globsum) AS 3.4254, Trichoderma viride AS 3.2942.
- the breaking strength of the mildew-resistant polyamide filament is 4.34 cN/dtex, the elongation at break is 58.2%, the moisture regain is 4.53%, the limiting oxygen index is 32.3%, and the mildew resistance is grade 0.
- the amino content of functional slices is 42.4 mmol/kg.
- the vacuum drying process is as follows: first dry at 50 °C for 10 hours, then heat up to 90 °C for 8 hours, then heat up to 110 °C for 5 hours, and continue Incubate at 130°C for 3h. After drying, the slices have a water content of 362 ppm and a melting point of 251°C.
- the spinning speed 1000m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder.
- the four zones are 280°C, the fifth zone is 280°C, the box temperature is 280°C, the metering pump temperature is 280°C, and the metering pump speed is 15rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 23°C, and the wind pressure is 420Pa, then the strands are oiled with an oil concentration of 4%, and then cold drawn at 0°C for 1.08 times to obtain polyamide 56 tows.
- the polyamide 56 tow is subjected to two-stage drafting, the first-drawing multiple is 3.03, the second-drawing multiple is 1.10, the first-drawing temperature is 110 °C, the second-drawing temperature is 180 °C, and then heat-set at 200 °C, 900m/min winding, Mildew-resistant polyamide 56 filaments were obtained.
- the anti-mildew performance of the filament was evaluated, wherein the concentration of mixed spore solution: 1.2*106 CFU/mL, and the molds used for the detection were Aspergillus niger AS 3.4463, Penicillium funiculosum AS 3.3875, globosa ( chaetoomium globsum) AS 3.4254, Trichoderma viride AS 3.2942.
- the breaking strength of the mildew-resistant polyamide filament is 4.41 cN/dtex, the elongation at break is 50.7%, the moisture regain is 4.33%, the limiting oxygen index is 33.8%, and the mildew resistance is grade 0.
- the viscosity index of the functional slices was 144.1 ml/g, and the vacuum drying process was the same as that in Example 3. After drying, the slices had a water content of 584 ppm and a melting point of 251°C.
- the obtained polyamide 56 tow was drawn 2.00 times under the condition of 180 ° C, the speed of the drawing roller was 800 m/min, and the filament was S-twisted after drawing, the twisting tension was 45cN, and the untwisting tension was 48cN; the D /Y is 1.8, network air pressure is 1.2 bar; nozzle diameter is 1.3 mm, heat setting temperature is 190° C., and the winding speed is 900 m/min.
- the breaking strength of the flame retardant polyamide stretched textured yarn is 5.38cN/dtex, the elongation at break is 34.2%, the moisture regain is 4.26%, the limiting oxygen index is 37.8%, and the degree of network (the number of nodes) is 101.
- the terminal amino group value of the functional slice is 63.1 mmol/kg, and the vacuum drying process is the same as that in Example 5. After drying, the slice contains 412 ppm of water and has a melting point of 251°C.
- the process parameters of spinning, cold drawing and hot drawing are the same as those in Example 5, and the drawn polyamide 56 tow is obtained.
- the tow was thermally drawn at 160°C by 1.10 times, the thermal jet deformation temperature was 230°C, the air jet pressure was 300kPa, the overfeed rate was 25%, the cooling air temperature was 15°C, and the winding speed was 1400m/min.
- An easily dyeable polyamide 56 air textured yarn was obtained.
- the breaking strength of the easily dyeable polyamide air-textured yarn is 5.13cN/dtex, the elongation at break is 46.1%, the moisture regain is 4.32%, the limiting oxygen index is 33.4%, and the dyeing rate is 99.4%.
- the vacuum drying process of the slices is as follows: firstly, dry at 120°C for 24h.
- the slices were slightly yellowed, the viscosity index was 118.6 ml/g, the amino group content was 19.1 mmol/kg, the water content of the slices was 372 ppm, and the melting point was 251°C.
- the polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 2.0, the second-draw multiple is 1.10, the first-draw temperature is 80°C, and the second-draw temperature is 150°C, and then heat-set at 165°C, 600m/min winding, Polyamide 56 filaments were obtained.
- the properties of the comparative example filaments breaking strength 2.87cN/dtex, breaking elongation breaking elongation 86.8%, moisture regain 4.21%, limiting oxygen index 22.3%.
- the filament has high breaking strength; when the viscosity index and the terminal amino value are within a certain range, the limiting oxygen index of the filament is high, and the flame retardant performance is good; when the amino value of the slice end is high, the low-temperature dyeing performance of the filament is significantly better than other Filament prepared under conditions; when the amino value of slices is within a certain range, the filament has anti-mildew properties.
- the high-temperature vacuum drying process was used, and the chips with low viscosity index and terminal amino value were selected. Under the condition of low-speed spinning, polyamide 56 filament and textured yarn were prepared by low-drawing. The results showed that the breaking strength and limit of the product were Oxygen index and dye uptake are not as good as the filament products of the examples.
- the moisture in the polyamide 56 slices is removed by a segmented vacuum drying process, which reduces the defects such as thermal degradation of the slices, decreased viscosity, and deepened color, and at the same time improves the crystallinity of the slices, which is helpful for uniform and stable spinning;
- Spinning The cooling and drawing process is added to the silk process. This is because the cooling crystallization rate of polyamide 56 is found to be slow in the research, and the incompletely cooled tow not only affects the winding and oiling process, but also directly draws and shapes the product. The mechanical properties are unstable. Therefore, adding a cooling drafting process to rapidly cool the tow formed by the spinneret is beneficial to the subsequent high-stretching to obtain polyamide filaments with stable performance and excellent performance.
- Polyamide 56 filaments and textured yarns with excellent mechanical properties, flame retardant properties, dyeing properties, and mildew resistance can be prepared according to different viscosity, terminal amino group, draft ratio and other indicators to meet the use in special environments. requirements, widely used in all walks of life.
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Abstract
Disclosed are a functional polyamide 56 filament and a manufacturing method therefor. The manufacturing method comprises the following steps: 1) chip drying: segmented vacuum drying treatment is performed on a selected functional polyamide 56 chip; 2) melt spinning: the dried chip is ejected from a screw extruder and a spinneret of a spinning box to obtain a thin stream of melt, the thin stream of melt is cooled by blowing air and solidified into strands; after being bundled and oiled, the strands are cooled and drafted to obtain a polyamide 56 tow; and 3) filament post-processing: the tow is subjected to heat drafting, heat setting, and winding of different processes to obtain a functional polyamide 56 filament. 1) The segmented vacuum drying process can reduce chip damage and achieve uniform spinning; 2) the cooling and drafting process is beneficial to high-power drafting to obtain a filament having stable performance; 3) by screening indicators such as a viscosity index and a terminated amino group of the chip and adjusting the drafting process, the polyamide 56 filament and textured yarn having excellent performance can be manufactured, thereby satisfying use requirements in a special environment, and being widely applied to various industries.
Description
本发明涉及一种功能性聚酰胺56长丝及其制备方法,属于纺织领域。The invention relates to a functional polyamide 56 filament and a preparation method thereof, belonging to the field of textiles.
聚酰胺(PA)的重复单元(单体)具有酰胺基团作为特征性特征。聚酰胺纤维即尼龙,在我国也称为聚酰胺。聚酰胺是产量仅次于聚酯纤维的第二大合成纤维,由于其断裂强度高、耐磨、耐疲劳、轻质柔软、透气吸湿、弹性好等特点,在纺织、工程塑料、军工产品、橡胶骨架材料、绳、网、索类、篷布、工业滤布以及在高档缝纫线用丝等领域拥有良好的市场前景。The repeating units (monomers) of polyamide (PA) have amide groups as a characteristic feature. Polyamide fiber is nylon, also known as polyamide in our country. Polyamide is the second largest synthetic fiber after polyester fiber. Due to its high breaking strength, wear resistance, fatigue resistance, light weight and softness, breathability and moisture absorption, and good elasticity, it is widely used in textiles, engineering plastics, military products, Rubber frame materials, ropes, nets, ropes, tarpaulins, industrial filter cloths and silk for high-grade sewing threads have good market prospects.
