WO2022116462A1 - 一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备 - Google Patents

一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备 Download PDF

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WO2022116462A1
WO2022116462A1 PCT/CN2021/086574 CN2021086574W WO2022116462A1 WO 2022116462 A1 WO2022116462 A1 WO 2022116462A1 CN 2021086574 W CN2021086574 W CN 2021086574W WO 2022116462 A1 WO2022116462 A1 WO 2022116462A1
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polyamide
temperature
drafting
salt solution
spinning
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PCT/CN2021/086574
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English (en)
French (fr)
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郝新敏
郭亚飞
闫金龙
乔荣荣
董梦杰
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军事科学院系统工程研究院军需工程技术研究所
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Publication of WO2022116462A1 publication Critical patent/WO2022116462A1/zh

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    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/28—Preparatory processes
    • 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
    • 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
    • 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
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
    • D02G1/0206—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/16—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics using jets or streams of turbulent gases, e.g. air, steam
    • D02G1/165—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics using jets or streams of turbulent gases, e.g. air, steam characterised by the use of certain filaments or yarns
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/08—Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D02J1/224—Selection or control of the temperature during stretching
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D02J1/225—Mechanical characteristics of stretching apparatus
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • 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 belongs to the field of textiles, and relates to a preparation process and equipment for one-step continuous forming and flexible deformation of polyamide 56 filaments.
  • Polyamide (PA) is an important fiber, commonly known as "nylon". It is the world's first commercialized synthetic fiber product. It brings real advantages in end-use fields: in clothing fabrics, it has Better moisture absorption, flex and drapability, softer hand feel; enormous durability and compression resistance in industrial applications; higher abrasion resistance and lamination recovery than any other fiber in carpet . In addition, the final product of polyamide fiber has low initial modulus, good elastic recovery, excellent abrasion resistance, and high breaking strength, which can make high-performance materials.
  • Polyamide fibers are usually produced by a melt spinning process.
  • Melt spinning generally has two methods, slice melt spinning and melt direct spinning.
  • the chip spinning process the high polymer needs to be made into chips first, and the chips are extracted, dried, and then melt spun.
  • the chip spinning method has good product quality and flexible production, but the production cost is high.
  • the melt direct spinning process is to send the polymer melt directly to the spinning machine for spinning.
  • the melt is pressurized by a specific equipment, extruded from the spinneret to form a thin stream of melt, and cooled and solidified to form primary fibers , and then the fiber is wound on a specific receiving mechanism.
  • the nascent fiber In order to meet the requirements of the finished fiber, the nascent fiber also needs to undergo a series of subsequent processing steps, such as stretching, shaping, deformation, etc.
  • This process saves tape injection, granulation and other processes, the process flow is short, energy saving and high efficiency, but the The method requires high stability of polymerization and spinning.
  • the purpose of the present invention is to provide a one-step continuous forming and flexible deformation preparation process and equipment of polyamide 56 filament.
  • the invention provides a one-step continuous forming and flexible deformation preparation process of polyamide 56 filament, which is mainly divided into three parts: polyamide salt solution polymerization process, spinning forming process, and flexible post-processing technology.
  • the method of the invention can be used for one-step continuous preparation.
  • the method for preparing polyamide 56 filament by one-step continuous molding and flexible deformation includes a polyamide salt solution polymerization process, a spinning molding process, and a flexible post-processing process;
  • pentamethylene diamine and adipic acid are neutralized in water to form a salt to obtain a polyamide 56 salt solution.
  • the polyamide 56 salt solution is added with auxiliary agents to prepare and mix, and then concentrated.
  • the concentrated salt solution undergoes prepolymerization, Pre-polymerization and post-polymerization to obtain polyamide 56 polymer melt;
  • the nitrogen protection is three flushes and three rows; the three flushes are three flushes of nitrogen; the three rows are exhaust air;
  • the molar ratio of the pentamethylene diamine to the adipic acid is 1-1.05:1; specifically, 1:1.01, 1:1.02, 1:1.03, 1:1.04;
  • the neutralization and salt-forming reaction temperature is 30-50°C; specifically 30°C, 35°C, 40°C, 45°C; the reaction time is 30-60min; specifically 35, 40, 45, 50, 55min;
  • the mass percentage of the polyamide 56 salt solution is 20% to 80%; specifically 25, 30, 35, 40, 45, 50, 55 or 75%;
  • the auxiliary agent can be one or more of molecular weight regulator, matting agent, flame retardant, antistatic agent, antibacterial agent, etc.; the addition amount of the auxiliary agent is the pentamethylenediamine 0.1% ⁇ 6% of the sum of the mass of adipic acid; specifically 0.1-1 or 0.1-0.5%;
  • the viscosity index of the prepared polyamide 56 polymer melt is 120-160 ml/g.
  • prepolymerization reaction conditions temperature 210 ⁇ 240 °C (specifically 212 °C, 217 °C, 218 °C, 228 °C, 229 °C, 238 °C), pressure 1.70 ⁇ 1.85MPa (specifically 1.73, 1.75, 1.78 , 1.8, 1.82MPa), the pressure holding time is 30min ⁇ 180min (specifically 90, 100, 120, 150, 160min); after the reaction is completed, the pressure is flashed and decompressed rapidly, and the temperature is raised to 270 ⁇ 290°C (specifically 278°C, 285°C) , 286°C); prepolymerization reaction conditions: temperature 270°C ⁇ 290°C (specifically 278°C, 285°C, 286°C), reaction time 20min ⁇ 150min (specifically 50, 60, 80, 90 or 100min); post-polymerization Reaction conditions: temperature 270 °C ⁇ 290 °C (specifically 278 °C),
  • step 1) After the polyamide 56 polymer melt prepared in step 1) is extruded by a screw, it is sprayed through a spinneret to obtain a thin stream of melt, which is solidified by cooling and blowing to become a thread, and the thread is coiled and oiled. , cold and hot drawing, heat setting to obtain polyamide 56 tow;
  • the temperature in each zone of the screw used is as follows: the temperature in the first zone is 260 to 300°C (specifically 260°C, 265°C, 270°C, 275°C, 278°C, 288°C or 298°C), and the temperature in the second zone is 260°C to 300°C.
  • the temperature in the three zones is 250-295°C (specifically 255°C, 260°C, 265°C, 270°C, 275°C, 278°C, 288°C or 298°C)
  • the temperature of the four zones is 250-295°C (specifically 255°C, 260°C, 265°C, 270°C, 275°C, 278°C, 288°C or 298°C)
  • the temperature of the five zones is 250 to 290°C (specifically 255°C, 260°C, 265°C, 270°C, 275°C, 278°C, 288°C or 298°C)
  • the temperature of the six zones is 250 to 290°C (specifically 255°C °C, 260 °C, 265°C, 270°C, 275°C, 278°C, 288°C or 298°C)
  • the temperature of the six zones is 250 to 290°C (specifically 255°C
  • the rotation speed of the screw is 50 ⁇ 100r/min; specifically 55, 65, 70, 75, 80, 85, 90 or 95r/min;
  • the temperature of the spinning box is 270-290°C (specifically, 270°C, 275°C, 278°C, 280°C, 285°C or 288°C);
  • the cooling air blowing is a side air blowing process and a ring air blowing process.
  • the process conditions are as follows: the wind speed can be 0.30-0.80m/min; the air temperature can be 18-25°C (specifically 18, 19, 20, 22, or 24°C) ; Wind pressure can be 350 ⁇ 500Pa (specifically can be 350, 380, 400, 450 or 480Pa);
  • the amount of oil supplied by the pump is controlled to be 0.3% to 0.5% of the fineness of the product; specifically, it may be 0.4%;
  • the spinning speed is 3000-5000 m/min; specifically, it can be 3500, 4000, 4500, 3800 or 4800 m/min;
  • the cold drafting ratio is 1.01-1.50 (specifically, it can be 1.02, 1.03, 1.2, 1.3, 1.4 or 1.5), and the temperature is 0-20°C, which is a primary drafting;
  • the hot drawing ratio is 3.00 to 5.50 (specifically, 3.5, 4.0, 4.5, and 4.8), and the temperature is 100 to 210 °C (specifically, 150, 180, 190, 200, 208, and 215 °C), and it can be a first-class drafting, two-stage drafting or multi-stage drafting;
  • the setting temperature is 130-200°C (specifically 135, 140, 145, 150, 155, 165, 178, 170, 188 or 190°C), and the setting time is 1-5min (specifically, 1, 2, 3 , 4 or 5min);
  • the flexible post-processing is to prepare polyamide 56 filaments of different styles according to different market demands for products
  • the polyamide 56 tow prepared and formed in step 2) needs to undergo the post-processing process of hot drawing, heat setting and winding in sequence;
  • the thermal drawing process can be one-stage drawing, two-stage drawing or multi-stage drawing, and the temperature is 100-230 ° C (specifically, it can be 110, 115, 120, 125, 130, 135, 140, 145, 150, 155, 165, 178, 170, 188, 190°C, 200, 210 or 220°C), the draft ratio is 1.01 to 2.00 (specifically 1.02, 1.03, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7 or 1.9), the speed of the drafting roll is 500 ⁇ 1500m/min (specifically 800, 900, 1000, 1100, 1200 or 1450m/min); the heat setting temperature is 150 ⁇ 1500m/min 200°C (specifically 155, 165, 178, 170, 188 or 190°C); winding speed is 1000-1500m/min (specifically 1100, 1150, 1200, 1250 or
  • polyamide 56 stretched textured yarn DTY
  • the polyamide 56 tow prepared and formed in step 2) needs to undergo thermal drawing, twisting, networking, heat setting, oiling, and winding in sequence. post-processing;
  • the thermal drawing process can be one-stage drafting, two-stage drafting or multi-stage drafting, and the temperature is 100-200 ° C (specifically can be 110, 115, 120, 125, 130, 135, 140, 145, 150, 155, 165, 178, 170, 188 or 190°C), the draft ratio is 1.01 to 2.00 (specifically 1.02, 1.03, 1.2, 1.3, 1.4, 1.5 , 1.6, 1.7 or 1.9), the speed of the drafting roll is 300 ⁇ 1000m/min (specifically, it can be 400, 500, 600, 700, 800, 900 or 950m/min), and the twisting is divided into S twist or Z twist.
