WO2022048663A1 - 一种功能化聚酰胺56短纤维的制备方法 - Google Patents

一种功能化聚酰胺56短纤维的制备方法 Download PDF

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WO2022048663A1
WO2022048663A1 PCT/CN2021/116658 CN2021116658W WO2022048663A1 WO 2022048663 A1 WO2022048663 A1 WO 2022048663A1 CN 2021116658 W CN2021116658 W CN 2021116658W WO 2022048663 A1 WO2022048663 A1 WO 2022048663A1
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temperature
polyamide
drafting
box
ratio
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French (fr)
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郝新敏
郭亚飞
闫金龙
乔荣荣
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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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    • 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
    • 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
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • 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
    • D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D7/00—Collecting the newly-spun products
    • 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
    • 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

Definitions

  • the repeating units (monomers) of polyamide (PA) have amide groups as a characteristic feature. When the repeating units between amide bonds are substantially aliphatic, they form polymers known as polyamides.
  • Polyamide fiber is the second largest synthetic fiber after polyester fiber, due to its high strength, wear resistance, fatigue resistance, impact resistance, breathability and moisture absorption, light weight and softness, good dimensional stability, good drapability and good elasticity It has good market prospects in the fields of military products, rubber skeleton materials, ropes, nets, cables, tarpaulins, industrial filter cloths, as well as high-end sewing thread, T-shirt silk, umbrella fabrics, sports textiles and other fields.
  • the purpose of the present invention is to provide a preparation method of functionalized polyamide 56 short fibers.
  • a method for preparing a functionalized polyamide 56 staple fiber comprises the following steps:
  • step 2) Spinning molding: the polyamide 56 slices dried in vacuum in step 1) are melted in a spinning box, and the melt is sprayed with a thin stream of melt through the spinneret of the spinning box, and the melt is The thin stream is cooled and solidified by side air blowing and solidifies into a thread, and the thread is oiled, drawn, and tensioned and heat-set to form a drawn tow;
  • Fiber processing the drawn tow is bundled, folded, crimped, relaxed and heat-set, dried, cut, and packaged to obtain functionalized polyamide 56 short fibers.
  • the parameter of the polyamide 56 slice through described vacuum drying is as follows:
  • Viscosity index 130 ⁇ 180ml/g.
  • the viscosity index of the polyamide 56 slices is 130-140 ml/g
  • the prepared functionalized polyamide 56 short fibers are polyamide 56 flame-retardant short fibers;
  • the viscosity index of the polyamide 56 chips is 140-160 ml/g;
  • the viscosity index of the polyamide 56 slices is 160-180 ml/g;
  • the mass percentage content of water after drying of the slices 0.01-0.05%; the melting index is 23-24 g/10min; the melting point is 251-255° C.; the yellowing index is less than or equal to -1.
  • step 2) also includes adding an auxiliary agent through the auxiliary agent tank, mixing with the polyamide 56 chips for modification, and then performing melt spinning;
  • the added amount of the auxiliary agent is 0.2-2% of the mass of the polyamide 56 slices.
  • the conditions for forming the melt thin stream by blowing cooling are as follows: wind pressure: 400Pa ⁇ 440Pa; side blowing speed: 45 ⁇ 50m/min; wind temperature: 18 ⁇ 23°C;
  • the blowing cooling can be side blowing cooling or ring blowing cooling
  • the concentration of the oiling agent is 3% to 5%.
  • the drawing conditions are as follows: 25 ⁇ 35 °C normal temperature drawing, drafting ratio 1.01 ⁇ 1.05; 5 °C ⁇ 10 °C low temperature drawing, 1.01 ⁇ 1.05 drafting ratio; 60 ⁇ 190 °C hot drawing drawing, the drawing ratio is 1.01-5.0; the hot drawing can be one-stage drawing, two-stage drawing or multi-stage drawing.
  • the conditions of the thermal drawing may specifically be a first drawing ratio of 2.00 to 5.00, a second draw ratio of 1.01 to 1.30, and a first drawing roll temperature of 60 to 130 °C, the temperature of the steam drafting box is 120 ⁇ 170°C; the temperature of the second drafting roll is 150 ⁇ 170°C, the temperature of the hot plate drafting box is 170 ⁇ 190°C, and the temperature of the third drafting roll is 170 ⁇ 190°C.
  • the conditions of the thermal drawing are as follows: the first-drawing ratio is 2.78-3.00, the second-drawing ratio is 1.09-1.1, and the temperature of the first drawing roll is 75-75 85°C, the temperature of the steam drafting box is 155-165°C; the temperature of the second drafting roll is 165-175°C, the temperature of the hot plate drafting box is 180-190°C, and the temperature of the third drafting roll is 180-185°C.
  • the conditions of the thermal drawing are: a first-drawing ratio of 2.5-2.8, a second-drawing ratio of 1.1-1.2, and a first drawing roll temperature of 65- 75°C, steam drafting box temperature 120-130°C, second drafting roll temperature 150-160°C, hot plate drafting box temperature 180-185°C, third drafting roll temperature 175-180°C.