聚酰胺是通过二胺和二酸之间的缩合反应来制备。目前的聚酰胺纤维基本上都是有以石油的衍生物为原料制备,例如市场占有量最大的聚酰胺6和聚酰胺66,它们的原料己内酰胺和己二酸是通过苯类同系物经过加氢再氧化等一系列反应制得,己二胺是通过丁二烯或丙烯腈先合成己二腈再通过催化加氢方法制备,目前均由石油化工方法制备。Polyamides are prepared by condensation reactions between diamines and diacids. At present, polyamide fibers are basically prepared from petroleum derivatives, such as polyamide 6 and polyamide 66, which have the largest market share. Their raw materials, caprolactam and adipic acid, are hydrogenated by benzene homologues. It is prepared by a series of reactions such as oxidation, and hexamethylene diamine is prepared by first synthesizing adiponitrile from butadiene or acrylonitrile and then by catalytic hydrogenation. Currently, it is prepared by petrochemical methods.
热塑性聚合物后续纤维产品开发是一项重要的任务。熔融纺丝法是最常用的纺丝方法,分为熔体直接纺丝法和切片纺丝法。熔融纺丝不需要溶剂,可直接纺丝,工艺简单,成本较低,无溶剂回收问题。The subsequent fiber product development of thermoplastic polymers is an important task. Melt spinning is the most commonly used spinning method, which is divided into melt direct spinning and chip spinning. Melt spinning does not require solvent, it can be directly spun, the process is simple, the cost is low, and there is no solvent recovery problem.
发明内容SUMMARY OF THE INVENTION
本发明涉及的一种功能性聚酰胺56长丝属于新型生物基聚合物产品,其原料戊二胺主要是利用生物发酵方法制备,再通过与己二酸合成得到生物基聚酰胺56聚合物。The invention relates to a functional polyamide 56 filament, which belongs to a novel bio-based polymer product. The raw material, pentamethylene diamine, is mainly prepared by a biological fermentation method, and then synthesized with adipic acid to obtain a bio-based polyamide 56 polymer.
本发明提供的一种功能性聚酰胺56长丝的制备方法,包括如下工艺流程:The preparation method of a functional polyamide 56 filament provided by the invention comprises the following technological process:
1)功能性切片干燥:对功能性聚酰胺56切片进行分段真空干燥处理;1) Functional slice drying: segmented vacuum drying is performed on functional polyamide 56 slices;
2)熔融纺丝:干燥后的所述功能性聚酰胺56切片经螺杆挤压机、纺丝箱体的喷丝板喷出得到熔体细流,所述熔体细流经吹风冷却凝固成丝条;2) Melt spinning: the dried functional polyamide 56 slices are sprayed out through the screw extruder and the spinneret of the spinning box to obtain a melt stream, which is cooled and solidified by air blowing. thread;
3)冷牵伸:所述丝条经集束上油后,由冷却牵伸辊冷却牵伸,得到聚酰胺56丝束;3) cold drafting: after the strands are bundled and oiled, they are cooled and drafted by cooling drafting rollers to obtain polyamide 56 tow;
4)长丝后加工:所述聚酰胺56丝束经过热牵伸、热定型和卷绕,或变形加工工艺得到功能性聚酰胺56长丝。4) Filament post-processing: the polyamide 56 tow is subjected to thermal drawing, heat setting and winding, or a texturing process to obtain functional polyamide 56 filaments.
上述的制备工艺1)中,所述功能性聚酰胺56切片的指标如下:In above-mentioned preparation technique 1), the index of described functional polyamide 56 slices is as follows:
特别地,当制备的所述功能性聚酰胺56长丝为高强聚酰胺56长丝时,所述切片粘度指标为145~180ml/g;In particular, when the prepared functional polyamide 56 filament is a high-strength polyamide 56 filament, the slice viscosity index is 145-180 ml/g;
特别地,当制备的所述功能性聚酰胺56长丝为阻燃聚酰胺56长丝时,所述切片粘度指标为135~160ml/g;In particular, when the prepared functional polyamide 56 filament is a flame-retardant polyamide 56 filament, the slice viscosity index is 135-160 ml/g;
特别地,当制备的所述功能性聚酰胺56长丝为易染聚酰胺56长丝时,所述切片端氨基含量指标为40~70mmol/kg;In particular, when the prepared functional polyamide 56 filament is an easy-dyeing polyamide 56 filament, the amino group content index at the end of the slice is 40-70 mmol/kg;
特别地,当制备的所述功能性聚酰胺56长丝为防霉聚酰胺56长丝时,所述切片端氨基含量指标为30~55mmol/kg。In particular, when the prepared functional polyamide 56 filament is a mildew-proof polyamide 56 filament, the amino group content index at the end of the slice is 30-55 mmol/kg.
上述的制备工艺1)中,所述分段真空干燥处理的条件如下:In above-mentioned preparation technique 1), the condition of described subsection vacuum drying is as follows:
首先在40~60℃的条件下干燥10~12h,然后升温至80~95℃干燥7~10h,再升温至105~115℃的条件下干燥5~7h,继续在130~140℃的条件下保温3~6h。First dry at 40-60°C for 10-12h, then heat up to 80-95°C for 7-10h, then heat up to 105-115°C and dry for 5-7h, continue at 130-140°C Heat preservation for 3 to 6 hours.
经步骤1)中所述分段真空干燥处理后的所述功能性聚酰胺56切片的指标如下:The index of the described functional polyamide 56 slices after the segmental vacuum drying described in step 1) is as follows:
切片含水≤600ppm;熔点为245~260℃。The water content of the slices is ≤600ppm; the melting point is 245~260℃.
上述的制备工艺2)中,所述纺丝箱螺杆各区温度:螺杆各区温度:一区260~290℃,二区260~290℃,三区260~290℃,四区260~290℃,五区260~290℃,箱体温度260~290℃,计量泵温度260~290℃,计量泵转速12rpm~16rpm,纺丝速度为800m/min~4500m/min;In the above-mentioned preparation process 2), the temperature of each zone of the screw of the spinning box: the temperature of each zone of the screw: 260-290 ℃ in the first zone, 260-290 ℃ in the second zone, 260-290 ℃ in the third zone, 260-290 ℃ in the fourth zone, and 5. Zone 260~290℃, box temperature 260~290℃, metering pump temperature 260~290℃, metering pump speed 12rpm~16rpm, spinning speed 800m/min~4500m/min;
特别地,当制备的所述功能性聚酰胺56长丝为高强聚酰胺56长丝时,所述纺丝速度具体为3000m/min~4500m/min;In particular, when the prepared functional polyamide 56 filament is a high-strength polyamide 56 filament, the spinning speed is specifically 3000m/min~4500m/min;
上述的制备工艺2)中,采用环吹风或侧吹风的吹风冷却方式,条件如下:风速:30~60m/min;风温:18~26℃;风压:350Pa~600Pa;In the above-mentioned preparation process 2), the cooling mode of air blowing by ring blowing or side blowing is adopted, and the conditions are as follows: wind speed: 30~60m/min; wind temperature: 18~26 ℃; wind pressure: 350Pa~600Pa;
所述上油的油剂质量浓度3%~5%。The mass concentration of the oiling agent is 3% to 5%.