  • Twisting tension 20-60cN (specifically 25, 30, 35, 40, 45, 50 or 55cN), untwisting tension 25-65cN (specifically 25, 30, 35, 40, 45, 50, 55 or 60cN)
  • the 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 to 2.0; in the network step, the wind pressure is 1.0 to 1.6 bar; the diameter of the nozzle is 1.2 to 1.6 mm , the heat setting temperature is 180-220°C (specifically 188, 190, 195, 200, 210 or 215°C), and the winding speed is 600-1200m/min (specifically 650, 700, 750, 800, 850, 900, 950, 1000, 1100 or 1150m/min).
  • step 2 If it is required to prepare polyamide 56 air-textured yarn (ATY), then the polyamide 56 tow prepared and shaped as described in step 2) needs to undergo the post-processing process of thermal drawing, thermal jet deformation, cooling stabilization, and winding in turn;
  • the thermal drawing process can be one-stage drafting, two-stage drafting or multi-stage drafting, the temperature is 100-190 ° C, and the drafting ratio is 1.01-2.00 ( Specifically, it can be 1.02, 1.03, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7 or 1.9), and the speed of the drafting roller is 1500-2500m/min (specifically, it can be 1600, 1650, 1700, 1750, 1800, 1900, 2000, 2100, 2200, 2300 or 2450m/min); thermal jet deformation air temperature 190 ⁇ 230 °C (specifically can be 195, 200, 210, 215, 220 or 225 °C), air injection pressure 195 ⁇ 550kPa (specifically can be 200, 300, 350, 400, 450, 500kPa), overfeed rate 15-30% (specifically 18, 20, 25 or 28%), cooling air temperature 15-30°C (specific
  • the equipment used in the method for preparing polyamide 56 filaments by one-step continuous molding is composed of three units: a polymerization reaction device, a spinning forming device and a flexible post-processing device, wherein the polymerization reaction device is connected with the spinning forming device to directly prepare the polyamide 56 ultra-high-speed filament; according to the different needs of the market for products, connect flexible post-processing devices to prepare polyamide 56 filaments of different styles;
  • the flexible post-processing device connected after the above-mentioned spinning and forming device includes a full-drawn yarn (FDY) preparation device, a stretch-textured yarn (DTY) preparation device, an air-textured yarn (ATY) preparation device, etc.;
  • FDY full-drawn yarn
  • DTY stretch-textured yarn
  • ATY air-textured yarn
  • the polymerization reaction device consists of a raw material still, a salt-forming still (for mixing the two raw materials of pentamethylenediamine and adipic acid in the still, and neutralization reaction), a salt solution storage tank, a salt solution preparation tank, a salt solution Liquid intermediate tank, concentration tank, U-shaped reactor, flash evaporator, pre-polymerizer and post-polymerizer;
  • raw material stills which are respectively a pentamethylene diamine raw material still and an adipic acid raw material still;
  • the spinning forming device consists of a spinning box with a spinneret, a spinning shaft through which the melt stream produced by the spinning box flows, a blowing device for blowing the melt stream, and a After the blowing, the device for clustering and oiling the melt stream is composed of a cold and hot drawing device;
  • the flexible post-processing device is any one of the following flexible post-processing devices a to c:
  • the flexible post-processing device full drawn yarn (FDY) preparation device a is composed of a drafting roller, a setting device and a winding device connected in sequence;
  • the flexible post-processing device stretched textured yarn (DTY) preparation device b is composed of a drafting roller, a false twisting device, a network device, a setting device, an oiling device and a winding device that are connected in sequence;
  • the flexible post-processing device air-textured yarn (ATY) preparation device c is composed of a drawing roll, a cooling device, a jet deformation device, and a winding device connected in sequence, and is used for preparing an air-textured yarn process device.
  • the setting device is a hot plate or a hot box.
  • the linear density of the polyamide 56 filament is 1-7 dtex; the breaking strength is 3-12 cN/dtex, and it has flame retardancy, and the limiting oxygen index is ⁇ 32%.
  • Fig. 1 is a polymerization reaction, spinning and forming device; 1, a raw material kettle; 2, a salt forming kettle; 3, a salt solution storage tank; 4, a salt solution preparation tank; 5, a salt solution intermediate tank; 6, a concentration tank; 7, U-shaped reactor; 8. Flash evaporator; 9. Front polymerizer; 10. Post polymerizer; 11. Spinning box; 12. Air blowing device; 13. Spinning shaft; 14. Cluster oiling device; 15. Roll Winding device; 16. Cold drafting device; 17. Hot drafting device; 18. Forming device;
  • Fig. 2 is a flexible post-processing device used for preparing fully drawn yarn (FDY); 17, a thermal drawing device; 18, a setting device; 22, a winding device.
  • Figure 3 shows the flexible post-processing device used for preparing the drawn textured yarn (DTY); 17, thermal drawing device; 19, false twisting device; 20, network device; 18, setting device; 21, oiling device; 22, winding device.
  • Figure 4 shows a flexible post-processing device used for preparing air-textured yarn (ATY); 17, a thermal drawing device; 23, a thermal jet texturing device; 24, a cooling device, 22, a winding device.
  • Figure 5 is a comparison chart of the dye uptake of nylon 56 and nylon 66.
  • the present invention will be further described below in conjunction with specific embodiments, but the present invention is not limited to the following embodiments.
  • the methods are conventional methods unless otherwise specified.
  • the raw materials can be obtained from open commercial sources unless otherwise specified.
  • the polyamide 56 filament samples in the following examples were tested for performance according to the following methods:
  • Breaking strength and breaking elongation GB/T 14344-2008 Test method for tensile properties of chemical fiber filaments
  • Antibacterial property GB/T 20944.3-2008 Evaluation of antibacterial properties of anti-textiles Part 3 Concussion method.
  • Pentamethylenediamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.01:1, the reaction temperature is 40°C, the reaction time is 50min, and the solution is stirred until completely dissolved to obtain an aqueous polyamide 56 salt solution. Under nitrogen protection, the polyamide 56 salt solution was added to the salt solution preparation tank, 0.5% of the auxiliary pentamethylene diamine was added to the salt solution preparation tank, the pH value of the salt solution was adjusted to 7.73, and the mixed salt solution was concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 210°C and the pressure was 1.70MPa for 120min to carry out the prepolymerization reaction. After the prepolymerization reaction, the pressure was quickly decompressed in the flash vessel. And heat up to 280 °C, enter the front polymerizer, the temperature is 280 °C, last 90min, at this time the degree of polymerization is close to the finished product, and then enter the rear polymerizer, the temperature is 280 °C, and the vacuum degree is 0.25MPa under the conditions of stirring to carry out the polymerization reaction After 50 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 70 r/min, the spinning speed is 4350 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 278 ° C, and the temperature of the second zone is 281 ° C.
  • the temperature in the third zone is 283 °C
  • the temperature in the fourth zone is 283 °C
  • the temperature in the fifth zone is 283 °C
  • the temperature in the sixth zone is 283 °C
  • a thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands through side blowing, and the cooling wind speed is 0.6 m/min
  • the amount of oil supplied by the pump is controlled to be 0.3% of the product fineness, and then cold-drawn at 10°C for 1.10 times, at 145°C for 3.54 times, and set at 155°C for 1min to obtain polyamide 56 tow;
  • the above-mentioned tow is drawn 1.50 times at 170°C, the final drawing roll speed is 1200m/min, heat-set at 180°C, and wound at 1300m/min to become polyamide 56 fully drawn yarn.
  • the performance test results of the fully drawn yarn the breaking strength is 4.93cN/dtex, the breaking elongation is 38.2%, the moisture regain is 4.12%, the melting point is 253.3°C, and the limiting oxygen index is 33.2%.