  • the conditions of the thermal drawing are as follows: the first drawing ratio is 2.1-2.50, the second-drawing ratio is 1.2-1.3, and the temperature of the first drawing roll is 80 ⁇ 2.50. 90°C, the temperature of the steam drafting box is 140-150°C; the temperature of the second drafting roll is 160-170°C, the temperature of the hot plate drafting box is 180-185°C, and the temperature of the third drafting roll is 180-185°C.
  • the conditions of the thermal drawing are as follows: the first drawing ratio is 3.5-5.00, the second-drawing ratio is 1.05-1.25, and the temperature of the first drawing roll is 120-130 °C, the temperature of the steam drafting box is 170-180°C; the temperature of the second drafting roller is 185-190°C, the temperature of the hot plate is 185-190°C, and the temperature of the third drafting roller is 185-190°C.
  • the heat setting is steam heat setting, hot plate setting, and water bath heat setting
  • the temperature of the heat setting is 150-190°C;
  • the crimping temperature is 60-90°C, and the number of crimps is 20-30;
  • the temperature of the relaxation heat setting is 95-190°C.
  • the present invention also provides the functional polyamide 56 short fibers prepared by the above method.
  • the specific performance parameters of the functional polyamide 56 staple fibers are as follows: the breaking strength is 3.5-4.9 cN/dtex, the breaking elongation is 20-60%, and the limiting oxygen index is 27-30%.
  • the breaking strength of the functionalized polyamide 56 cotton-type staple fiber is 4.9-5.50 CN/dtex, the breaking elongation is 40-60%, and the limiting oxygen index is 27-30%;
  • the breaking strength of the functionalized polyamide 56 wool-type short fibers is 4-5 CN/dtex, the breaking elongation is 60-70%, and the limiting oxygen index is 27-30%;
  • the breaking strength of the functionalized polyamide 56 flame-retardant short fiber is 3.5-6 cN/dtex, and the limiting oxygen index is 30-38%;
  • the breaking strength of the functionalized polyamide 56 high-strength staple fiber is 6-10 cN/dtex, and the limiting oxygen index is 30-35%.
  • Fig. 1 is the flow chart of the preparation method of polyamide 56 staple fiber of the present invention.
  • test method in the following examples is as follows:
  • DSC Differential scanning calorimeter
  • Embodiment 1 polyamide 56 conventional staple fiber
  • 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 6 hours, and continue to keep at 130 °C for 4 hours.
  • the slice viscosity index was 139ml/g; the mass percentage of water was 0.02%; the melt index was 23.3g/10min; the melting point was 252.3°C, and the yellowing index was -1.8.
  • Polyamide 56 polymer enters the spinning box for spinning, screw temperature: 282 °C in the first zone, 283 °C in the second zone, 283 °C in the third zone, 283 °C in the fourth zone, 280 °C in the fifth zone, loop temperature: 283 °C, box temperature 285°C, metering pump temperature 285°C, metering pump speed 15rpm/min, spinning assembly temperature 286°C, spinning speed 1500m/min, side blowing speed 45m/min; wind temperature 20°C, wind pressure 440Pa;
  • the filaments ejected from the spinneret were air-cooled and oiled with an oil concentration of 5% (winding oil was F5103, commercially available from Takemoto, Japan).
  • the fibers After shaping, the fibers are bundled, and then three pieces of filaments are stacked into one and then crimped.
  • the main crimping pressure is 2bar
  • the back pressure is 1bar
  • the crimping temperature is 60°C
  • the speed can be 300m/min
  • the number of crimps is 15, and then dried at 150°C.
  • Under-relaxation heat-setting, cutting, and baling, the conventional short fibers of polyamide 56 are obtained.
  • the vacuum drying process of polyamide 56 is the same as that of Example 1 of the present invention. After drying, the viscosity index of the slices is 134ml/g; the mass percentage of water is 0.02%; the melt index is 23.1g/10min; .
  • Screw temperature 282°C in the first zone, 282°C in the second zone, 282°C in the third zone, 282°C in the fourth zone, 282°C in the fifth zone, loop temperature: 282°C, box temperature 280°C, metering pump temperature 282°C, metering pump speed 13rpm
  • the spinning box the polyamide 56 polymer melt is distributed through pipelines and delivered to each spinneret with equal residence time and pressure drop; the spinning speed can be 1000m/min, the wind speed is 50m/min, and the 18°C, wind pressure 440Pa, oil concentration 5%; drafting and setting process: 30°C normal temperature drafting, drafting ratio 1.01. 5°C low temperature drafting, drafting ratio 1.01.
  • the first drafting ratio is 2.8; the second drafting ratio is 1.09; the temperature of the first drafting roll is 80 °C, the temperature of the steam drafting box is 160 °C; The stretching roll temperature is 180°C, and the hot plate setting temperature is 185°C.