所述冷却牵伸辊的温度为0~20℃,牵伸倍数1.05~1.45。The temperature of the cooling drafting roll is 0-20°C, and the drafting ratio is 1.05-1.45.
上述的制备工艺3)中,所述热牵伸工艺可为一级牵伸、二级牵伸或多级牵伸,工艺条件:牵伸倍数为1.01~5.50,牵伸温度为80~200℃;In the above-mentioned preparation process 3), the hot drawing process can be one-stage drafting, two-stage drafting or multi-stage drafting, and the process conditions: the drafting ratio is 1.01~5.50, and the drafting temperature is 80~200 ℃ ;
特别地,制备高强聚酰胺56长丝,牵伸倍数为3.00~5.50。In particular, high-strength polyamide 56 filaments are prepared with a draw ratio of 3.00 to 5.50.
上述的制备工艺4)中,所述变形加工工艺包括制备功能化聚酰胺56拉伸变形丝的工艺和制备功能化聚酰胺56空气变形丝的工艺。In the above preparation process 4), the texturing process includes a process for preparing functionalized polyamide 56 drawn textured yarn and a process for preparing functionalized polyamide 56 air-textured yarn.
制备功能化聚酰胺56拉伸变形丝的工艺包括热牵伸、加捻、网络、热定型和卷绕的步骤,各条件如下:The process for preparing the functionalized polyamide 56 stretched textured yarn includes the steps of hot drawing, twisting, networking, heat setting and winding, and the conditions are as follows:
热牵伸温度为100~200℃,牵伸倍数为1.10~2.50,牵伸辊速度为300~1000m/min;加捻分为S捻或Z捻,加捻张力20~60cN,解捻张力为25~65cN,D/Y为摩擦盘的表面速度与丝条离开假捻器速度之比,具体为1.5~2.0;网络步骤中,风压为1.0~1.6bar;喷嘴直径为1.2~1.6mm,热定型温度为180~220℃,卷绕速度为600~1200m/min。The hot drafting temperature is 100~200℃, the drafting ratio is 1.10~2.50, the speed of the drafting roller is 300~1000m/min; the twisting is divided into S twist or Z twist, the twisting tension is 20~60cN, and the untwisting tension is 25~65cN, D/Y is the ratio of the surface speed of the friction disc and the speed of the thread leaving the false twister, specifically 1.5~2.0; in the network step, the wind pressure is 1.0~1.6bar; the diameter of the nozzle is 1.2~1.6mm, The heat setting temperature is 180~220℃, and the winding speed is 600~1200m/min.
制备功能化聚酰胺56空气变形丝的工艺包括热牵伸、热喷射变形、冷却稳定、卷绕的步骤。各条件如下:The process for preparing the functionalized polyamide 56 air-textured yarn includes the steps of thermal drawing, thermal jet texturing, cooling stabilization and winding. The conditions are as follows:
热牵伸温度为100~190℃,牵伸倍数为1.05~3.50,牵伸辊速度为1500~2500m/min;热喷射变形空气温度为190~230℃,空气喷射压力为195~550kPa,超喂率为15~30%,冷却空气温度为15~30℃,卷绕速度为1500~2800m/min。The hot drawing temperature is 100~190℃, the drawing ratio is 1.05~3.50, the speed of the drafting roller is 1500~2500m/min; The rate is 15-30%, the cooling air temperature is 15-30°C, and the winding speed is 1500-2800 m/min.
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。The experimental methods used in the following examples are conventional methods unless otherwise specified.
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。The materials, reagents, etc. used in the following examples can be obtained from commercial sources unless otherwise specified.
下述实施例中功能性聚酰胺56长丝样品,根据以下方法检测性能:The functional polyamide 56 filament samples in the following examples were tested for performance according to the following methods:
1.断裂强度、断裂伸长率:GB/T 14344-2008化学纤维长丝拉伸性能试验方法;1. Breaking strength and breaking elongation: GB/T 14344-2008 Test method for tensile properties of chemical fiber filaments;
2.回潮率:GB/T 6503-2017化学纤维回潮率试验方法;2. Moisture regain: GB/T 6503-2017 Chemical fiber moisture regain test method;
3.极限氧指数:GB/T 5454-1997纺织品燃烧性能试验氧指数法;3. Limiting oxygen index: GB/T 5454-1997 Textile combustion performance test oxygen index method;
4.防霉性能:GB/T 24346-2009纺织品防霉性能的评价;4. Anti-mildew properties: GB/T 24346-2009 Evaluation of anti-mildew properties of textiles;
5.网络测定:采用R2071型网络度仪,根据FZ/T 50001合成纤维长丝网络度试验方法;5. Network measurement: R2071 network degree meter is used, according to FZ/T 50001 synthetic fiber filament network degree test method;
6.上染率测试:用分光光度计在最大吸收波长处分别测定染色前后染液的吸光度,根据下式计算上染百分率:Ct=(1–A
1/A
0)×100%(式中:A
0为原染液吸光度;A
1为染色后残液的吸光度,选择10g/L酸性红2B染料试验。)
6. Dyeing rate test: use a spectrophotometer to measure the absorbance of the dye solution before and after dyeing at the maximum absorption wavelength, and calculate the dyeing percentage according to the following formula: Ct=(1-A 1 /A 0 )×100% (wherein : A 0 is the absorbance of the original dye solution; A 1 is the absorbance of the residual solution after dyeing, choose 10g/L acid red 2B dye test.)
实施例1、高强聚酰胺56长丝Example 1, high-strength polyamide 56 filament
功能性切片的粘度指数163ml/g,氨基含量36.4mmol/kg,切片真空干燥的过程如下:先在50℃的条件下干燥12h,后升温至85℃的条件下干燥8h,再升温至110℃的条件下干燥6h,继续在130℃的条件下保温5h。干燥后功能性切片含水427ppm,熔点256℃。The viscosity index of functional slices is 163ml/g, and the amino group content is 36.4mmol/kg. The vacuum drying process of slices is as follows: first dry at 50°C for 12h, then heat up to 85°C for 8h, and then heat up to 110°C It was dried for 6h under the condition of 130°C and kept at 130°C for 5h. After drying, the functional chips contained 427 ppm of water and a melting point of 256°C.
设定纺丝速度:4250m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区288℃,二区288℃,三区288℃,四区288℃,五区288℃,箱体温度288℃,计量泵温度288℃,计量泵转速14rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为40m/min,风温为21℃,风压430Pa,再对丝条上油,油剂浓度3%,再经过5℃冷牵伸1.23倍,得到聚酰胺56丝束。Set the spinning speed: 4250m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The fourth zone is 288°C, the fifth zone is 288°C, the temperature of the box is 288°C, the temperature of the metering pump is 288°C, and the speed of the metering pump is 14rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 21°C, and the wind pressure is 430Pa, and then the strands are oiled with a concentration of 3% oil, and then cold-drawn at 5°C for 1.23 times to obtain polyamide 56 strands bundle.
将聚酰胺56丝束进行二级牵伸,一牵倍数4.53,二牵倍数1.12、一牵温度110℃,二牵温度175℃,然后在185℃条件下进行热定型,3800m/min卷绕,得到高强聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 4.53, the second-drawing multiple is 1.12, the first-drawing temperature is 110 °C, the second-drawing temperature is 175 °C, and then heat-set at 185 °C, 3800m/min winding, High-strength polyamide 56 filaments were obtained.
高强聚酰胺长丝的断裂强度8.45cN/dtex,断裂伸长率断裂伸长率33.7%,回潮率4.36%,极限氧指数35.5%。The breaking strength of the high-strength polyamide filament is 8.45cN/dtex, the elongation at break is 33.7%, the moisture regain is 4.36%, and the limiting oxygen index is 35.5%.