  • Pentamethylene diamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.02:1, the reaction temperature is 50° C., the reaction time is 40 min, and the solution is stirred until completely dissolved to obtain a polyamide 56 salt solution. Under nitrogen protection, the polyamide 56 salt solution was added to the salt solution preparation tank, 2.5% of the matting agent titanium dioxide was added to the salt solution preparation tank, the pH value of the salt solution was adjusted to 7.86, and the mixed salt solution was concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 218°C and the pressure was 1.73MPa for 100 minutes to carry out the prepolymerization reaction.
  • heat up to 278°C enter the front polymerizer, the temperature is 278°C, and last for 60min.
  • the degree of polymerization is close to the finished product, and then enter the back polymerizer, the temperature is 278°C, and the vacuum degree is 0.21MPa.
  • Stir under the conditions of 0.21MPa to carry out the polymerization reaction After 40 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 65r/min, the spinning speed is 3180m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 290°C, and the temperature of the second zone is 290°C , the temperature in the third zone is 290 °C, the temperature in the fourth zone is 290 °C, the temperature in the fifth zone is 290 °C, and the temperature in the sixth zone is 290 °C; A thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands by side blowing, and the cooling wind speed is 0.8m/min; The amount of oil supplied by the pump is controlled to be 0.35% of the product fineness, and then cold-drawn at 5°C for 1.13 times, at 150°C for 3.32 times, and set at 160°C for 1min to obtain polyamide 56 tow;
  • the above-mentioned tow was drawn 1.71 times at 190°C, the final drafting roll speed was 800m/min, heat-set at 190°C, and wound at 900m/min to become polyamide 56 fully drawn yarn.
  • the performance test results of the fully drawn yarn the breaking strength is 5.86cN/dtex, the breaking elongation is 32.8%, the moisture regain is 4.08%, the melting point is 253.9°C, and the limiting oxygen index is 34.4%.
  • Pentamethylenediamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.05:1, the reaction temperature is 60° C., the reaction time is 30 min, and the solution is stirred until completely dissolved to obtain an aqueous polyamide 56 salt solution. Under nitrogen protection, the polyamide 56 salt solution was added to the salt solution preparation tank, 6% of the flame retardant TL was added to the salt solution preparation tank, the pH value of the salt solution was adjusted to 7.81, and the mixed salt solution was concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 228°C and the pressure was 1.75MPa for 90min and the prepolymerization reaction was carried out.
  • the pressure was quickly decompressed in the flash vessel.
  • the temperature is raised to 283°C, and it enters the front polymerizer, the temperature is 283°C, and lasts for 50 minutes.
  • the degree of polymerization is close to the finished product, and then enters the back polymerizer, and the temperature is 283°C and the vacuum degree is 0.25MPa.
  • Stir under the conditions of 0.25MPa to carry out the polymerization reaction After 40 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 85r/min, the spinning speed is 3710m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 265°C, and the temperature of the second zone is 265°C , the temperature of the third zone is 265 °C, the temperature of the fourth zone is 265 °C, the temperature of the fifth zone is 265 °C, and the temperature of the sixth zone is 265 °C; A thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands through side blowing, and the cooling wind speed is 0.4m/min; The amount of oil supplied by the pump is controlled to be 0.4% of the product fineness, and then cold-drawn at 0°C for 1.06 times, at 160°C for 3.41 times, and set at 170°C for 1min to obtain polyamide 56 tow;
  • the above-mentioned tow was drawn 1.51 times at 190°C, the final drafting roll speed was 1000m/min, heat-set at 200°C, and wound at 1100m/min to become polyamide 56 fully drawn yarn.
  • the performance test results of the fully drawn yarn the breaking strength is 4.71cN/dtex, the breaking elongation is 39.6%, the moisture regain is 4.07%, the melting point is 252.8°C, and the limiting oxygen index is 35.7%.
  • Pentamethylene diamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.02:1, the reaction temperature is 50° C., the reaction time is 35 min, and the solution is stirred until completely dissolved to obtain a polyamide 56 salt solution.
  • the polyamide 56 salt solution was added to the salt solution preparation tank, 2% of the antibacterial agent KS-116 was added to the salt solution preparation tank, the pH value of the salt solution was adjusted to 7.86, and the mixed salt solution was concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 229°C and the pressure was 1.75MPa for 100 minutes to carry out the prepolymerization reaction.
  • the pressure was quickly decompressed in the flash vessel.
  • heat up to 280 °C enter the front polymerizer, the temperature is 280 °C, last 60min, at this time the degree of polymerization is close to the finished product, and then enter the rear polymerizer, the temperature is 280 °C, the vacuum degree is 0.25MPa under the conditions of stirring to carry out the polymerization reaction After 30 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 75 r/min, the spinning speed is 3450 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 276 °C, and the temperature of the second zone is 276 °C , the temperature in the third zone is 276 °C, the temperature in the fourth zone is 276 °C, the temperature in the fifth zone is 276 °C, and the temperature in the sixth zone is 276 °C; A thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands through side blowing, and the cooling wind speed is 0.4m/min; The amount of oil supplied by the pump is controlled to be 0.4% of the product fineness, and then cold-drawn at 10°C for 1.10 times, at 165°C for 3.51 times, and set at 175°C for 1min to obtain polyamide 56 tow;
  • the above-mentioned tow is drawn 1.30 times at 190°C, the final drafting roll speed is 1000m/min, heat-set at 200°C, and wound at 1100m/min to become polyamide 56 fully drawn yarn.
  • the performance test results of the fully drawn yarn the breaking strength is 4.66cN/dtex, the breaking elongation is 40.6%, the moisture regain is 4.01%, the melting point is 252.0°C, the limiting oxygen index is 35.5%, and the fiber antibacterial rate is 91.2%.
  • Pentamethylene diamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.03:1, the reaction temperature is 40° C., the reaction time is 45 min, and the solution is stirred until completely dissolved to obtain an aqueous polyamide 56 salt solution. Under nitrogen protection, the polyamide 56 salt solution is added to the salt solution preparation tank and fully mixed, the pH value of the salt solution is adjusted to 7.83, and the mixed salt solution is concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 217°C and the pressure was 1.75MPa for 150 minutes to carry out the prepolymerization reaction.
  • the pressure was quickly decompressed in the flash vessel.
  • heat up to 285 °C enter the front polymerizer, the temperature is 285 °C, last 80min, at this time the degree of polymerization is close to the finished product, and then enter the rear polymerizer, the temperature is 285 °C, the vacuum degree is 0.25MPa under the conditions of stirring to carry out the polymerization reaction After 60 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 60 r/min, the spinning speed is 3200 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 282 ° C, and the temperature of the second zone is 285 ° C.
  • the temperature in the third zone is 285 °C
  • the temperature in the fourth zone is 285 °C
  • the temperature in the fifth zone is 285 °C
  • the temperature in the sixth zone is 285 °C
  • a thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands through side blowing, and the cooling wind speed is 0.5m/min
  • the amount of oil supplied by the pump is controlled to be 0.3% of the product fineness, and then cold-drawn at 10°C for 1.10 times, at 150°C for 3.11 times, and set at 155°C for 1min to obtain polyamide 56 tow;
  • the polyamide 56 tow is drawn 1.15 times at 170°C, the final draft roll speed is 800m/min, Z twist, twist tension 33cN, untwist tension 37cN; D/Y is 1.5; network wind pressure is 1.0bar ; The diameter of the nozzle is 1.2mm, heat-setting at 180°C, and winding at a speed of 1000m/min to obtain polyamide 56 stretched textured yarn.
  • Pentamethylenediamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.03:1, the reaction temperature is 30°C, the reaction time is 50min, and the solution is stirred until completely dissolved to obtain a polyamide 56 salt solution. Under nitrogen protection, add 3% flame retardant TL-012 salt solution to the polyamide 56 salt solution to fully mix, adjust the pH value of the salt solution to 7.85, and concentrate the mixed salt solution;
  • the concentrated salt solution was injected into the U-type reactor to start the prepolymerization reaction.
  • the temperature was 228°C and the pressure was 1.78MPa for 150min to carry out the prepolymerization reaction.
  • heat up to 286 °C enter the front polymerizer, the temperature is 286 °C, last 90min, at this time the degree of polymerization is close to the finished product, and then enter the rear polymerizer, the temperature is 286 °C, the vacuum degree is 0.26MPa under the conditions of stirring to carry out the polymerization reaction
  • the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 75 r/min, the spinning speed is 3450 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 282° C., and the temperature of the second zone is 282° C.
  • the temperature of the third zone is 282 °C
  • the temperature of the fourth zone is 282 °C
  • the temperature of the fifth zone is 282 °C
  • the temperature of the sixth zone is 282 °C
  • a thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands through side air blowing, and the cooling wind speed is 0.3m/min
  • the amount of oil supplied by the pump is controlled to be 0.4% of the fineness of the product, and then cold-drawn at 3°C for 1.18 times, at 120°C for 3.20 times, and set at 130°C for 2 minutes to obtain polyamide 56 tow;
  • the polyamide 56 tow is drawn 1.31 times at 160°C, the final drafting roll speed is 1000m/min, S twist, twist tension 20cN, untwist tension 25cN; D/Y is 1.6; network wind pressure is 1.2bar ; The diameter of the nozzle is 1.3mm, heat-setting at 180°C, and winding at a speed of 1000m/min to obtain polyamide 56 stretched textured yarn.