  • Example 1 The subsequent steps are the same as those in Example 1. After shaping, the fibers are bundled, stacked, crimped, dried, tensioned, cut, and packaged to obtain cotton-type polyamide 56 staple fibers. The performance test results are shown in Table 1.
  • Embodiment 3 hair type staple fiber
  • the vacuum drying process of polyamide 56 is the same as that of Example 1 of the present invention. After drying, the viscosity index of the slices is 138ml/g; the mass percentage of water is 0.018%; the melt index is 23.2g/10min; .
  • the screw temperature is 285°C in the first zone, 285°C in the second zone, 285°C in the third zone, 285°C in the fourth zone, and 285°C in the fifth zone.
  • the polyamide 56 polymer melt is distributed through pipelines and delivered to each spinneret with equal residence time and pressure drop; the spinning speed can be 1200m/min, the wind speed is 0.50m/min, and the 21 °C, wind pressure 440Pa, oil concentration 5%; drafting and setting process: 30 °C normal temperature drafting, drafting ratio 1.01. 5 °C low temperature drafting, drafting ratio 1.01.
  • the first drafting ratio is 2.60; the second drafting ratio is 1.15; the temperature of the first drafting roll is 70°C, the temperature of the steam drafting box is 120°C; the temperature of the second drafting roll is 150°C; the temperature of the hot plate drafting box is 180°C, and the temperature of the third drafting box
  • the stretching roll temperature is 180°C, and the hot plate setting temperature is 180°C.
  • Example 1 The subsequent steps are the same as those in Example 1. After shaping, the fibers are bundled, folded, crimped, dried, relaxed and heat-set, cut, and packaged to obtain wool-type polyamide 56 staple fibers. The performance test results are shown in Table 1.
  • Vacuum drying process first dry at 60 °C for 10 hours, then heat up to 90 °C for 6 hours, then heat up to 115 °C for 6 hours, and finally dry at 135 °C for 5 hours.
  • the slice viscosity index is 148ml/g; the mass percentage of water is 0.02%; the melt index is 23.5g/10min; the melting point is 252.2°C, and the yellowing index is -1.4.
  • the screw temperature is 283°C in the first zone, 285°C in the second zone, 285°C in the third zone, 285°C in the fourth zone, and 285°C in the fifth zone.
  • the polyamide 56 polymer melt is distributed through pipelines and delivered to each spinneret with equal residence time and pressure drop; the spinning speed can be 4200m/min, the wind speed is 0.50m/min, The wind temperature is 21°C, the wind pressure is 440Pa, and the oil concentration is 5%; the drafting and setting process: 30°C normal temperature drafting, the drafting ratio is 1.01. 5°C low temperature drafting, the drafting ratio is 1.01.
  • the first drafting ratio is 2.20; the second drafting ratio is 1.25; the temperature of the first drafting roll is 80 °C, the temperature of the steam drafting box is 140 °C; the temperature of the second drafting roll is 160 °C; The roll temperature was 185°C, and the setting temperature was 190°C.
  • Example 1 The subsequent steps are the same as those in Example 1. After shaping, the fibers are bundled, folded, crimped, dried, relaxed and heat-set, cut, and packaged to obtain polyamide 56 flame-retardant staple fibers. The performance test results are shown in Table 1.
  • Vacuum drying process first dry at 60 °C for 12 hours, then heat up to 90 °C for 8 hours, then heat up to 120 °C for 6 hours, and finally dry at 140 °C for 4 hours.
  • the slice viscosity index was 164ml/g; the mass percentage of water was 0.02%; the melt index was 23.4g/10min; the melting point was 252.2°C, and the yellowing index was -1.4.
  • the screw temperature is 285°C in the first zone, 285°C in the second zone, 285°C in the third zone, 285°C in the fourth zone, and 285°C in the fifth zone.
  • the polyamide 56 polymer melt is distributed through pipelines and delivered to each spinneret with equal residence time and pressure drop; the spinning speed can be 3000m/min, the wind speed is 0.50m/min, and the 21 °C, wind pressure 440Pa, oil concentration 5%; drafting and setting process: 30 °C normal temperature drafting, drafting ratio 1.01. 5 °C low temperature drafting, drafting ratio 1.01.
  • the first drafting ratio of hot drawing is 3.86; the second drafting ratio is 1.20; the temperature of the first drafting roll is 120 °C, the temperature of the steam drafting box is 175 °C; the temperature of the second drafting roll is 185 °C; The stretching roll temperature is 190°C, and the setting temperature is 190°C.
  • Example 1 The subsequent steps are the same as those in Example 1. After shaping, the fibers are bundled, stacked, crimped, dried, relaxed and heat-set, cut, and packaged to obtain polyamide 56 high-strength staple fibers. The performance test results are shown in Table 1.
  • the viscosity index of the slices is 161.1ml/g; the water content is 0.08%; the melt index is 24.7g/10min; the melting point is 251.9°C, and the yellow index is -0.3. Meet the appearance requirements of industrial production slices.
  • Polyamide 56 staple fibers with excellent mechanical properties and flame retardant properties are prepared by changing process parameters.