实施例2、高强聚酰胺56长丝Example 2, high-strength polyamide 56 filament
功能性切片的粘度指数148ml/g,氨基含量36.4mmol/kg,真空干燥的 过程如下:先在60℃的条件下干燥10h,后升温至95℃的条件下干燥8h,再升温至115℃的条件下干燥5h,继续在140℃的条件下保温3h。干燥后切片切片含水302ppm,熔点254℃。The viscosity index of the functional chips is 148ml/g, and the amino group content is 36.4mmol/kg. The vacuum drying process is as follows: first dry at 60°C for 10h, then heat up to 95°C for 8h, and then heat up to 115°C. Condition drying for 5h, continue to keep at 140 ℃ for 3h. After drying, the slices have a water content of 302 ppm and a melting point of 254 °C.
设定纺丝速度:3650m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区290℃,二区290℃,三区290℃,四区290℃,五区290℃,箱体温度290℃,计量泵温度290℃,计量泵转速16rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为60m/min,风温为18℃,风压360Pa,再对所述丝条上油,油剂浓度3%,再经过15℃冷牵伸1.35倍,得到聚酰胺56丝束。Set the spinning speed: 3650m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zones are 290°C, the fifth zone is 290°C, the box temperature is 290°C, the metering pump temperature is 290°C, and the metering pump speed is 16rpm. It solidifies into strands, the cooling wind speed is 60m/min, the wind temperature is 18°C, and the wind pressure is 360Pa, and then the strands are oiled with an oil concentration of 3%, and then cold-drawn at 15°C for 1.35 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数4.13,二牵倍数1.25、一牵温度130℃,二牵温度180℃,然后在190℃条件下进行热定型,3500m/min卷绕,得到高强聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 4.13, the second-draw multiple is 1.25, the first-draw temperature is 130°C, and the second-draw temperature is 180°C, and then heat-set at 190°C and wound at 3500m/min, High-strength polyamide 56 filaments were obtained.
高强聚酰胺长丝的断裂强度7.83cN/dtex,断裂伸长率断裂伸长率37.7%,回潮率4.28%,极限氧指数34.7%。The breaking strength of the high-strength polyamide filament is 7.83cN/dtex, the elongation at break is 37.7%, the moisture regain is 4.28%, and the limiting oxygen index is 34.7%.
实施例3、阻燃聚酰胺56长丝Example 3, flame retardant polyamide 56 filament
功能性切片的粘度指数142ml/g,真空干燥的过程如下:先在60℃的条件下干燥12h,后升温至90℃的条件下干燥8h,再升温至105℃的条件下干燥5h,继续在135℃的条件下保温4h。干燥后切片的切片含水447ppm,熔点255℃。The viscosity index of functional slices is 142ml/g. The vacuum drying process is as follows: first dry at 60°C for 12h, then heat up to 90°C for 8h, then heat up to 105°C for 5h, and continue to dry at 105°C for 5 hours. Incubate at 135°C for 4h. After drying, the sliced slices have a water content of 447 ppm and a melting point of 255°C.
设定纺丝速度:3100m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区286℃,二区286℃,三区286℃,四区286℃,五区286℃,箱体温度286℃,计量泵温度286℃,计量泵转速14rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为45m/min,风温为23℃,风压450Pa,再对所述丝条上油,油剂浓度3%,再经过10℃冷牵伸1.18倍,得到聚酰胺56丝束。Set the spinning speed: 3100m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zone is 286°C, the fifth zone is 286°C, the temperature of the box is 286°C, the temperature of the metering pump is 286°C, and the speed of the metering pump is 14rpm. It solidifies into strands, the cooling wind speed is 45m/min, the wind temperature is 23°C, and the wind pressure is 450Pa, then the strands are oiled with an oil concentration of 3%, and then cold drawn at 10°C for 1.18 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数3.68,二牵倍数1.02、一牵温度80℃,二牵温度165℃,然后在175℃条件下进行热定型,2400m/min 卷绕,得到阻燃聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drafting, the first-drawing multiple is 3.68, the second-drawing multiple is 1.02, the first-drawing temperature is 80 °C, the second-drawing temperature is 165 °C, and then heat-set at 175 °C, 2400m/min winding, A flame retardant polyamide 56 filament was obtained.
阻燃聚酰胺长丝的断裂强度5.18cN/dtex,断裂伸长率断裂伸长率34.2%,回潮率4.48%,极限氧指数37.3%。The breaking strength of the flame-retardant polyamide filament is 5.18cN/dtex, the elongation at break is 34.2%, the moisture regain is 4.48%, and the limiting oxygen index is 37.3%.
实施例4、阻燃聚酰胺56长丝Example 4, flame retardant polyamide 56 filament
功能性切片的粘度指数137.7ml/g,真空干燥的过程如下:先在40℃的条件下干燥12h,后升温至80℃的条件下干燥8h,再升温至105℃的条件下干燥6h,继续在135℃的条件下保温5h。切片的切片含水579ppm,熔点253℃。The viscosity index of functional slices is 137.7ml/g. The vacuum drying process is as follows: first dry at 40°C for 12h, then heat up to 80°C for 8h, then heat up to 105°C for 6h, and continue Incubate at 135°C for 5h. The sliced slices have a water content of 579 ppm and a melting point of 253°C.
设定纺丝速度:2000m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区287℃,二区287℃,三区287℃,四区287℃,五区287℃,箱体温度287℃,计量泵温度287℃,计量泵转速13rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为40m/min,风温为21℃,风压480Pa,再对所述丝条上油,油剂浓度5%,再经过0℃冷牵伸1.30倍,得到聚酰胺56丝束。Set the spinning speed: 2000m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zone is 287°C, the fifth zone is 287°C, the temperature of the box is 287°C, the temperature of the metering pump is 287°C, and the speed of the metering pump is 13rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 21°C, and the wind pressure is 480Pa, then the strands are oiled with an oil concentration of 5%, and then cold-drawn at 0°C for 1.30 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数3.30,二牵倍数1.15、一牵温度100℃,二牵温度170℃,然后在180℃条件下进行热定型,1800m/min卷绕,得到阻燃聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 3.30, the second-drawing multiple is 1.15, the first-drawing temperature is 100 °C, the second-drawing temperature is 170 °C, and then heat-set at 180 °C, 1800m/min winding, A flame retardant polyamide 56 filament was obtained.
阻燃聚酰胺长丝的断裂强度4.99cN/dtex,断裂伸长率断裂伸长率40.4%,回潮率4.37%,极限氧指数36.4%。The breaking strength of the flame-retardant polyamide filament is 4.99cN/dtex, the elongation at break is 40.4%, the moisture regain is 4.37%, and the limiting oxygen index is 36.4%.
实施例5、易染聚酰胺56长丝Example 5. Easy-dyeing polyamide 56 filament
功能性切片的端氨基含量为68.8mmol/kg,真空干燥的过程如下:先在55℃的条件下干燥10h,后升温至90℃的条件下干燥10h,再升温至110℃的条件下干燥6h,继续在130℃的条件下保温5h。干燥后切片含水363ppm,熔点249℃。The content of terminal amino group of functional slices is 68.8mmol/kg. The vacuum drying process is as follows: first drying at 55℃ for 10h, then heating to 90℃ for 10h, and then heating to 110℃ for 6h , and continue to incubate at 130 °C for 5 h. After drying, the slices have a water content of 363 ppm and a melting point of 249°C.