  • the performance test results of the stretched textured yarn the breaking strength is 4.64cN/dtex, the breaking elongation is 32.6%, the moisture regain is 4.46%, the melting point is 252.1°C, and the limiting oxygen index is 35.7%.
  • Pentamethylene diamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.02:1, the reaction temperature is 45° C., the reaction time is 40 min, and the solution is stirred until completely dissolved to obtain a polyamide 56 salt solution. Under nitrogen protection, add 3% antibacterial agent KS-116 salt solution to the polyamide 56 salt solution and mix thoroughly, adjust the pH value of the salt solution to 7.80, and concentrate the mixed salt solution;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 212°C and the pressure was 1.82MPa for 150 minutes to carry out the prepolymerization reaction.
  • the pressure was quickly decompressed in the flash vessel.
  • heat up to 283°C enter the front polymerizer, the temperature is 283°C, and last for 100min.
  • the degree of polymerization is close to the finished product, and then enter the back polymerizer, the temperature is 283°C, and the vacuum degree is 0.28MPa.
  • Stir under the conditions of 0.28MPa to carry out the polymerization reaction After 30 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 83r/min, the spinning speed is 4150m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 287°C, and the temperature of the second zone is 287°C.
  • the temperature in the third zone is 287 °C
  • the temperature in the fourth zone is 287 °C
  • the temperature in the fifth zone is 287 °C
  • the temperature in the sixth zone is 287 °C
  • a thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands by side blowing, and the cooling wind speed is 0.4m/min
  • the amount of oil supplied by the pump is controlled to be 0.4% of the product fineness, and then cold-drawn at 8°C for 1.24 times, at 145°C for 3.25 times, and set at 155°C for 1.5min to obtain polyamide 56 tow;
  • the polyamide 56 tow is drawn 1.46 times at 190°C, the final drafting roll speed is 900m/min, S twist, twist tension 40cN, untwisting tension 45cN; D/Y is 1.8; network wind pressure is 1.3bar ; The diameter of the nozzle is 1.6mm, heat-setting at 200°C, and winding at a speed of 1000m/min to obtain polyamide 56 stretched textured yarn.
  • Pentamethylenediamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.05:1, the reaction temperature is 45° C., the reaction time is 40 min, and the solution is stirred until completely dissolved to obtain an aqueous polyamide 56 salt solution. Under nitrogen protection, the polyamide 56 salt solution is added to the salt solution preparation tank and fully mixed, the pH value of the salt solution is adjusted to 7.86, and the mixed salt solution is concentrated;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 238°C and the pressure was 1.85MPa for 180 minutes to carry out the prepolymerization reaction.
  • the pressure was quickly decompressed in the flasher.
  • heat up to 288°C enter the front polymerizer, the temperature is 288°C, and last for 50min.
  • the degree of polymerization is close to the finished product, and then enter the back polymerizer, the temperature is 288°C, and the vacuum degree is 0.28MPa.
  • Stir under the conditions of 0.28MPa to carry out the polymerization reaction After 15 minutes, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 80 r/min, the spinning speed is 3600 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 290 °C, and the temperature of the second zone is 290 °C , the temperature in the third zone is 290 °C, the temperature in the fourth zone is 290 °C, the temperature in the fifth zone is 290 °C, and the temperature in the sixth zone is 290 °C; A thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands by side blowing, and the cooling wind speed is 0.5m/min; The amount of oil supplied by the pump is controlled to be 0.3% of the product fineness, and then after cold drawing at 10°C 1.14 times, 150°C drafting 3.83 times, and 155°C setting for 1min, polyamide 56 tow is obtained;
  • the polyamide 56 tow was drawn 1.31 times at 165°C, the final drafting roll speed was 2000m/min, hot air jet deformation at 210°C, air jet pressure 280kPa, overfeed rate 18%, 15°C air cooling, and then 2000m /min speed winding to obtain polyamide 56 air textured yarn.
  • Pentamethylenediamine and adipic acid are neutralized and salt-formed in water according to the ratio of 1.04:1, the reaction temperature is 50°C, the reaction time is 35min, and the solution is stirred until completely dissolved to obtain a polyamide 56 salt solution. Under nitrogen protection, add 4% flame retardant FR-310 salt solution to the polyamide 56 salt solution to fully mix, adjust the pH value of the salt solution to 7.84, and concentrate the mixed salt solution;
  • the concentrated salt solution was injected into the U-shaped reactor to start the prepolymerization reaction.
  • the temperature was 230°C and the pressure was 1.80MPa for 160min to carry out the prepolymerization reaction. After the prepolymerization reaction, the pressure was quickly decompressed in the flasher. And heat up to 286 °C, enter the front polymerizer, the temperature is 286 °C, last 100min, at this time the degree of polymerization is close to the finished product, and then enter the rear polymerizer, the temperature is 286 °C, and the vacuum degree is 0.3MPa under the conditions of stirring to carry out the polymerization reaction After 40 min, the water in the system was discharged to complete the polymerization reaction to obtain a polyamide 56 polymer melt.
  • the polyamide 56 polymer melt is extruded through a screw, the rotation speed of the screw is 80 r/min, the spinning speed is 3200 m/min, and the temperature of each zone of the screw used is as follows: the temperature of the first zone is 293 °C, and the temperature of the second zone is 293 °C , the temperature in the third zone is 293 °C, the temperature in the fourth zone is 293 °C, the temperature in the fifth zone is 293 °C, and the temperature in the sixth zone is 293 °C; A thin stream of melt is obtained, and the thin stream of melt is cooled and solidified into strands by side blowing, and the cooling wind speed is 0.8m/min; The amount of oil supplied by the pump is controlled to be 0.5% of the product fineness, and then cold-drawn at 0°C for 1.08 times, at 155°C for 4.14 times, and set at 165°C for 1min to obtain polyamide 56 tow;
  • the polyamide 56 tow was drawn 1.18 times at 170°C, the final drafting roll speed was 1800m/min, hot air jet deformation at 190°C, air jet pressure 350kPa, overfeed rate 20%, 18°C air cooling, and then 2000m /min speed winding to obtain polyamide 56 air textured yarn.
  • polyamide 56 salt solution and polymer in the early stage is exactly the same as that of Example 1.
  • the polymer melt is sprayed through the screw extruder and the spinneret of the spinning box to obtain a thin stream of melt, it is cooled by a side blowing device.
  • the traditional spinning process is carried out, and post-processing processes such as clustering are directly carried out (the process parameters are set according to Example 1 of the present invention) to prepare different types of filaments.
  • the polyamide 56 filament prepared by this process has poor performance and many filaments, and some filaments cannot be wound, easy to fry, and cannot be formed. This is because the cooling rate of polyamide 56 is higher than that of polyamide 66. Slow, the temperature of the filament before winding is still very high, and the filament cannot dissipate heat in time during high-speed winding, so the fuse phenomenon will occur, and the explosion may even occur due to the high temperature. Under the experimental conditions, the performance of the filaments formed by winding is tested. The breaking strength is only 0.5-2.0cN/dtex, and the limiting oxygen index is 20-24%. The filaments prepared by this process have low strength and no flame retardant properties. And the performance is unstable and cannot meet the application standards.
  • the cooling and drafting process is added in the spinning process.
  • the tow not only has an impact on the winding and oiling process, but also the properties of the products prepared by direct post-processing are unstable. Therefore, the addition of the cooling and drawing process makes the tow formed by the spinneret rapidly cool, and the molecular chains rapidly accumulate and crystallize. It is not perfect, which is conducive to the subsequent drawing and shaping at high temperature to obtain polyamide filaments with stable performance and excellent quality.
  • the patented process has short process, low energy consumption, low cost, stable product and strong functionality.
  • polyamide filaments can be prepared according to different needs, providing guidance for the industrialized one-step spinning of bio-based polyamide and polyamide polymer filaments.
  • the polyamide 56 filament prepared by the invention can be widely used in the fields of textile industry, automobile industry, home improvement, electronic appliance industry, construction industry and the like.