  • polyamide 56 polymer chips should meet the following indicators: viscosity index: 130 ⁇ 180ml/g; moisture content after drying: 0.01 ⁇ 0.05%; melt index: 23 ⁇ 24g/10min; melting point: 251 ⁇ 255 °C; yellowing Index ⁇ -1.
  • the moisture in the polyamide 56 polymer chips when heated and melted, will cause large-scale degradation of the chips, resulting in a decrease in viscosity, which will seriously affect the quality of the finished product and cause defects such as brittle fibers and deepening color.
  • Removing the moisture in the slices can improve the crystallinity.
  • the crystallinity of the slices can be improved by drying and heating up.
  • the slices with good crystallinity can prevent the slices from softening and sticking prematurely when heated, and avoid affecting the subsequent melt extrusion process.
  • the drying process ensures that the water content in the slices is 0.01-0.05%, thereby preparing polyamide 56 fibers with excellent performance.

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Abstract

一种功能化聚酰胺56短纤维制备方法，包括如下步骤：1)将聚酰胺56切片进行真空干燥；2)纺丝成型：将真空干燥的聚酰胺56切片在纺丝箱中熔融，其熔体经纺丝箱的喷丝板喷出熔体细流，熔体细流经侧吹风冷却凝固成为丝条，丝条经上油、牵伸、紧张热定型形成牵伸丝束；3)纤维加工：牵伸丝束经集束、叠丝、卷曲、松弛热定型、烘干、切断、打包步骤，得到功能化聚酰胺56短纤维。该制备方法通过对原料聚酰胺56聚合物切片选取和处理以及纤维加工工艺参数的改变，能够根据不同需求及用途制备力学性能、阻燃性能优异的聚酰胺56短纤维。

Description

一种功能化聚酰胺56短纤维的制备方法 技术领域
本发明涉及一种功能化聚酰胺56短纤维制备方法，属于纤维材料领域。
背景技术
切片纺丝是将物料从加料口进到螺杆的螺槽中，由于螺杆的转动，把切片向前推进。切片吸收的热能一方面来源于加热装置供给的热能；另一方面来源于切片和切片、切片与螺杆及套筒的摩擦及液层之间的剪切作用，导致一部分机械能转化成热能，切片在前进过程中温度不断升高而逐渐熔化成熔体。熔化过程聚合物在温度、压力、粘度和形态等方面发生变化，由固态(玻璃态)转变为高弹态，随温度的进一步提高，出现塑性流动，成为粘流体(粘流态)。粘流态的聚合物经螺杆的推进和螺杆出口的阻力作用，以一定的压力向熔体管道输送，最终经喷丝口形成熔体细流，再经过后续加工过程形成纤维。
聚酰胺(PA)的重复单元(单体)具有酰胺基团作为特征性特征。当酰胺键之间的重复单元基本上是脂肪族时，它们形成被称为聚酰胺的聚合物。聚酰胺纤维是产量仅次于聚酯纤维的第二大合成纤维，由于其强度高、耐磨、耐疲劳、耐冲击、透气吸湿、轻质柔软、尺寸稳定性好、悬垂性好、弹性好等特点，在军工产品、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、T恤衫用丝、雨伞面料、运动纺织品等领域拥有良好的市场前景。
随着人们生活水平的日益提高，人们对聚酰胺需求越来越多，品质、性能要求也越来越高，为了适应市场需求，开发出一种高效快速，节能减排，性能良好的聚酰胺产品是非常必要的。
发明公开
本发明的目的是提供一种功能化聚酰胺56短纤维制备方法。
本发明提供的一种功能化聚酰胺56短纤维制备方法，包括如下步骤：
1)将聚酰胺56切片进行真空干燥；
2)纺丝成型：步骤1)中真空干燥的所述聚酰胺56切片在纺丝箱中熔融，其熔体经所述纺丝箱的喷丝板喷出熔体细流，所述熔体细流经侧吹风冷却凝固成为丝条，所述丝条经上油、牵伸、紧张热定型形成牵伸丝束；
