CN114293278B - Polyamide 5X fully drawn yarn and preparation method and application thereof - Google Patents

Polyamide 5X fully drawn yarn and preparation method and application thereof Download PDF

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Publication number
CN114293278B
CN114293278B CN202011000012.6A CN202011000012A CN114293278B CN 114293278 B CN114293278 B CN 114293278B CN 202011000012 A CN202011000012 A CN 202011000012A CN 114293278 B CN114293278 B CN 114293278B
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polyamide
pair
temperature
drawn yarn
fully drawn
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CN114293278A (en
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孙朝续
陈万钟
刘修才
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Cathay Wusu Biomaterial Co ltd
Shanxi Institute Of Synthetic Biology Co ltd
Cathay R&D Center Co Ltd
Cathay Jinxiang Biomaterial Co Ltd
CIBT America Inc
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Cathay Wusu Biomaterial Co ltd
Shanxi Institute Of Synthetic Biology Co ltd
Cathay R&D Center Co Ltd
Cathay Jinxiang Biomaterial Co Ltd
CIBT America Inc
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Abstract

The invention provides a polyamide 5X fully drawn yarn, a preparation method and application thereof, wherein the monofilament dpf of the polyamide 5X fully drawn yarn is less than or equal to 4, the breaking strength is 5.5-8.5 cN/dtex, the boiling water shrinkage is less than or equal to 10%, the elongation at break is less than or equal to 50%, and the initial modulus is 15-40 cN/dtex. The polyamide 5X fully drawn yarn has the characteristics of fine denier, high strength and low shrinkage, and has excellent softness and dyeing property, so that the polyamide 5X fully drawn yarn can be widely applied to the field of knitting and tatting fabrics.