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Abstract

一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备，制备工艺主要包括三部分：聚酰胺盐液聚合工艺、纺丝成型工艺、柔性后加工工艺，一步连续制备得到全拉伸丝或拉伸变形丝或空气变形丝。

Description

一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备 技术领域
本发明属于纺织领域，涉及一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备。
背景技术
聚酰胺(PA)是一种重要纤维，俗称“尼龙”，是世界上第一个商业化的合成纤维制品，它于终端用途领域，带来了实实在在的优势：在服装织物中它具有更好的吸湿性、挠曲和悬垂性，手感更柔软；在工业领域它具有难以致信的耐久性和抗压性；在地毯方面，它的抗磨损性和层叠回复力高于其它任何纤维。此外，聚酰胺纤维最终产品具有低的初始模量，良好的弹性回复性，优异的耐磨性能，以及高的抗断裂强力，可制备高性能材料。
聚酰胺纤维的生产通常采用的是熔体纺丝法工艺。熔体纺丝，一般有两种方法，切片熔融纺丝法和熔体直接纺丝法。切片纺丝工艺，先需要将高聚物制成切片，切片经萃取、干燥，再熔融纺丝，切片纺丝法产品质量好、生产柔性，但是生产成本高。熔体直纺纺丝工艺，是将聚合物熔体直接送到纺丝机进行纺丝，熔体经过特定的设备加压，从喷丝板挤出形成熔体细流，冷却固化形成初生纤维，再将纤维卷绕在特定的受丝机构上。为了达到成品纤维的要求，初生纤维还需要进行一系列的后续处理步骤，如拉伸、定型、变形等，该工艺省去了注带、造粒等工序，工艺流程短，节能高效，但是该方法对聚合和纺丝的稳定性要求较高。
目前，我国聚酰胺纤维熔体直纺工艺技术尚未成熟，纺丝稳定性差，因此工业化生产制备聚酰胺66和聚酰胺6纤维的工艺主要采用切片纺丝法，该工艺步骤繁琐、耗时长、能耗高。因而针对新型生物基聚酰胺56纤维，亟需开发一种高效节能，集聚合、纺丝、牵伸一步连续成型为一体的制备工艺。
发明公开
本发明的目的是提供一种聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备。
本发明提供一种聚酰胺56长丝一步连续成型与柔性变形制备工艺，主要分为三部分：聚酰胺盐液聚合工艺、纺丝成型工艺、柔性后加工工艺，采用 本发明方法可以一步连续制备全拉伸丝(FDY)，拉伸变形丝(DTY)、空气变形丝(ATY)等。
本发明提供的一步连续成型与柔性变形制备聚酰胺56长丝的方法，包括聚酰胺盐液聚合工艺、纺丝成型工艺、柔性后加工工艺；
1)聚酰胺盐液聚合工艺：
在氮气保护下，戊二胺和己二酸在水中进行中和成盐反应，得到聚酰胺56盐水溶液，聚酰胺56盐水溶液加入助剂调配混合后浓缩，浓缩后的盐液经过预聚合反应、前聚合反应、后聚合反应，得到聚酰胺56聚合物熔体；
上述聚合工艺中，所述氮气保护为三冲三排；所述三冲即三次冲氮气；三排即排空气；
上述聚合工艺中，所述戊二胺与己二酸的摩尔比为1～1.05：1；具体为1:1.01、1:1.02、1:1.03、1:1.04；
上述聚合工艺中，所述中和成盐反应温度为30～50℃；具体为30℃、35℃、40℃、45℃；反应时间为30～60min；具体为35、40、45、50、55min；
上述聚合工艺中，所述聚酰胺56盐水溶液的质量百分含量为20％～80％；具体为25、30、35、40、45、50、55或75％；
上述聚合工艺中，所述助剂可以为分子量调节剂、消光剂、阻燃剂、抗静电剂、抗菌剂等其中的一种或多种；所述助剂的加入量为所述戊二胺与己二酸质量之和的0.1％～6％；具体为0.1-1或0.1-0.5％；
上述聚合工艺中，制备的聚酰胺56聚合物熔体的粘度指数为120～160ml/g。
上述聚合工艺中，预聚反应条件：温度210～240℃(具体为212℃、217℃、218℃、228℃、229℃、238℃)、压强1.70～1.85MPa(具体为1.73、1.75、1.78、1.8、1.82MPa)，保压时间30min～180min(具体为90、100、120、150、160min)；反应结束后快速闪蒸解压，并升温至270～290℃(具体为278℃、285℃、286℃)；前聚合反应条件：温度270℃～290℃(具体为278℃、285℃、286℃)，反应时间20min～150min(具体为50、60、80、90或100min)；后聚合反应条件：温度270℃～290℃(具体为278℃、280℃或288℃)，真空度0.2～0.3MPa(具体为0.21、0.25、0.26或0.28MPa)，反应时间10min～150min(具体为15、30、40、50或60min)，排出体系中的水分，得到聚酰胺56聚合物熔体；
2)纺丝成型工艺：
步骤1)中制备的聚酰胺56聚合物熔体由螺杆挤压后，经喷丝板喷出得到熔体细流，熔体细流经过冷却吹风凝固成为丝条，丝条经过卷绕上油、冷热牵伸，热定型得到聚酰胺56丝束；
上述纺丝成型步骤中，所用螺杆各区温度依次为：一区温度为260～300℃(具体为260℃、265℃、270℃、275℃、278℃、288℃或298℃)，二区温度为260～300℃(具体为260℃、265℃、270℃、275℃、278℃、288℃或298℃)，三区温度为250～295℃(具体为255℃、260℃、265℃、270℃、275℃、278℃、288℃或298℃)，四区温度为250～295℃(具体为255℃、260℃、265℃、270℃、275℃、278℃、288℃或298℃)，五区温度为250～290℃(具体为255℃、260℃、265℃、270℃、275℃、278℃、288℃或298℃)，六区温度为250～290℃(具体为255℃、260℃、265℃、270℃、275℃、278℃、288℃或298℃)；
螺杆的转速为50～100r/min；具体为55、65、70、75、80、85、90或95r/min；
所述纺丝箱体的温度为270～290℃(具体为270℃、275℃、278℃、280℃、285℃或288℃)；
所述冷却吹风为侧吹风工艺、环吹风工艺，其工艺条件：风速可为0.30～0.80m/min；风温可为18～25℃(具体为18、19、20、22、或24℃)；风压可为350～500Pa(具体可为350、380、400、450或480Pa)；
所述上油步骤中，泵供量控制上油量为产品纤度的0.3％～0.5％；具体可为0.4％；
所述纺丝成型工艺中，纺丝速度为3000～5000m/min；具体可为3500、4000、4500、3800或4800m/min；
所述牵伸步骤中，包括冷牵伸、热牵伸步骤；
所述冷牵伸倍率1.01～1.50(具体可为1.02、1.03、1.2、1.3、1.4或1.5)，温度为0～20℃，为一级牵伸；
所述热牵伸倍率3.00～5.50(具体可为3.5、4.0、4.5、4.8)，温度为100～210℃(具体可为150、180、190、200、208、215℃)，可为一级牵伸、二级牵伸或多级牵伸；
所述定型温度为130～200℃(具体可为135、140、145、150、155、165、 178、170、188或190℃)，定型时间为1～5min(具体可为1、2、3、4或5min)；
3)柔性后加工工艺：
所述柔性后加工是根据市场对产品的不同需求，制备不同风格的聚酰胺56长丝；
若要求制备聚酰胺56全拉伸丝(FDY)，则步骤2)中所述制备成型的聚酰胺56丝束需依次经过热牵伸、热定型、卷绕的后加工过程；
上述柔性后加工步骤中，制备全牵伸丝工艺条件：热牵伸过程可为一级牵伸、二级牵伸或多级牵伸，温度为100～230℃(具体可为110、115、120、125、130、135、140、145、150、155、165、178、170、188、190℃、200、210或220℃)，牵伸倍数为1.01～2.00(具体可为1.02、1.03、1.2、1.3、1.4、1.5、1.6、1.7或1.9)，牵伸辊速度为500～1500m/min(具体可为800、900、1000、1100、1200或1450m/min)；热定型温度为150～200℃(具体可为155、165、178、170、188或190℃)；卷绕速度为1000～1500m/min(具体可为1100、1150、1200、1250或1450m/min)；
若要求制备聚酰胺56拉伸变形丝(DTY)，则步骤2)中所述制备成型的聚酰胺56丝束需依次经过热牵伸、加捻、网络、热定型、上油、卷绕的后加工过程；
上述柔性后加工步骤中，制备拉伸变形丝工艺条件：热牵伸过程可为一级牵伸、二级牵伸或多级牵伸，温度为100～200℃(具体可为110、115、120、125、130、135、140、145、150、155、165、178、170、188或190℃)，牵伸倍数为1.01～2.00(具体可为1.02、1.03、1.2、1.3、1.4、1.5、1.6、1.7或1.9)，牵伸辊速度为300～1000m/min(具体可为400、500、600、700、800、900或950m/min)，加捻分为S捻或Z捻，加捻张力20～60cN(具体可为25、30、35、40、45、50或55cN)，解捻张力25～65cN(具体可为25、30、35、40、45、50、55或60cN)；所述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；所述网络步骤中，风压为1.0～1.6bar；喷嘴直径为1.2～1.6mm，热定型温度为180～220℃(具体可为188、190、195、200、210或215℃)，所述卷绕速度为600～1200m/min(具体可为650、700、750、800、850、900、950、1000、1100或1150m/min)。
若要求制备聚酰胺56空气变形丝(ATY)，则步骤2)中所述制备成型的 聚酰胺56丝束需依次经过热牵伸、热喷射变形、冷却稳定、卷绕的后加工过程；