设定纺丝速度:1550m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区283℃,二区283℃,三区283℃,四区283℃,五区283℃,箱体温度283℃,计量泵温度283℃,计量泵转速15rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹 风冷却凝固成为丝条,冷却风速为48m/min,风温为20℃,风压460Pa,再对所述丝条上油,油剂浓度3%,再经过10℃冷牵伸1.28倍,得到聚酰胺56丝束。Set the spinning speed: 1550m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The temperature of the four zone is 283°C, the zone five is 283°C, the temperature of the box is 283°C, the temperature of the metering pump is 283°C, and the speed of the metering pump is 15rpm. It solidifies into strands, the cooling wind speed is 48m/min, the wind temperature is 20°C, and the wind pressure is 460Pa, and then the strands are oiled with an oil concentration of 3%, and then cold-drawn at 10°C for 1.28 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数3.11,二牵倍数1.10、一牵温度100℃,二牵温度185℃,然后在200℃条件下进行热定型,1300m/min卷绕,得到易染聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-drawing ratio is 3.11, the second-drawing ratio is 1.10, the first-drawing temperature is 100 °C, the second-drawing temperature is 185 °C, and then heat-set at 200 °C, 1300m/min winding, Easy-dyeing polyamide 56 filaments were obtained.
易染聚酰胺长丝的断裂强度4.63cN/dtex,断裂伸长率断裂伸长率51.1%,回潮率4.51%,极限氧指数32.1%,上染率99.2%。The breaking strength of the easily dyed polyamide filament is 4.63cN/dtex, the elongation at break is 51.1%, the moisture regain is 4.51%, the limiting oxygen index is 32.1%, and the dyeing rate is 99.2%.
实施例6、易染聚酰胺56长丝Example 6, easy-dyeing polyamide 56 filament
功能性切片的端氨基含量为68.8mmol/kg,真空干燥的过程如下:先在55℃的条件下干燥12h,后升温至95℃的条件下干燥10h,再升温至115℃的条件下干燥6h,继续在140℃的条件下保温4h。干燥后切片含水398ppm,熔点253℃。The amino-terminal content of functional slices is 68.8 mmol/kg. The vacuum drying process is as follows: first drying at 55°C for 12h, then heating to 95°C for 10h, and then heating to 115°C for 6h , and kept at 140°C for 4h. After drying, the slices have a water content of 398 ppm and a melting point of 253°C.
设定纺丝速度:1200m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区270℃,二区270℃,三区270℃,四区270℃,五区270℃,箱体温度270℃,计量泵温度270℃,计量泵转速15rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为40m/min,风温为25℃,风压400Pa,再对所述丝条上油,油剂浓度3%,再经过5℃冷牵伸1.20倍,得到聚酰胺56丝束。Set the spinning speed: 1200m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zones are 270°C, the fifth zone is 270°C, the box temperature is 270°C, the metering pump temperature is 270°C, and the metering pump speed is 15rpm. Solidify into strands, the cooling wind speed is 40m/min, the wind temperature is 25°C, and the wind pressure is 400Pa, then the strands are oiled with an oil concentration of 3%, and then cold drawn at 5°C for 1.20 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数3.00,二牵倍数1.10、一牵温度100℃,二牵温度160℃,然后在180℃条件下进行热定型,1000m/min卷绕,得到易染聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-drawing multiple is 3.00, the second-drawing multiple is 1.10, the first-drawing temperature is 100 °C, the second-drawing temperature is 160 °C, and then heat-setting at 180 °C, 1000m/min winding, Easy-dyeing polyamide 56 filaments were obtained.
易染聚酰胺长丝的断裂强度4.60cN/dtex,断裂伸长率断裂伸长率51.4%,回潮率4.44%,极限氧指数32.2%,上染率99.5%。The breaking strength of the easily dyeable polyamide filament is 4.60cN/dtex, the elongation at break is 51.4%, the moisture regain is 4.44%, the limiting oxygen index is 32.2%, and the dyeing rate is 99.5%.
实施例7、防霉聚酰胺56长丝Example 7, mildew-proof polyamide 56 filament
功能性切片的氨基含量32.4mmol/kg,真空干燥的过程如下:先在55℃的条件下干燥10h,后升温至90℃的条件下干燥10h,再升温至110℃的条件下干燥6h,继续在130℃的条件下保温5h。干燥后切片含水412ppm,熔 点251℃。The amino content of functional slices is 32.4mmol/kg. The vacuum drying process is as follows: first dry at 55°C for 10h, then heat up to 90°C for 10h, then heat up to 110°C for 6h, and continue Incubate at 130°C for 5h. After drying, the slices had a water content of 412 ppm and a melting point of 251°C.
设定纺丝速度:1000m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区283℃,二区283℃,三区283℃,四区283℃,五区283℃,箱体温度283℃,计量泵温度283℃,计量泵转速15rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为45m/min,风温为20℃,风压440Pa,再对所述丝条上油,油剂浓度3%,再经过10℃冷牵伸1.25倍,得到聚酰胺56丝束。Set the spinning speed: 1000m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The temperature of the four zone is 283°C, the zone five is 283°C, the temperature of the box is 283°C, the temperature of the metering pump is 283°C, and the speed of the metering pump is 15rpm. Solidify into strands, the cooling wind speed is 45m/min, the wind temperature is 20°C, and the wind pressure is 440Pa, and then the strands are oiled with an oil concentration of 3%, and then cold-drawn at 10°C for 1.25 times to obtain a polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数2.30,二牵倍数1.15、一牵温度80℃,二牵温度155℃,然后在165℃条件下进行热定型,900m/min卷绕,得到防霉聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 2.30, the second-draw multiple is 1.15, the first-draw temperature is 80 °C, and the second-draw temperature is 155 °C, and then heat-set at 165 °C, 900m/min winding, Mildew-resistant polyamide 56 filaments were obtained.
对该长丝防霉性能进行评价,其中混合孢子液浓度:1.2×106CFU/mL,检测用霉菌为黑曲霉(Aspergillus niger)AS 3.4463、绳状青霉(Penicillium funiculosum)AS 3.3875、球毛壳(chaetoomium globsum)AS 3.4254、绿色木霉(Trichoderma viride)AS 3.2942。The anti-fungal properties of the filament were evaluated, wherein the concentration of mixed spore solution: 1.2 × 106 CFU/mL, and the molds used for detection were Aspergillus niger AS 3.4463, Penicillium funiculosum AS 3.3875, globosa ( chaetoomium globsum) AS 3.4254, Trichoderma viride AS 3.2942.
防霉聚酰胺长丝的断裂强度4.34cN/dtex,断裂伸长率断裂伸长率58.2%,回潮率4.53%,极限氧指数32.3%,防霉性能0级。The breaking strength of the mildew-resistant polyamide filament is 4.34 cN/dtex, the elongation at break is 58.2%, the moisture regain is 4.53%, the limiting oxygen index is 32.3%, and the mildew resistance is grade 0.
实施例8、防霉聚酰胺56长丝Example 8, mildew-proof polyamide 56 filament
功能性切片的氨基含量42.4mmol/kg,真空干燥的过程如下:先在50℃的条件下干燥10h,后升温至90℃的条件下干燥8h,再升温至110℃的条件下干燥5h,继续在130℃的条件下保温3h。干燥后切片含水362ppm,熔点251℃。The amino content of functional slices is 42.4 mmol/kg. The vacuum drying process is as follows: first dry at 50 °C for 10 hours, then heat up to 90 °C for 8 hours, then heat up to 110 °C for 5 hours, and continue Incubate at 130°C for 3h. After drying, the slices have a water content of 362 ppm and a melting point of 251°C.