3)纤维加工：所述牵伸丝束经集束，叠丝、卷曲、松弛热定型、烘干、切 断、打包步骤，即得到功能化聚酰胺56短纤维。
上述的方法中，所述真空干燥的过程如下：
先在50～60℃的条件下干燥8～12h，后升温至80～90℃的条件下干燥5～10h，再升温至100～120℃的条件下干燥5～8h，最后在120～140℃的条件下干燥3～5h。
上述的方法中，经所述真空干燥的聚酰胺56切片的参数如下：
粘度指数：130～180ml/g。
上述的方法中，当制备的所述功能化聚酰胺56短纤维为棉型或毛型的聚酰胺56短纤维时，所述聚酰胺56切片的粘度指数为130～140ml/g；
当制备的所述功能化聚酰胺56短纤维为聚酰胺56阻燃型短纤维；所述聚酰胺56切片的粘度指数为140～160ml/g；
当制备的所述功能化聚酰胺56短纤维为聚酰胺56高强型短纤维时，所述聚酰胺56切片的粘度指数160～180ml/g；
所述切片干燥后含水的质量百分含量：0.01～0.05％；熔融指数为23～24g/10min；熔点为251～255℃；变黄指数≦-1。
上述的方法中，步骤2)中还包括通过所述助剂槽加入助剂，与所述聚酰胺56切片混合进行改性，然后进行熔融纺丝；
所述助剂加入量为所述聚酰胺56切片质量的0.2～2％。
上述的方法中，在所述纺丝箱进行纺丝的条件如下：
螺杆各区温度：一区278～290℃，二区280～290℃，三区280～290℃，四区275～288℃，五区278～288℃，回路温度：280～290℃，箱体温度275～288℃，计量泵温度280～288℃，计量泵转速12rpm～16rpm在纺丝箱体内，所述聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速度为500m/min～4300m/min。
上述的方法中，所述熔体细流经吹风冷却成型的条件如下：风压：400Pa～440Pa；侧吹风速：45～50m/min；风温：18～23℃；
所述吹风冷却可为侧吹风冷却或环吹风冷却；
所述上油的油剂浓度3％～5％。
上述的方法中，所述牵伸的条件如下：25～35℃常温牵伸，牵伸倍率1.01～1.05；5℃～10℃低温牵伸，牵伸倍率1.01～1.05；60～190℃热牵伸，牵伸倍 率1.01～5.0；所述热牵伸可为一级牵伸、二级牵伸或多级牵伸。
上述的方法中，制备所述功能化聚酰胺56短纤维时，所述热牵伸的条件具体可为一牵倍率2.00～5.00，二牵倍率1.01～1.30，第一牵伸辊温度60～130℃，蒸汽牵伸箱温度120～170℃；第二牵伸辊温度150～170℃，热板牵伸箱温度170～190℃，第三牵伸辊温度170～190℃。
上述的方法中，制备所述功能化聚酰胺56棉型的短纤维时，所述热牵伸的条件为一牵倍率2.78～3.00，二牵倍率1.09～1.1，第一牵伸辊温度75～85℃，蒸汽牵伸箱温度155～165℃；第二牵伸辊温度165～175℃，热板牵伸箱温度180～190℃，第三牵伸辊温度180～185℃。
上述的方法中，制备所述功能化聚酰胺56毛型的短纤维时，所述热牵伸的条件为一牵倍率2.5～2.8，二牵倍率1.1～1.2，第一牵伸辊温度65～75℃，蒸汽牵伸箱温度120～130℃，第二牵伸辊温度150～160℃，热板牵伸箱温度180～185℃，第三牵伸辊温度175～180℃。
上述的方法中，制备所述功能化聚酰胺56阻燃型短纤维时，所述热牵伸的条件为一牵倍率2.1～2.50，二牵倍率1.2～1.3，第一牵伸辊温度80～90℃，蒸汽牵伸箱温度140～150℃；第二牵伸辊温度160～170℃，热板牵伸箱温度180～185℃，第三牵伸辊温度180～185℃。
上述的方法中，制备所述功能化聚酰胺56高强型短纤维时，所述热牵伸的条件为一牵倍率3.5～5.00，二牵倍率1.05～1.25，第一牵伸辊温度120～130℃，蒸汽牵伸箱温度170～180℃；第二牵伸辊温度185～190℃，热板温度185～190℃，第三牵伸辊温度185～190℃。
上述的方法中，所述热定型为蒸汽热定型、热板定型、水浴热定型；
所述热定型的温度为150～190℃；
所述卷曲温度为60～90℃，卷曲数20～30个；
所述松弛热定型的温度为95～190℃。
本发明还提供了上述的方法制备得到的功能性聚酰胺56短纤维；
进一步地，所述功能性聚酰胺56短纤维具体性能参数如下：断裂强度为3.5～4.9cN/dtex，断裂伸长率为20～60％，极限氧指数为27～30％。
进一步地，所述功能化聚酰胺56棉型的短纤维的断裂强度为4.9～5.50CN/dtex，断裂伸长率为40～60％，极限氧指数为27～30％；
所述功能化聚酰胺56毛型的短纤维的断裂强度为4～5CN/dtex，断裂伸长率为60～70％，极限氧指数为27～30％；
所述功能化聚酰胺56阻燃型短纤维的断裂强度为3.5～6cN/dtex，极限氧指数为30～38％；