上述柔性后加工步骤中，制备空气变形丝工艺条件：热牵伸过程可为一级牵伸、二级牵伸或多级牵伸，温度为100～190℃，牵伸倍数为1.01～2.00(具体可为1.02、1.03、1.2、1.3、1.4、1.5、1.6、1.7或1.9)，牵伸辊速度为1500～2500m/min(具体可为1600、1650、1700、1750、1800、1900、2000、2100、2200、2300或2450m/min)；热喷射变形空气温度190～230℃(具体可为195、200、210、215、220或225℃)，空气喷射压力195～550kPa(具体可为200、300、350、400、450、500kPa)，超喂率15～30％(具体可为18、20、25或28％)，冷却空气温度15～30℃(具体可为18、20、25或28℃)，所述卷绕速度为1500～2800m/min(具体可为1600、1650、1700、1750、1800、1900、2000、2100、2200、2300、2450、2500、2600、2700或2750m/min)。
所述一步连续成型制备聚酰胺56长丝的方法所用设备，由聚合反应装置、纺丝成型装置和柔性后加工装置三个单元组成，其中聚合反应装置与纺丝成型装置相连，直接制备聚酰胺56超高速长丝；再根据市场对产品的不同需求，连接柔性后加工装置，从而制备不同风格的聚酰胺56长丝；
上述纺丝成型装置后连接的柔性后加工装置，包括全拉伸丝(FDY)制备装置、拉伸变形丝(DTY)制备装置，空气变形丝(ATY)制备装置等；
所述聚合反应装置由依次连接的原料釜、成盐釜(用于将戊二胺和己二酸两种原料在釜中混合，发生中和反应)、盐液储罐、盐液调配罐、盐液中间罐、浓缩槽、U型反应器、闪蒸器、前聚合器和后聚合器组成；
具体的，所述原料釜为两个，分别为戊二胺原料釜、己二酸原料釜；
所述纺丝成型装置由带喷丝板的纺丝箱体、纺丝箱体产出的熔体细流流经的纺丝甬道、对所述熔体细流进行吹风的吹风装置和在所述吹风后对所述熔体细流进行集束上油的装置和冷热牵伸装置组成；
所述柔性后加工装置为如下柔性后加工装置a～c中任意一种：
所述柔性后加工装置全拉伸丝(FDY)制备装置a由依次连接的牵伸辊、定型装置和卷绕装置组成；
所述柔性后加工装置拉伸变形丝(DTY)制备装置b由依次连接的牵伸辊、假捻装置、网络装置、定型装置、上油装置和卷绕装置组成；
所述柔性后加工装置空气变形丝(ATY)制备装置c由依次连接的牵伸 辊、冷却装置、喷射变形装置、卷绕装置组成，用于制备空气变形丝工艺装置。
所述柔性后加工中，定型装置为热板或热箱。
具体的，所述聚酰胺56长丝的线密度为1～7dtex；断裂强度为3～12cN/dtex，具有阻燃性，极限氧指数≥32％。
附图说明
图1为聚合反应、纺丝成型装置；1、原料釜；2、成盐釜；3、盐液储罐；4、盐液调配罐；5、盐液中间罐；6、浓缩槽；7、U型反应器；8、闪蒸器；9、前聚合器；10、后聚合器；11、纺丝箱体；12、吹风装置；13、纺丝甬道；14、集束上油装置；15、卷绕装置；16、冷牵伸装置；17、热牵伸装置；18、定型装置；
图2为制备全牵伸丝(FDY)所用柔性后加工装置；17、热牵伸装置；18、定型装置；22、卷绕装置。
图3为制备拉伸变形丝(DTY)所用柔性后加工装置；17、热牵伸装置；19、假捻装置；20、网络装置；18、定型装置；21、上油装置；22、卷绕装置。
图4为制备空气变形丝(ATY)所用柔性后加工装置；17、热牵伸装置；23、热喷射变形装置；24、冷却装置、22、卷绕装置。
[根据细则91更正 11.05.2021]　
图5为锦纶56和锦纶66上染率对比图。
实施发明的最佳方式
下面结合具体实施例对本发明作进一步阐述，但本发明并不限于以下实施例。所述方法如无特别说明均为常规方法。所述原材料如无特别说明均能从公开商业途径获得。下述实施例中聚酰胺56长丝样品，根据以下方法检测性能：
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；
2.回潮率：GB/T6503-2017 化学纤维 回潮率试验方法；
3.极限氧指数：GB/T5454-1997 纺织品 燃烧性能试验 氧指数法；
4.熔点：采用美国TA公司的Q2000型差示扫描量热仪进行测试，在氮气保护下，以10℃/min的速度从室温升到300℃；
5.抗菌性：GB/T 20944.3-2008 防纺织品抗菌性能的评价 第3部分 震荡 法。
实施例1、
将戊二胺和己二酸按照1.01：1的比例在水中进行中和成盐反应，反应温度40℃，反应时间50min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐，在盐液调配罐中加入0.5％的助剂戊二胺，调节盐液pH值7.73，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为210℃、压强为1.70MPa的条件下保压120min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至280℃，进入前聚合器，温度为280℃，持续90min，此时聚合度接近成品，再进入后聚合器，温度为280℃，真空度为0.25MPa的条件下搅拌，进行聚合反应50min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为70r/min，纺丝速度4350m/min，所用螺杆各区温度依次为：一区温度为278℃，二区温度为281℃，三区温度为283℃，四区温度为283℃，五区温度为283℃，六区温度为283℃；纺丝箱体温度285℃，聚合物经螺杆挤压，由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0.6m/min；风温为21℃，风压可为400Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.3％，然后经过10℃冷牵伸1.10倍，145℃牵伸3.54倍，155℃定型1min，得到聚酰胺56丝束；
上述丝束再经过170℃牵伸1.50.倍，终极牵伸辊速度为1200m/min，180℃热定型，以1300m/min卷绕成为聚酰胺56全拉伸丝。
全拉伸丝性能检测结果：断裂强度4.93cN/dtex，断裂伸长率38.2％，回潮率4.12％，熔点253.3℃，极限氧指数33.2％。
实施例2、
将戊二胺和己二酸按照1.02：1的比例在水中进行中和成盐反应，反应温度50℃，反应时间40min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐，在盐液调配罐中加入2.5％的消光剂二氧化钛，调节盐液pH值7.86，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为218℃、压强为1.73MPa的条件下保压100min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至278℃，进入前聚合器，温度为278℃，持续60min，此时聚合度接近成品，再进入后聚合器，温度为278℃，真空度为0.21MPa的条件下搅拌，进行聚合反应40min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为65r/min，纺丝速度3180m/min，所用螺杆各区温度依次为：一区温度为290℃，二区温度为290℃，三区温度为290℃，四区温度为290℃，五区温度为290℃，六区温度为290℃；纺丝箱体温度290℃，聚合物经螺杆挤压，由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0.8m/min；风温为25℃，风压可为480Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.35％，然后经过5℃冷牵伸1.13倍，150℃牵伸3.32倍，160℃定型1min，得到聚酰胺56丝束；
上述丝束再经过190℃牵伸1.71倍，终极牵伸辊速度为800m/min，190℃热定型，以900m/min卷绕成为聚酰胺56全拉伸丝。
全拉伸丝性能检测结果：断裂强度5.86cN/dtex，断裂伸长率32.8％，回潮率4.08％，熔点253.9℃，极限氧指数34.4％。
实施例3、
将戊二胺和己二酸按照1.05：1的比例在水中进行中和成盐反应，反应温度60℃，反应时间30min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐，在盐液调配罐中加入6％的阻燃剂TL，调节盐液pH值7.81，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为228℃、压强为1.75MPa的条件下保压90min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至283℃，进入前聚合器，温度为283℃，持续50min，此时聚合度接近成品，再进入后聚合器，温度为283℃，真空度为0.25MPa的条件下搅拌，进行聚合反应40min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为85r/min，纺丝 速度3710m/min，所用螺杆各区温度依次为：一区温度为265℃，二区温度为265℃，三区温度为265℃，四区温度为265℃，五区温度为265℃，六区温度为265℃；纺丝箱体温度265℃，聚合物经螺杆挤压，由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0.4m/min；风温为21℃，风压可为380Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.4％，然后经过0℃冷牵伸1.06倍，160℃牵伸3.41倍，170℃定型1min，得到聚酰胺56丝束；
上述丝束再经过190℃牵伸1.51倍，终极牵伸辊速度为1000m/min，200℃热定型，以1100m/min卷绕成为聚酰胺56全拉伸丝。
全拉伸丝性能检测结果：断裂强度4.71cN/dtex，断裂伸长率39.6％，回潮率4.07％，熔点252.8℃，极限氧指数35.7％。
实施例4、