设定纺丝速度:1000m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区280℃,二区280℃,三区280℃,四区280℃,五区280℃,箱体温度280℃,计量泵温度280℃,计量泵转速15rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为40m/min,风温为23℃,风压420Pa,再对所述丝条上油,油剂浓度4%,再经过0℃冷牵伸1.08倍,得到聚酰胺56丝束。Set the spinning speed: 1000m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zones are 280°C, the fifth zone is 280°C, the box temperature is 280°C, the metering pump temperature is 280°C, and the metering pump speed is 15rpm. It solidifies into strands, the cooling wind speed is 40m/min, the wind temperature is 23°C, and the wind pressure is 420Pa, then the strands are oiled with an oil concentration of 4%, and then cold drawn at 0°C for 1.08 times to obtain polyamide 56 tows.
将聚酰胺56丝束进行二级牵伸,一牵倍数3.03,二牵倍数1.10、一牵温度110℃,二牵温度180℃,然后在200℃条件下进行热定型,900m/min卷绕,得到防霉聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drafting, the first-drawing multiple is 3.03, the second-drawing multiple is 1.10, the first-drawing temperature is 110 °C, the second-drawing temperature is 180 °C, and then heat-set at 200 °C, 900m/min winding, Mildew-resistant polyamide 56 filaments were obtained.
对该长丝防霉性能进行评价,其中混合孢子液浓度:1.2*106CFU/mL,检测用霉菌为黑曲霉(Aspergillus niger)AS 3.4463、绳状青霉(Penicillium funiculosum)AS 3.3875、球毛壳(chaetoomium globsum)AS 3.4254、绿色木霉(Trichoderma viride)AS 3.2942。The anti-mildew performance of the filament was evaluated, wherein the concentration of mixed spore solution: 1.2*106 CFU/mL, and the molds used for the detection were Aspergillus niger AS 3.4463, Penicillium funiculosum AS 3.3875, globosa ( chaetoomium globsum) AS 3.4254, Trichoderma viride AS 3.2942.
防霉聚酰胺长丝的断裂强度4.41cN/dtex,断裂伸长率断裂伸长率50.7%,回潮率4.33%,极限氧指数33.8%,防霉性能0级。The breaking strength of the mildew-resistant polyamide filament is 4.41 cN/dtex, the elongation at break is 50.7%, the moisture regain is 4.33%, the limiting oxygen index is 33.8%, and the mildew resistance is grade 0.
实施例9、阻燃型聚酰胺56拉伸变形丝Example 9, flame retardant polyamide 56 stretched textured yarn
功能性切片的粘度指数144.1ml/g,真空干燥的过程同实施例3,干燥后切片含水584ppm,熔点251℃。The viscosity index of the functional slices was 144.1 ml/g, and the vacuum drying process was the same as that in Example 3. After drying, the slices had a water content of 584 ppm and a melting point of 251°C.
纺丝、冷牵伸、热牵伸过程参数设定与实施例3相同,得到牵伸后聚酰胺56丝束。The parameter settings of spinning, cold drawing, and hot drawing are the same as those in Example 3, and the drawn polyamide 56 tow is obtained.
将得到的聚酰胺56丝束在180℃条件下,牵伸2.00倍,牵伸辊速度为800m/min,牵伸后长丝加S捻,加捻张力45cN,解捻张力48cN;所述D/Y为1.8,网络风压为1.2bar;喷嘴直径1.3mm,热定型温度为190℃,所述卷绕速度为900m/min。The obtained polyamide 56 tow was drawn 2.00 times under the condition of 180 ° C, the speed of the drawing roller was 800 m/min, and the filament was S-twisted after drawing, the twisting tension was 45cN, and the untwisting tension was 48cN; the D /Y is 1.8, network air pressure is 1.2 bar; nozzle diameter is 1.3 mm, heat setting temperature is 190° C., and the winding speed is 900 m/min.
阻燃聚酰胺拉伸变形丝的断裂强度5.38cN/dtex,断裂伸长率断裂伸长率34.2%,回潮率4.26%,极限氧指数37.8%,网络度(结点数)101。The breaking strength of the flame retardant polyamide stretched textured yarn is 5.38cN/dtex, the elongation at break is 34.2%, the moisture regain is 4.26%, the limiting oxygen index is 37.8%, and the degree of network (the number of nodes) is 101.
实施例10、易染型聚酰胺56空气变形丝Example 10. Easy-dyeing polyamide 56 air textured yarn
功能性切片的端氨基值63.1mmol/kg,真空干燥的过程同实施例5,干燥后切片含水412ppm,熔点251℃。The terminal amino group value of the functional slice is 63.1 mmol/kg, and the vacuum drying process is the same as that in Example 5. After drying, the slice contains 412 ppm of water and has a melting point of 251°C.
纺丝、冷牵伸、热牵伸过程参数设定与实施例5相同,得到牵伸后聚酰胺56丝束。牵伸后丝束在160℃下热牵伸1.10倍,热喷射变形温度230℃、空气喷射压力300kPa,超喂率25%,冷却空气温度15℃,以1400m/min的卷绕速度卷绕,得到易染型聚酰胺56空气变形丝。The process parameters of spinning, cold drawing and hot drawing are the same as those in Example 5, and the drawn polyamide 56 tow is obtained. After drawing, the tow was thermally drawn at 160°C by 1.10 times, the thermal jet deformation temperature was 230°C, the air jet pressure was 300kPa, the overfeed rate was 25%, the cooling air temperature was 15°C, and the winding speed was 1400m/min. An easily dyeable polyamide 56 air textured yarn was obtained.
易染性聚酰胺空变丝的断裂强度5.13cN/dtex,断裂伸长率断裂伸长率46.1%,回潮率4.32%,极限氧指数33.4%,上染率99.4%。The breaking strength of the easily dyeable polyamide air-textured yarn is 5.13cN/dtex, the elongation at break is 46.1%, the moisture regain is 4.32%, the limiting oxygen index is 33.4%, and the dyeing rate is 99.4%.
对比例、聚酰胺56长丝制备Comparative example, polyamide 56 filament preparation
切片真空干燥的过程如下:先在120℃的条件下干燥24h。切片略有泛黄,粘度指数118.6ml/g,氨基含量19.1mmol/kg,切片含水372ppm,熔点251℃。The vacuum drying process of the slices is as follows: firstly, dry at 120°C for 24h. The slices were slightly yellowed, the viscosity index was 118.6 ml/g, the amino group content was 19.1 mmol/kg, the water content of the slices was 372 ppm, and the melting point was 251°C.
设定纺丝速度:500m/min,将干燥后聚酰胺56切片,经螺杆挤压机进入纺丝箱,纺丝箱螺杆各区温度:一区285℃,二区285℃,三区285℃,四区285℃,五区285℃,箱体温度285℃,计量泵温度285℃,计量泵转速15rpm,切片熔体经喷丝板喷出得到熔体细流,熔体细流经侧吹风冷却凝固成为丝条,冷却风速为45m/min,风温为20℃,风压440Pa,再对所述丝条上油,油剂浓度3%,卷绕得到聚酰胺56丝束。Set the spinning speed: 500m/min, cut the dried polyamide 56 into slices, and enter the spinning box through the screw extruder. The four zones are 285°C, the fifth zone is 285°C, the box temperature is 285°C, the metering pump temperature is 285°C, and the metering pump speed is 15rpm. It solidifies into strands, the cooling wind speed is 45m/min, the wind temperature is 20°C, and the wind pressure is 440Pa, then the strands are oiled with an oil concentration of 3%, and the polyamide 56 tow is obtained by winding.