所述功能化聚酰胺56高强型短纤维的断裂强度为6～10cN/dtex，极限氧指数为30～35％。
附图说明
图1为本发明聚酰胺56短纤维制备方法流程图。
实施发明的最佳方式
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。
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。
下述实施例中测试方法如下：
1.HG/T 3862塑料黄色指数试验方法，检测时加入黑色底
2.GB/T 14336化学纤维短纤维长度试验方法
3.GB/T 14337化学纤维短纤维拉伸性能试验方法
4.GB/T 6503化学纤维回潮率试验方法
5.GB/T5454-1997纺织品燃烧性能试验氧指数法；
6.差示扫描量热仪(DSC)测试纤维的熔点、结晶度；
实施例1、聚酰胺56常规短纤维
按照本发明图1中本发明聚酰胺56短纤维制备方法流程进行制备，具体步骤如下：
1)将原料釜中聚酰胺56切片经干燥装置进行真空干燥；
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6h，继续在130℃的条件下保温4h。
干燥后切片粘度指数139ml/g；含水的质量百分含量为0.02％；熔融指数为23.3g/10min；熔点252.3℃，变黄指数-1.8。
2)纺丝成型：
聚酰胺56聚合物进入纺丝箱进行纺丝，螺杆温度：一区282℃，二区283℃，三区283℃，四区283℃，五区280℃，回路温度：283℃，箱体温度285℃，计量泵温度285℃，计量泵转速15rpm/min，纺丝组件温度为286℃，纺丝速率1500m/min，侧吹风速为45m/min；风温为20℃，风压为440Pa；喷丝板喷出的丝条吹风冷却后上油，油剂浓度5％(卷绕油剂为F5103，商购于日本竹本)；上油后纤维进行30℃常温牵伸，牵伸倍率1.01。5℃低温牵伸，牵伸倍率1.01。二级热牵伸，一牵倍率3.05；二牵倍率1.05；第一牵伸辊温度70℃；蒸汽牵伸箱温度120℃；第二牵伸辊温度160℃；热板牵伸箱温度165℃；第三牵伸辊温度170℃；热板定型温度170℃。
3)纤维加工：
定型后纤维集束，再将三片丝叠成一片后进行卷曲，卷曲主压力2bar，背压力1bar，卷曲温度为60℃，速率可为300m/min，卷曲数15个，然后干燥、150℃条件下松弛热定型、切断、打包，即得到聚酰胺56常规短纤维。
实施例2、棉型短纤维
聚酰胺56真空干燥工艺同本发明实施例1相同，干燥后切片粘度指数134ml/g；含水的质量百分含为0.02％；熔融指数为23.1g/10min；熔点251.4℃，变黄指数-1.6。
改变纺丝、牵伸、定型工艺参数，制备棉型短纤维，具体如下：
螺杆温度：一区282℃，二区282℃，三区282℃，四区282℃，五区282℃，回路温度：282℃，箱体温度280℃，计量泵温度282℃，计量泵转速13rpm在纺丝箱体内，聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速率可为1000m/min，风速50m/min，风温18℃，风压440Pa，油剂浓度5％；牵伸定型工艺：30℃常温牵伸，牵伸倍率1.01。5℃低温牵伸，牵伸倍率1.01。热牵伸一牵倍率2.8；二牵倍率1.09；第一牵伸辊温度80℃，蒸汽牵伸箱温度160℃；第二牵伸辊温度170℃；热板牵伸箱温度180℃，第三牵伸辊温度180℃，热板定型温度185℃。
后续步骤与本实施例1中条件相同，定型后纤维集束、叠丝、卷曲、干燥、调节张力、切断、打包得到棉型聚酰胺56短纤维，性能测试结果如表1所示。
实施例3、毛型短纤维
聚酰胺56真空干燥工艺同本发明实施例1相同，干燥后切片粘度指数 138ml/g；含水的质量百分含为0.018％；熔融指数为23.2g/10min；熔点251.7℃，变黄指数-1.5。
改变纺丝、牵伸、定型工艺参数，制备毛型短纤维，具体如下：
螺杆温度一区285℃，二区285℃，三区285℃，四区285℃，五区285℃，回路温度：285℃，箱体温度285℃，计量泵温度285℃，计量泵转速15rpm在纺丝箱体内，聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速率可为1200m/min，风速0.50m/min，风温21℃，风压440Pa，油剂浓度5％；牵伸定型工艺：30℃常温牵伸，牵伸倍率1.01。5℃低温牵伸，牵伸倍率1.01。热牵伸一牵倍率2.60；二牵倍率1.15；第一牵伸辊温度70℃，蒸汽牵伸箱温度120℃；第二牵伸辊温度150℃；热板牵伸箱温度180℃，第三牵伸辊温度180℃，热板定型温度180℃。
后续步骤与本实施例1中条件相同，定型后纤维集束、叠丝、卷曲、干燥、松弛热定型、切断、打包得到毛型聚酰胺56短纤维，其性能测试结果如表1所示。
实施例4、阻燃型短纤维