将戊二胺和己二酸按照1.02：1的比例在水中进行中和成盐反应，反应温度50℃，反应时间35min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐，在盐液调配罐中加入2％的抗菌剂KS-116，调节盐液pH值7.86，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为229℃、压强为1.75MPa的条件下保压100min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至280℃，进入前聚合器，温度为280℃，持续60min，此时聚合度接近成品，再进入后聚合器，温度为280℃，真空度为0.25MPa的条件下搅拌，进行聚合反应30min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为75r/min，纺丝速度3450m/min，所用螺杆各区温度依次为：一区温度为276℃，二区温度为276℃，三区温度为276℃，四区温度为276℃，五区温度为276℃，六区温度为276℃；纺丝箱体温度276℃，聚合物经螺杆挤压，由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0.4m/min；风温为20℃，风压可为400Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.4％，然后经过10℃冷牵伸1.10倍，165℃牵伸3.51倍，175℃定型1min，得到聚酰胺56丝束；
上述丝束再经过190℃牵伸1.30倍，终极牵伸辊速度为1000m/min，200℃热定型，以1100m/min卷绕成为聚酰胺56全拉伸丝。
全拉伸丝性能检测结果：断裂强度4.66cN/dtex，断裂伸长率40.6％，回潮率4.01％，熔点252.0℃，极限氧指数35.5％，纤维抑菌率91.2％。
实施例5、
将戊二胺和己二酸按照1.03：1的比例在水中进行中和成盐反应，反应温度40℃，反应时间45min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐充分混合，调节盐液pH值7.83，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为217℃、压强为1.75MPa的条件下保压150min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至285℃，进入前聚合器，温度为285℃，持续80min，此时聚合度接近成品，再进入后聚合器，温度为285℃，真空度为0.25MPa的条件下搅拌，进行聚合反应60min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为60r/min，纺丝速度3200m/min，所用螺杆各区温度依次为：一区温度为282℃，二区温度为285℃，三区温度为285℃，四区温度为285℃，五区温度为285℃，六区温度为285℃；纺丝箱体温度286℃，聚合物经螺杆挤压，由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0.5m/min；风温为20℃，风压可为430Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.3％，然后经过10℃冷牵伸1.10倍，150℃牵伸3.11倍，155℃定型1min，得到聚酰胺56丝束；
聚酰胺56丝束在170℃温度下牵伸1.15倍，终极牵伸辊速度为800m/min，Z捻，加捻张力33cN，解捻张力37cN；D/Y为1.5；网络风压为1.0bar；喷嘴直径为1.2mm，180℃热定型，以1000m/min速度卷绕，得到聚酰胺56拉伸变形丝。
拉伸变形丝性能检测结果：断裂强度4.34cN/dtex，断裂伸长率44.7％，回潮率4.76％，熔点252.5℃，极限氧指数35.5％。
实施例6、
将戊二胺和己二酸按照1.03：1的比例在水中进行中和成盐反应，反应温度30℃，反应时间50min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入3％阻燃剂TL-012盐液调配罐充分混合，调节盐液pH值7.85，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为228℃、压强为1.78MPa的条件下保压150min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至286℃，进入前聚合器，温度为286℃，持续90min，此时聚合度接近成品，再进入后聚合器，温度为286℃，真空度为0.26MPa的条件下搅拌，进行聚合反应50min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为75r/min，纺丝速度3450m/min，所用螺杆各区温度依次为：一区温度为282℃，二区温度为282℃，三区温度为282℃，四区温度为282℃，五区温度为282℃，六区温度为282℃；纺丝箱体温度283℃，聚合物经螺杆挤压，由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0.3m/min；风温为20℃，风压可为460Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.4％，然后经过3℃冷牵伸1.18倍，120℃牵伸3.20倍，130℃定型2min，得到聚酰胺56丝束；
聚酰胺56丝束在160℃温度下牵伸1.31倍，终极牵伸辊速度为1000m/min，S捻，加捻张力20cN，解捻张力25cN；D/Y为1.6；网络风压为1.2bar；喷嘴直径为1.3mm，180℃热定型，以1000m/min速度卷绕，得到聚酰胺56拉伸变形丝。
拉伸变形丝性能检测结果：断裂强度4.64cN/dtex，断裂伸长率32.6％，回潮率4.46％，熔点252.1℃，极限氧指数35.7％。
实施例7、
将戊二胺和己二酸按照1.02：1的比例在水中进行中和成盐反应，反应温度45℃，反应时间40min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入3％抗菌剂KS-116盐液调配罐充分混合，调节盐液pH值7.80，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为212℃、压强为1.82MPa的条件下保压150min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至283℃，进入前聚合器，温度为283℃，持续100min，此时聚合度接近成品，再进入后聚合器，温度为283℃，真空度为0.28MPa的条件下搅拌，进行聚合反应30min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为83r/min，纺丝速度4150m/min，所用螺杆各区温度依次为：一区温度为287℃，二区温度为287℃，三区温度为287℃，四区温度为287℃，五区温度为287℃，六区温度为287℃；纺丝箱体温度287℃，聚合物经螺杆挤压，由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0.4m/min；风温为22℃，风压可为420Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.4％，然后经过8℃冷牵伸1.24倍，145℃牵伸3.25倍，155℃定型1.5min，得到聚酰胺56丝束；
聚酰胺56丝束在190℃温度下牵伸1.46倍，终极牵伸辊速度为900m/min，S捻，加捻张力40cN，解捻张力45cN；D/Y为1.8；网络风压为1.3bar；喷嘴直径为1.6mm，200℃热定型，以1000m/min速度卷绕，得到聚酰胺56拉伸变形丝。
拉伸变形丝性能检测结果：断裂强度5.04cN/dtex，断裂伸长率32.5％，回潮率4.16％，熔点252.5℃，极限氧指数33.7％，纤维抑菌率.93.3％
实施例8、
将戊二胺和己二酸按照1.05：1的比例在水中进行中和成盐反应，反应温度45℃，反应时间40min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入盐液调配罐充分混合，调节盐液pH值7.86，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为238℃、压强为1.85MPa的条件下保压180min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至288℃，进入前聚合器，温度为288℃，持续50min，此时聚合度接近成品，再进入后聚合器，温度为288℃，真空度为0.28MPa的条件下搅拌，进行聚合反应15min，排出体系中的水分，完成聚合反应， 得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为80r/min，纺丝速度3600m/min，所用螺杆各区温度依次为：一区温度为290℃，二区温度为290℃，三区温度为290℃，四区温度为290℃，五区温度为290℃，六区温度为290℃；纺丝箱体温度290℃，聚合物经螺杆挤压，由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0.5m/min；风温为20℃，风压可为450Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.3％，然后经过10℃冷牵伸1.14倍，150℃牵伸3.83倍，155℃定型1min，得到聚酰胺56丝束；
聚酰胺56丝束在165℃牵伸1.31倍，终极牵伸辊速度为2000m/min，210℃下热空气喷射变形，空气喷射压力280kPa，超喂率18％，15℃空气冷却，然后以2000m/min速度卷绕，得到聚酰胺56空气变形丝。
空气变形丝性能检测结果：断裂强度5.11cN/dtex，断裂伸长率20.2％，回潮率4.18％，熔点251.7℃，极限氧指数33.4％。
实施例9、