将聚酰胺56丝束进行二级牵伸,一牵倍数2.0,二牵倍数1.10、一牵温度80℃,二牵温度150℃,然后在165℃条件下进行热定型,600m/min卷绕,得到聚酰胺56长丝。The polyamide 56 tow is subjected to two-stage drawing, the first-draw multiple is 2.0, the second-draw multiple is 1.10, the first-draw temperature is 80°C, and the second-draw temperature is 150°C, and then heat-set at 165°C, 600m/min winding, Polyamide 56 filaments were obtained.
对比例长丝性能:断裂强度2.87cN/dtex,断裂伸长率断裂伸长率86.8%,回潮率4.21%,极限氧指数22.3%。The properties of the comparative example filaments: breaking strength 2.87cN/dtex, breaking elongation breaking elongation 86.8%, moisture regain 4.21%, limiting oxygen index 22.3%.
实施例1-10和对比例制备的PA56长丝的性能数据可以看出,不同工艺参数条件下,长丝的性能差异较大,由实施例1-4可知,高粘度切片在高速纺条件下,长丝断裂强度高;当粘度指数和端氨基值在一定范围内,长丝极限氧指数高,阻燃性能好;当切片端氨基值较高时,长丝的低温染色性能明显好于其他条件下制备的长丝;当切片氨基值在一定范围内,长丝具有防霉性能。对比例采用高温真空干燥工艺,选择粘度指数、端氨基值均偏低的切片,在低速纺丝条件下,低倍牵伸制备聚酰胺56长丝及变形丝,结果表明产品的断裂强度、极限氧指数、上染率均不如实施例长丝产品。It can be seen from the performance data of the PA56 filaments prepared in Examples 1-10 and Comparative Examples that under different process parameters, the performance of the filaments is quite different. , the filament has high breaking strength; when the viscosity index and the terminal amino value are within a certain range, the limiting oxygen index of the filament is high, and the flame retardant performance is good; when the amino value of the slice end is high, the low-temperature dyeing performance of the filament is significantly better than other Filament prepared under conditions; when the amino value of slices is within a certain range, the filament has anti-mildew properties. In the comparative example, the high-temperature vacuum drying process was used, and the chips with low viscosity index and terminal amino value were selected. Under the condition of low-speed spinning, polyamide 56 filament and textured yarn were prepared by low-drawing. The results showed that the breaking strength and limit of the product were Oxygen index and dye uptake are not as good as the filament products of the examples.
工业应用Industrial application
本发明具有如下有益技术效果:The present invention has the following beneficial technical effects:
(1)采用分段真空干燥工艺除去聚酰胺56切片中的水分,减少切片受热降解,粘度下降,色泽加深等缺陷,同时提高切片的结晶性,有助于均匀稳定纺丝;(2)纺丝工艺中增加冷却牵伸工艺,这是由于研究中发现 聚酰胺56的冷却结晶速率慢,而未完全冷却的丝束不仅对卷绕上油工艺有影响,而且直接牵伸、定型使产品的力学性能不稳定,因此,加入冷却牵伸工艺使喷丝板形成的丝束迅速冷却,有利于后续高倍牵伸得到性能稳定、优异的聚酰胺长丝。(3)根据不同的粘度、端氨基、牵伸倍数等指标,可以制备出力学性能、阻燃性能、染色性能、防霉性能优异的聚酰胺56长丝及变形丝,满足特殊环境下的使用要求,广泛应用于各行各业。(1) The moisture in the polyamide 56 slices is removed by a segmented vacuum drying process, which reduces the defects such as thermal degradation of the slices, decreased viscosity, and deepened color, and at the same time improves the crystallinity of the slices, which is helpful for uniform and stable spinning; (2) Spinning The cooling and drawing process is added to the silk process. This is because the cooling crystallization rate of polyamide 56 is found to be slow in the research, and the incompletely cooled tow not only affects the winding and oiling process, but also directly draws and shapes the product. The mechanical properties are unstable. Therefore, adding a cooling drafting process to rapidly cool the tow formed by the spinneret is beneficial to the subsequent high-stretching to obtain polyamide filaments with stable performance and excellent performance. (3) Polyamide 56 filaments and textured yarns with excellent mechanical properties, flame retardant properties, dyeing properties, and mildew resistance can be prepared according to different viscosity, terminal amino group, draft ratio and other indicators to meet the use in special environments. requirements, widely used in all walks of life.
Claims (12)
- 一种功能性聚酰胺56长丝的制备方法,其特征在于:包括如下步骤:A preparation method of functional polyamide 56 filament, characterized in that: comprising the steps:1)功能性切片干燥:对功能性聚酰胺56切片进行分段真空干燥处理;1) Functional slice drying: segmented vacuum drying is performed on functional polyamide 56 slices;2)熔融纺丝:干燥后的所述功能性聚酰胺56切片经螺杆挤压机、纺丝箱体的喷丝板喷出得到熔体细流,所述熔体细流经吹风冷却凝固成丝条;2) Melt spinning: the dried functional polyamide 56 slices are sprayed out through the screw extruder and the spinneret of the spinning box to obtain a melt stream, which is cooled and solidified by air blowing. thread;3)冷牵伸:所述丝条经集束上油后,由冷却牵伸辊冷却牵伸,得到聚酰胺56丝束;3) cold drafting: after the strands are bundled and oiled, they are cooled and drafted by cooling drafting rollers to obtain polyamide 56 tow;4)长丝后加工:所述聚酰胺56丝束经过热牵伸、热定型和卷绕,或变形加工工艺得到功能性聚酰胺56长丝。4) Filament post-processing: the polyamide 56 tow is subjected to thermal drawing, heat setting and winding, or a texturing process to obtain functional polyamide 56 filaments.
- 根据权利要求1所述的制备方法,其特征在于:步骤1)中,所述功能性聚酰胺56切片的指标如下:preparation method according to claim 1, is characterized in that: in step 1), the index of described functional polyamide 56 slices is as follows:a)当制备的所述功能性聚酰胺56长丝为高强聚酰胺56长丝时,切片指标:粘度为145~180ml/g;a) When the prepared functional polyamide 56 filament is a high-strength polyamide 56 filament, the slice index: the viscosity is 145-180ml/g;b)当制备的所述功能性聚酰胺56长丝为阻燃聚酰胺56长丝时,切片指标:粘度为135~160ml/g;b) When the prepared functional polyamide 56 filament is a flame retardant polyamide 56 filament, the slice index: the viscosity is 135-160ml/g;c)当制备的所述功能性聚酰胺56长丝为易染聚酰胺56长丝时,切片指标:端氨基含量为40~70mmol/kg;c) When the prepared functional polyamide 56 filament is easily dyed polyamide 56 filament, the slice index: the content of terminal amino groups is 40-70 mmol/kg;d)当制备的所述功能性聚酰胺56长丝为防霉聚酰胺56长丝时,切片指标:端氨基含量为30~50mmol/kg。d) When the prepared functional polyamide 56 filament is a mildew-proof polyamide 56 filament, the slice index: the content of terminal amino groups is 30-50 mmol/kg.
- 根据权利要求1或2所述的制备方法,其特征在于:步骤1)中,所述分段真空干燥处理的条件如下:preparation method according to claim 1 and 2, is characterized in that: in step 1), the condition of described segmental vacuum drying treatment is as follows:首先在40~60℃的条件下干燥10~12h,然后升温至80~95℃干燥7~10h,再升温至105~115℃的条件下干燥5~7h,继续在130~140℃的条件下保温3~6h。First dry at 40-60°C for 10-12h, then heat up to 80-95°C for 7-10h, then heat up to 105-115°C and dry for 5-7h, continue at 130-140°C Heat preservation for 3 to 6 hours.