真空干燥工艺：先在60℃的条件下干燥10h，后升温至90℃的条件下干燥6h，再升温至115℃的条件下干燥6h，最后在135℃的条件下干燥5h。干燥后切片粘度指数148ml/g；含水的质量百分含为0.02％；熔融指数为23.5g/10min；熔点252.2℃，变黄指数-1.4。
改变纺丝、牵伸、定型工艺参数，制备高强短纤维，具体如下：
螺杆温度一区283℃，二区285℃，三区285℃，四区285℃，五区285℃，回路温度：285℃，箱体温度283℃，计量泵温度285℃，计量泵转速15rpm在纺丝箱体内，所述聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速率可为4200m/min，风速0.50m/min，风温21℃，风压440Pa，油剂浓度5％；牵伸定型工艺：30℃常温牵伸，牵伸倍率1.01。5℃低温牵伸，牵伸倍率1.01。热牵伸一牵倍率2.20；二牵倍率1.25；第一牵伸辊温度80℃，蒸汽牵伸箱温度140℃；第二牵伸辊160℃；热板牵伸箱温度185℃，第三牵伸辊温度185℃，定型温度190℃。
后续步骤与本实施例1中条件相同，定型后纤维集束、叠丝、卷曲、干燥、松弛热定型、切断、打包得到聚酰胺56阻燃型短纤维，其性能测试结果如表1 所示。
实施例5、高强型短纤维
真空干燥工艺：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120℃的条件下干燥6h，最后在140℃的条件下干燥4h。干燥后切片粘度指数164ml/g；含水的质量百分含为0.02％；熔融指数为23.4g/10min；熔点252.2℃，变黄指数-1.4。
改变纺丝、牵伸、定型工艺参数，制备高强短纤维，具体如下：
螺杆温度一区285℃，二区285℃，三区285℃，四区285℃，五区285℃，回路温度：285℃，箱体温度283℃，计量泵温度285℃，计量泵转速15rpm在纺丝箱体内，聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速率可为3000m/min，风速0.50m/min，风温21℃，风压440Pa，油剂浓度5％；牵伸定型工艺：30℃常温牵伸，牵伸倍率1.01。5℃低温牵伸，牵伸倍率1.01。热牵伸一牵倍率3.86；二牵倍率1.20；第一牵伸辊温度120℃，蒸汽牵伸箱温度175℃；第二牵伸辊温度185℃；热板牵伸箱温度190℃，第三牵伸辊温度190℃，定型温度190℃。
后续步骤与本实施例1中条件相同，定型后纤维集束、叠丝、卷曲、干燥、松弛热定型、切断、打包得到聚酰胺56高强型短纤维，其性能测试结果如表1所示。
表1 1.5Dx38mm聚酰胺56短纤维测试数据
Figure PCTCN2021116658-appb-000001
对比例1、
改变真空干燥条件，在135℃条件下干燥25h。
干燥后切片粘度指数161.1ml/g；含水0.08％；熔融指数为24.7g/10min；熔点251.9℃，黄色指数-0.3，在高温下长时间干燥聚酰胺56切片，切片变黄现象严重，已不符合工业生产切片外观要求。
工业应用
1、通过工艺参数改变制备力学性能、阻燃性能优异的聚酰胺56短纤维。
2、优异性能聚酰胺56聚合物切片指标应满足：粘度指数：130～180ml/g；切片干燥后含水：0.01～0.05％；熔融指数为23～24g/10min；熔点251～255℃；变黄指数≦-1。
聚酰胺56聚合物切片中的水分，一方面在加热熔融时，会使切片发生大规模的降解，导致黏度下降，严重影响成品的质量，出现成品纤维变脆、色泽加深等缺陷；另一方面去除切片中水分可以提升结晶性，通过干燥升温提高切片的结晶性，结晶性好的切片可防止切片在受热时过早软化而黏结，避免对后续的熔融挤出过程产生影响，因此采用分段烘干工艺，确保切片中含水量在0.01～0.05％，从而制备优异性能的聚酰胺56纤维。

Claims (13)

  1. 一种功能化聚酰胺56短纤维制备方法，包括如下步骤：
    1)将聚酰胺56切片进行真空干燥；
    所述真空干燥的过程如下：
    先在50～60℃的条件下干燥8～12h，后升温至80～90℃的条件下干燥5～10h，再升温至100～120℃的条件下干燥5～8h，最后在120～140℃的条件下干燥3～5h；
    2)纺丝成型：步骤1)中真空干燥的所述聚酰胺56切片在纺丝箱中熔融，其熔体经所述纺丝箱的喷丝板喷出熔体细流，所述熔体细流经侧吹风冷却凝固成为丝条，所述丝条经上油、牵伸、紧张热定型形成牵伸丝束；
    3)纤维加工：所述牵伸丝束经集束，叠丝、卷曲、松弛热定型、烘干、切断、打包步骤，即得到功能化聚酰胺56短纤维。
  2. 根据权利要求1所述的方法，其特征在于：经所述真空干燥的聚酰胺56切片的参数如下：
    粘度指数：130～180ml/g；
    当制备的所述功能化聚酰胺56短纤维为棉型或毛型的聚酰胺56短纤维时，所述聚酰胺56切片的粘度指数为130～140ml/g；