将戊二胺和己二酸按照1.04：1的比例在水中进行中和成盐反应，反应温度50℃，反应时间35min，搅拌至完全溶解，得到聚酰胺56盐水溶液。在氮气保护下，在聚酰胺56盐水溶液加入4％阻燃剂FR-310盐液调配罐充分混合，调节盐液pH值7.84，经混合后的盐液进行浓缩；
将浓缩后的盐液注入U型反应器，开始预聚反应，温度为230℃、压强为1.80MPa的条件下保压160min进行预聚反应，预聚反应结束后，在闪蒸器中快速解压，并升温至286℃，进入前聚合器，温度为286℃，持续100min，此时聚合度接近成品，再进入后聚合器，温度为286℃，真空度为0.3MPa的条件下搅拌，进行聚合反应40min，排出体系中的水分，完成聚合反应，得到聚酰胺56聚合物熔体。
将所述聚酰胺56聚合物熔体经螺杆挤压，螺杆的转速为80r/min，纺丝速度3200m/min，所用螺杆各区温度依次为：一区温度为293℃，二区温度为293℃，三区温度为293℃，四区温度为293℃，五区温度为293℃，六区温度为293℃；纺丝箱体温度293℃，聚合物经螺杆挤压，由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0.8m/min；风温 为18℃，风压可为480Pa，再对所述冷却后丝条上油，泵供量控制上油量为产品纤度的0.5％，然后经过0℃冷牵伸1.08倍，155℃牵伸4.14倍，165℃定型1min，得到聚酰胺56丝束；
聚酰胺56丝束在170℃牵伸1.18倍，终极牵伸辊速度为1800m/min，190℃下热空气喷射变形，空气喷射压力350kPa，超喂率20％，18℃空气冷却，然后以2000m/min速度卷绕，得到聚酰胺56空气变形丝。
空气变形丝性能检测结果：断裂强度5.05cN/dtex，断裂伸长率31.7％，回潮率4.20％，熔点252.1℃，极限氧指数36.8％。
对比例1
前期聚酰胺56盐溶液、聚合物制备与实施例1完全相同，当聚合物熔体经螺杆挤压机、纺丝箱体的喷丝板喷出得到熔体细流，经侧吹风装置，冷却凝固成为丝条，上油后，按照传统纺丝加工进行，直接进行集束等后加工工艺(工艺参数参照本发明实施例1设定)制备不同类别的长丝。
试验结果发现，该工艺制备的聚酰56长丝性能差，毛丝多，部分长丝无法进行卷绕，容易炸筒，无法成形，这是由于聚酰胺56要比聚酰胺66的降温冷却速度慢，导致卷绕之前长丝的温度仍然很高，在高速卷绕的时候长丝不能及时散热，因此会发生熔丝现象，由于温度过高甚至发生炸筒。在该实验条件下，测试卷绕成型的长丝性能，断裂强度低仅为0.5～2.0cN/dtex，极限氧指数20～24％，该工艺制备的长丝强度偏低、无阻燃性能，并且各项性能不稳定，无法达到应用标准。
工业应用
本发明提供的聚酰胺56长丝一步连续成型与柔性变形制备工艺及设备，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，而且直接进行后加工制备的产品各项性能不稳定，因此，加入冷却牵伸工艺使喷丝板形成的丝束迅速冷却，分子链迅速堆积，结晶不完善，这样有利于后续高温下牵伸、定型得到性能稳定、质量优异的聚酰胺长丝。本专利流程短、能耗低、成本低、产品稳定、功能性强，可以根据不同需求制备不同种类聚酰胺长丝，为生物基聚酰胺以及聚酰胺类聚合物长丝的工业化一步纺提供指导。本发明制 备的聚酰胺56长丝可广泛应用于纺织业、汽车工业、家装、电子电器业、建筑业等领域。

Claims (10)

  1. 一种聚酰胺56长丝一步连续成型与柔性变形的制备方法，其特征在于：包括聚酰胺盐液聚合工艺、纺丝成型工艺、柔性后加工工艺：
    1)聚酰胺盐液聚合工艺：
    在氮气保护下，戊二胺和己二酸在水中进行中和成盐反应，得到聚酰胺56盐水溶液，聚酰胺56盐水溶液加入助剂调配混合后浓缩，浓缩后的盐液经过预聚合反应、前聚合反应、后聚合反应，得到聚酰胺56聚合物熔体；
    2)纺丝成型工艺：
    步骤1)制备得到的聚酰胺56聚合物熔体由螺杆挤压后，经喷丝板喷出得到熔体细流，熔体细流经过冷却吹风凝固成为丝条，丝条经过卷绕上油、冷热牵伸，热定型得到聚酰胺56丝束；
    3)柔性后加工工艺：
    所述柔性后加工是根据市场对产品的不同需求，制备不同风格的聚酰胺56长丝；
    当制备聚酰胺56全拉伸丝(FDY)，步骤2)中所述制备成型的聚酰胺56丝束需依次经过热牵伸、热定型、卷绕的后加工过程；
    当制备聚酰胺56拉伸变形丝(DTY)，则步骤2)中所述制备成型的聚酰胺56丝束需依次经过热牵伸、加捻、网络、热定型、上油、卷绕的后加工过程；
    当制备聚酰胺56空气变形丝(ATY)，则步骤2)中所述制备成型的聚酰胺56丝束需依次经过热牵伸、热喷射变形、冷却稳定、卷绕的后加工过程；
  2. 根据权利要求1所述的方法，其特征在于：所述步骤1)中，氮气保护为三冲三排；所述三冲即三次冲氮气；三排即排空气；
    所述戊二胺与己二酸的摩尔比为1～1.05：1；
    所述中和成盐反应温度为30～50℃；反应时间为30～60min；
    所述聚酰胺56盐水溶液的质量百分含量为20％～80％；
    所述助剂选自分子量调节剂、消光剂、阻燃剂、抗静电剂和抗菌剂中至少一种；
    所述助剂的加入量为所述戊二胺与己二酸质量之和的0.1％～6％；
    所述聚酰胺56聚合物熔体的粘度指数为120～160ml/g。
  3. 根据权利要求1或2所述的方法，其特征在于：所述步骤1)中，所述预聚反应的条件如下：温度210～240℃、压强1.7～1.85MPa，保压时间30min～180min；反应结束后快速闪蒸解压，并升温至270～290℃；
    所述前聚合反应的条件如下：温度270℃～290℃，反应时间20min～150min；
    所述后聚合反应的条件体系如下：温度270℃～290℃，真空度0.2～0.3MPa，反应时间10min～150min，排出体系中的水分。
  4. 根据权利要求1-3任一所述的方法，其特征在于：所述步骤2)纺丝成型步骤中，所用螺杆各区温度依次为：一区温度为260～300℃，二区温度为260～300℃，三区温度为250～295℃，四区温度为250～295℃，五区温度为250～290℃，六区温度为250～290℃；
    螺杆的转速为50～100r/min；
    纺丝箱体的温度为270～290℃；
    所述冷却吹风为侧吹风工艺或环吹风工艺；具体的，风速为0.30～0.80m/min；风温为18～25℃；风压为350～500Pa；
    所述上油步骤中，泵供量控制上油量为产品纤度的0.3％～0.5％；
    上述步骤中，纺丝速度为3000～5000m/min；
    所述牵伸步骤中，包括冷牵伸和热牵伸步骤；
    所述冷牵伸步骤中，冷牵伸倍率为1.01～1.50；温度为0～20℃；为一级牵伸；
    所述热牵伸步骤中，热牵伸倍率为3.00～5.50；温度为100～210℃；为一级牵伸、二级牵伸或多级牵伸；
    所述热定型步骤中，温度为130～200℃；定型时间为1～5min。
  5. 根据权利要求1-4任一所述的方法，其特征在于：所述步骤3)中，所述聚酰胺56长丝为全拉伸丝(FDY)时，工艺条件如下：所述牵伸为一级牵伸、二级牵伸或多级牵伸，温度为100～230℃，牵伸倍数为1.01～2.00，终极牵伸辊速度为500～1500m/min，热定型温度为150～200℃；卷绕速度为1000～1500m/min。
  6. 根据权利要求1-5任一所述的方法，其特征在于：所述步骤3)中，所述聚酰胺56长丝为拉伸变形丝(DTY)时，工艺条件如下：牵伸为一级牵伸、 二级牵伸或多级牵伸，温度为100～200℃，牵伸倍数为1.10～2.50，终极牵伸辊速度为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；所述网络步骤中，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。
  7. 根据权利要求1-6任一所述的方法，其特征在于：所述步骤3)中，所述聚酰胺56长丝为空气变形丝(ATY)时，工艺条件如下：牵伸为一级牵伸、二级牵伸或多级牵伸，温度为100～190℃，牵伸倍数为1.01～2.00，终极牵伸辊速度为1500～2500m/min；热喷射变形空气温度190～230℃，空气喷射压力195～550kPa，超喂率15～30％，冷却空气温度15～30℃，所述卷绕速度为1500～2800m/min。
  8. 权利要求1-7任一所述方法制备得到的聚酰胺56长丝。
  9. 根据权利要求8所述的聚酰胺56长丝，其特征在于：所述聚酰胺56长丝的线密度为1～7dtex；断裂强度为3～12cN/dtex，具有阻燃性，极限氧指数≥32％。
  10. 一种用于权利要求1-7任一所述制备聚酰胺56长丝方法的设备，包括：聚合反应装置、纺丝成型装置和柔性后加工装置三个单元组成，其中聚合反应装置与纺丝成型装置相连，直接制备聚酰胺56超高速长丝；再根据市场对产品的不同需求，连接柔性后加工装置，从而制备不同风格的聚酰胺56长丝；
    所述聚合反应装置由依次连接的原料釜、成盐釜、盐液储罐、盐液调配罐、盐液中间罐、浓缩槽、U型反应器、闪蒸器、前聚合器和后聚合器组成；
    所述原料釜为两个，分别为戊二胺原料釜和己二酸原料釜；
    所述纺丝成型装置由带喷丝板的纺丝箱体、纺丝箱体产出的熔体细流流经的纺丝甬道、对所述熔体细流进行吹风的吹风装置和在所述吹风后对所述熔体细流进行集束上油的装置和冷热牵伸装置组成；
    所述柔性后加工装置包括全拉伸丝(FDY)制备装置、拉伸变形丝(DTY)制备装置，空气变形丝(ATY)制备装置等，具体为如下a～c中任意一种：
    所述柔性后加工装置a由依次连接的牵伸辊、定型装置和卷绕装置组成，用于制备全拉伸丝工艺装置；
    所述柔性后加工装置b由依次连接的牵伸辊、假捻装置、网络装置、定 型装置、上油装置和卷绕装置组成，用于制备拉伸变形丝工艺装置；
    所述柔性后加工装置c由依次连接的牵伸辊、冷却装置、喷射变形装置、卷绕装置组成，用于制备空气变形丝工艺装置。
    所述柔性后加工中，定型装置为热板或热箱。
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