- 根据权利要求1-3中任一项所述的制备方法,其特征在于:经步骤1)中所述分段真空干燥处理后的所述功能性聚酰胺56切片的指标如下:The preparation method according to any one of claims 1-3, wherein the index of the functional polyamide 56 slices after the segmental vacuum drying treatment described in step 1) is as follows:切片含水≤600ppm;熔点为245~260℃。The water content of the slices is ≤600ppm; the melting point is 245~260℃.
- 根据权利要求1-4中任一项所述的制备方法,其特征在于:步骤2)中,所述熔融纺丝的条件如下:The preparation method according to any one of claims 1-4, characterized in that: in step 2), the conditions of the melt spinning are as follows:螺杆各区温度:一区温度为260~290℃,二区温度为260~290℃,三区温度为260~290℃,四区温度为260~290℃,五区温度为260~290℃,箱体的温度为260~290℃,计量泵的温度为260~290℃,计量泵的转速为12rpm~16rpm,纺丝速度为800m/min~4500m/min。The temperature of each zone of the screw: the temperature of the first zone is 260~290℃, the temperature of the second zone is 260~290℃, the temperature of the third zone is 260~290℃, the temperature of the fourth zone is 260~290℃, and the temperature of the fifth zone is 260~290℃. The temperature of the body is 260~290℃, the temperature of the metering pump is 260~290℃, the rotating speed of the metering pump is 12rpm~16rpm, and the spinning speed is 800m/min~4500m/min.
- 根据权利要求5所述的制备方法,其特征在于:当制备的所述功能性聚酰胺56长丝为高强聚酰胺56长丝时,纺丝速度为3000m/min~4500m/min;The preparation method according to claim 5, wherein: when the prepared functional polyamide 56 filament is a high-strength polyamide 56 filament, the spinning speed is 3000m/min~4500m/min;采用环吹风或侧吹风的吹风冷却方式,条件如下:The air cooling method of ring air blowing or side air blowing is adopted, and the conditions are as follows:风速为30~60m/min;风温为18~26℃;风压为350Pa~600Pa。The wind speed is 30~60m/min; the wind temperature is 18~26℃; the wind pressure is 350Pa~600Pa.
- 根据权利要求1-4中任一项所述的制备方法,其特征在于:步骤3)中,所述上油采用的油剂质量浓度为3%~5%。The preparation method according to any one of claims 1-4, characterized in that: in step 3), the mass concentration of the oil used in the oiling is 3% to 5%.所述冷却牵伸辊的温度为0~20℃,牵伸倍数为1.05~1.45;The temperature of the cooling drafting roll is 0-20°C, and the drafting ratio is 1.05-1.45;特别地,制备高强聚酰胺56长丝,牵伸倍数为3.00~5.50。In particular, high-strength polyamide 56 filaments are prepared with a draw ratio of 3.00 to 5.50.
- 根据权利要求1-4中任一项所述的制备方法,其特征在于:步骤4)中,所述热牵伸为一级牵伸、二级牵伸或多级牵伸,工艺条件:牵伸温度为80~200℃,牵伸倍数为1.01~5.50,特别地,制备高强聚酰胺56长丝,牵伸倍数为3.00~5.50。The preparation method according to any one of claims 1-4, characterized in that: in step 4), the thermal drafting is one-level drafting, two-level drafting or multi-level drafting, and process conditions: drawing The stretching temperature is 80-200° C., and the drafting ratio is 1.01-5.50. In particular, the high-strength polyamide 56 filament is prepared, and the drafting ratio is 3.00-5.50.
- 根据权利要求1-4中任一项所述的制备方法,其特征在于:步骤4)中,所述变形加工工艺包括制备功能化聚酰胺56拉伸变形丝的工艺和制备功能化聚酰胺56空气变形丝的工艺。The preparation method according to any one of claims 1-4, characterized in that: in step 4), the texturing process comprises a process for preparing functionalized polyamide 56 stretched textured yarn and preparing functionalized polyamide 56 Process of air textured yarn.
- 根据权利要求9所述的制备方法,其特征在于:制备功能化聚酰胺56拉伸变形丝的工艺包括热牵伸、加捻、网络、热定型和卷绕的步骤,各条件如下:The preparation method according to claim 9, wherein the process for preparing the functionalized polyamide 56 stretched textured yarn comprises the steps of thermal drawing, twisting, networking, heat setting and winding, and each condition is as follows:热牵伸温度为100~200℃,牵伸倍数为1.10~2.50,牵伸辊速度为300~1000m/min;加捻分为S捻或Z捻,加捻张力20~60cN,解捻张力为25~65cN,D/Y为摩擦盘的表面速度与丝条离开假捻器速度之比,具体为1.5~2.0;网络步骤中,风压为1.0~1.6bar;喷嘴直径为1.2~1.6mm,热定型温度为180~220℃,卷绕速度为600~1200m/min。The hot drafting temperature is 100~200℃, the drafting ratio is 1.10~2.50, the speed of the drafting roller is 300~1000m/min; the twisting is divided into S twist or Z twist, the twisting tension is 20~60cN, and the untwisting tension is 25~65cN, D/Y is the ratio of the surface speed of the friction disc and the speed of the thread leaving the false twister, specifically 1.5~2.0; in the network step, the wind pressure is 1.0~1.6bar; the diameter of the nozzle is 1.2~1.6mm, The heat setting temperature is 180~220℃, and the winding speed is 600~1200m/min.
- 根据权利要求9所述的制备方法,其特征在于:制备功能化聚酰胺56空气变形丝的工艺包括热牵伸、热喷射变形、冷却稳定、卷绕的步骤。各条件如下:The preparation method according to claim 9, wherein the process for preparing the functionalized polyamide 56 air-textured yarn comprises the steps of thermal drawing, thermal jet deformation, cooling stabilization and winding. The conditions are as follows:热牵伸温度为100~190℃,牵伸倍数为1.05~3.50,牵伸辊速度为1500~2500m/min;热喷射变形空气温度为190~230℃,空气喷射压力为195~550kPa,超喂率为15~30%,冷却空气温度为15~30℃,卷绕速度为1500~2800m/min。The hot drawing temperature is 100~190℃, the drawing ratio is 1.05~3.50, the speed of the drafting roller is 1500~2500m/min; The rate is 15-30%, the cooling air temperature is 15-30°C, and the winding speed is 1500-2800 m/min.
- 权利要求1-11中任一项所述方法制备的功能性聚酰胺56长丝;其特征在于:所述功能性聚酰胺56长丝的单丝线密度为1~7dtex,断裂强度3.5~12.0cN/dtex,性能为下述1)-4)中任一种:The functional polyamide 56 filament prepared by the method according to any one of claims 1-11; characterized in that: the monofilament linear density of the functional polyamide 56 filament is 1-7 dtex, and the breaking strength is 3.5-12.0 cN /dtex, the performance is any of the following 1)-4):1)当所述功能性聚酰胺56长丝为高强聚酰胺56长丝时,断裂强度为6.0~12.0cN/dtex;1) When the functional polyamide 56 filament is a high-strength polyamide 56 filament, the breaking strength is 6.0-12.0 cN/dtex;2)当所述功能性聚酰胺56长丝为阻燃型聚酰胺56长丝时,极限氧指数为33~38%;2) When the functional polyamide 56 filament is a flame-retardant polyamide 56 filament, the limiting oxygen index is 33-38%;3)当所述功能性聚酰胺56长丝为易染聚酰胺56长丝时,长丝的上染率达96.0%以上;3) When the functional polyamide 56 filament is an easy-dyeing polyamide 56 filament, the dyeing rate of the filament is over 96.0%;4)当所述功能性聚酰胺56长丝为防霉聚酰胺56长丝时,长丝的防霉等级≤1级。4) When the functional polyamide 56 filament is a mildew-proof polyamide 56 filament, the mildew-proof grade of the filament is ≤ grade 1.
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