    当制备的所述功能化聚酰胺56短纤维为聚酰胺56阻燃型短纤维；所述聚酰胺56切片的粘度指数为140～160ml/g；
    当制备的所述功能化聚酰胺56短纤维为聚酰胺56高强型短纤维时，所述聚酰胺56切片的粘度指数为160～180ml/g；
    所述切片干燥后含水的质量百分含量：0.01～0.05％；熔融指数为23～24g/10min；熔点为251～255℃；变黄指数≦-1。
  3. 根据权利要求1或2所述的方法，其特征在于：步骤2)中还包括通过所述助剂槽加入助剂，与所述聚酰胺56切片混合进行改性，然后进行熔融纺丝。
  4. 根据权利要求3所述的方法，其特征在于：所述助剂加入量为所述聚酰胺56切片质量的0.2～2％。
  5. 根据权利要求1或2所述的方法，其特征在于：在所述纺丝箱进行纺丝的条件如下：
    螺杆各区温度：一区278～290℃，二区280～290℃，三区280～290℃，四区275～288℃，五区278～288℃，回路温度：280～290℃，箱体温度275～288℃，计量 泵温度280～288℃，计量泵转速12rpm～16rpm在纺丝箱体内，所述聚酰胺56聚合物熔体通过管路分配，以相等的停留时间和压力降输送到每一个喷丝口；纺丝速度为500m/min～4300m/min。
  6. 根据权利要求1或2所述的方法，其特征在于：所述熔体细流经吹风冷却成型的条件如下：风压：400Pa～440Pa；侧吹风速：45～50m/min；风温：18～23℃；
    所述吹风冷却为侧吹风冷却或环吹风冷却；
    所述上油的油剂浓度3％～5％。
  7. 根据权利要求1或2所述的方法，其特征在于：所述牵伸的条件如下：25～35℃常温牵伸，牵伸倍率1.01～1.05；5℃～10℃低温牵伸，牵伸倍率1.01～1.05；60～190℃热牵伸，牵伸倍率1.01～5.0；所述热牵伸为一级牵伸、二级牵伸或多级牵伸。
  8. 根据权利要求7所述的方法，其特征在于：所述热牵伸的条件为一牵倍率2.00～5.00，二牵倍率1.01～1.30，第一牵伸辊温度60～130℃，蒸汽牵伸箱温度120～170℃；第二牵伸辊温度150～170℃，热板牵伸箱温度170～190℃，第三牵伸辊温度170～190℃。
  9. 根据权利要求7或8所述的方法，其特征在于：制备所述功能化聚酰胺56棉型的短纤维时，所述热牵伸的条件为一牵倍率2.78～3.00，二牵倍率1.09～1.1，第一牵伸辊温度75～85℃，蒸汽牵伸箱温度155～165℃；第二牵伸辊温度165～175℃，热板牵伸箱温度180～190℃，第三牵伸辊温度180～185℃；
    制备所述功能化聚酰胺56毛型的短纤维时，所述热牵伸的条件为一牵倍率2.5～2.8，二牵倍率1.1～1.2，第一牵伸辊温度65～75℃，蒸汽牵伸箱温度120～130℃，第二牵伸辊温度150-160℃，热板牵伸箱温度180-185℃，第三牵伸辊温度175-180℃；
    制备所述功能化聚酰胺56阻燃型短纤维时，所述热牵伸的条件为一牵倍率2.1～2.50，二牵倍率1.2～1.3，第一牵伸辊温度80～90℃，蒸汽牵伸箱温度140～150℃；第二牵伸辊温度160～170℃，热板牵伸箱温度180～185℃，第三牵伸辊温度180～185℃；
    制备所述功能化聚酰胺56高强型短纤维时，所述热牵伸的条件为一牵倍率3.5～5.00，二牵倍率1.05～1.25，第一牵伸辊温度120～130℃，蒸汽牵伸箱温度 170～180℃；第二牵伸辊温度185～190℃，热板温度185～190℃，第三牵伸辊温度185～190℃。
  10. 根据权利要求1或2所述的方法，其特征在于：所述热定型为蒸汽热定型、热板定型、水浴热定型；
    所述热定型的温度为150～190℃；
    所述卷曲温度为60～90℃，卷曲数20～30个；
    所述松弛热定型的温度为95～190℃。
  11. 权利要求1-10中任一项所述的方法制备得到的功能性聚酰胺56短纤维。
  12. 根据权利要求11所述功能性聚酰胺56短纤维，其特征在于：所述功能性聚酰胺56短纤维性能参数如下：断裂强度为3.5～4.9cN/dtex，断裂伸长率为20～60％，极限氧指数为27～30％。
  13. 根据权利要求11所述功能性聚酰胺56短纤维，其特征在于：所述功能化聚酰胺56棉型的短纤维的断裂强度为4.9～5.50CN/dtex，断裂伸长率为40～60％，极限氧指数为27～30％；所述功能化聚酰胺56毛型的短纤维的断裂强度为4～5CN/dtex，断裂伸长率为60～70％，极限氧指数为27～30％；所述功能化聚酰胺56阻燃型短纤维的断裂强度为3.5～6cN/dtex，极限氧指数为30～38％；所述功能化聚酰胺56高强型短纤维的断裂强度为6～10cN/dtex，极限氧指数为30～35％。
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