Description

Polyamide 5X fully drawn yarn and preparation method and application thereof
Technical Field
The invention relates to polyamide 5X, in particular to a polyamide 5X fully drawn yarn and a preparation method and application thereof.
Background
Polyamide fibers are one of the earliest synthetic fibers put into industrial production in the world, and play a significant role in the field of synthetic fibers. The polyamide fibers are various in types, and the most widely used polyamide 6 and polyamide 66 are mainly used in industrial production at present. The main application relates to: socks, lace underwear, corset, athletic underwear, wedding dress, leisure jacket, sportswear, coat, jacket, quick-drying clothes, cold protective clothing, outdoor tent, sleeping bag, mountain climbing bag and other fields; industrial yarns are widely used in such fields as cords, belts, hoses, ropes, fishing nets, tires, parachutes, etc.
The raw materials for producing the polyamide 56 fiber are prepared from biological materials, are green materials, do not depend on petroleum resources, do not cause serious pollution to the environment, can reduce the emission of carbon dioxide and reduce the generation of greenhouse effect. The polyamide 56 fiber has the advantages of high strength, low-temperature dyeing property, hygroscopicity, softness, wear resistance, high elasticity and the like, and has wide development prospect in the fields of household wires and industrial wires.
The mechanical properties of the polyamide civil filaments are slightly lower, the breaking strength is generally smaller than 4.0cN/dtex, the processing requirements of a high-speed warp knitting machine are not met more and more, the situation of filament breakage in the weaving process can be caused, the tensile mechanical properties and the wear resistance of the prepared fabric are lower, and the fuzzing and pilling phenomena are easy to occur.
Secondly, the polyamide fiber has large boiling water shrinkage rate, serious shrinkage in the dyeing process and easy occurrence of a dyeing phenomenon, especially in the cheese dyeing process, the shrinkage is large, and the yarns close to the bobbin are difficult to permeate and difficult to dye due to the large tension due to the different inner and outer tension of the yarns, so that the color difference phenomenon of inner and outer layer dyeing is caused. In addition, the tension is different after shrinkage in the cone yarn unwinding process, the unwinding is difficult, the yarn breakage is easy to cause, the processing difficulty is increased, and the production cost investment is large. And the shrinkage of boiling water is large, the fabric is easy to cause large shrinkage of breadth and difficult to control in the dyeing process, and particularly, after the subsequent fabric is made into clothing, if the shrinkage is large after hot water washing, the clothing shape retention is poor.
Disclosure of Invention
One embodiment of the invention provides a polyamide 5X fully drawn yarn, wherein the monofilament dpf is less than or equal to 4, more preferably less than or equal to 3, still more preferably less than or equal to 2, and still more preferably 0.5-2.
The fineness is less than or equal to 300dtex, further can be less than or equal to 200dtex, further can be less than or equal to 150dtex, further can be less than or equal to 100dtex, further can be 11dtex, 22dtex, 33dtex, 40dtex, 44dtex, 55dtex or 78dtex.
The invention also provides a preparation method of the polyamide 5X fully drawn yarn, which comprises the steps of carrying out drawing treatment on the primary yarn formed by the melt of the polyamide 5X to obtain the polyamide 5X fully drawn yarn;
the stretching treatment comprises two-stage drafting by using three pairs of hot rolls, wherein the speeds of the three pairs of hot rolls are respectively 300-5500 m/min. The three pairs of heated rolls include a first pair of heated rolls, a second pair of heated roll speeds, and a third pair of heated rolls. The speeds of the three pairs of hot rollers are respectively 500-3500 m/min, or 2800-4900 m/min.
The embodiment of the invention further provides an application of the polyamide 5X fully drawn yarn in knitting or tatting fabrics.
The polyamide 5X fully drawn yarn of one embodiment of the invention has the characteristics of fine denier, high strength and low shrinkage.
Detailed Description
Exemplary embodiments that embody features and advantages of the present invention will be described in detail in the following description. It will be understood that the invention is capable of various modifications in various embodiments, all without departing from the scope of the invention, and that the description is intended to be illustrative in nature and not to be limiting.
In one embodiment, polyamide 5X is prepared by polymerizing 1, 5-pentanediamine and a dicarboxylic acid, wherein X in 5X represents the number of carbon atoms of the dicarboxylic acid and x=4 to 18.
In one embodiment, the 1, 5-pentanediamine may be prepared from a bio-based feedstock by fermentation or enzymatic conversion.
In one embodiment, the dicarboxylic acid contains 4 to 18 carbon atoms, such as 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, or 17. The value of X in the polyamide 5X may be 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 or 18, depending on the number of carbon atoms of the dicarboxylic acid. Further, polyamide 56, polyamide 510, polyamide 512, polyamide 513, and the like are preferable.
In one embodiment, the dicarboxylic acid is a saturated or unsaturated linear aliphatic dicarboxylic acid.
In one embodiment, the dicarboxylic acid comprises one or more of succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecandioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanodioic acid, hexadecanedioic acid, heptadecanodioic acid, octadecanedioic acid, maleic acid, and Δ9-1, 18-octadecenedioic acid.
An embodiment of the invention provides a polyamide 5X fully drawn yarn, the fineness of which is less than or equal to 300dtex.
In one embodiment, the titer of the polyamide 5X fully drawn yarn may be 200dtex or less, further 150dtex or less, still further 100dtex or less, for example 20dtex, 22dtex, 44dtex, 45dtex, 55dtex, 60dtex, 70dtex, 75dtex, 78dtex, 80dtex, 90dtex, 120dtex, 150dtex, etc. And further may be 11dtex, 22dtex, 33dtex, 40dtex, 44dtex, 55dtex or 78dtex.
In one embodiment, the denier of the polyamide 5X fully drawn yarn may be 22 to 78dtex.
In one embodiment, the monofilament dpf of the polyamide 5X fully drawn yarn may be 4 or less, further may be 3 or less, still further may be 2 or less, still further may be 1 or less, such as 0.80, 0.86, 0.90, 1.15, 1.20, 1.50, 1.53, 1.55, 1.60, 1.63, 1.65, 2.00. The monofilament dpf is the denier per filament (dpf is an abbreviation of denier per filament).
In one embodiment, the monofilament dpf of the polyamide 5X fully drawn yarn may be 0.5 to 2, and further may be 0.8 to 2.
In one embodiment, the polyamide 5X fully drawn yarn has a tenacity at break of 5.5 to 8.5cN/dtex, further may be 5.8 to 8.3cN/dtex, still further may be 6.0 to 7.8cN/dtex, still further may be 6.3 to 7.5cN/dtex, such as 6.1cN/dtex, 6.2cN/dtex, 6.5cN/dtex, 6.8cN/dtex, 7.0cN/dtex, 7.2cN/dtex, 7.3cN/dtex, 7.5cN/dtex, 8.0cN/dtex.
In one embodiment, the boiling water shrinkage of the polyamide 5X fully drawn yarn may be 10% or less, more preferably 8% or less, still more preferably 7% or less, still more preferably 6% or less, such as 3.0%, 3.1%, 3.3%, 3.5%, 4.0%, 5.0%, 5.2%, 5.5%, 6.0%, 6.3%, 6.4%, 6.5%, 6.8%.
In one embodiment, the boiling water shrinkage of the polyamide 5X fully drawn yarn may be 3.0 to 7.0%.
In one embodiment, the elongation at break of the polyamide 5X fully drawn yarn may be 50% or less, more preferably 45% or less, still more preferably 40% or less, still more preferably 35% or less, such as 27.0%, 27.4%, 28.0%, 28.8%, 29.0%, 29.2%, 29.5%, 30.0%, 30.3%, 31.0%, 32.0%, 32.4%, 32.5%, 32.8%, 33.0%, 33.5%, 34.0%, 38.0%.
In one embodiment, the elongation at break of the polyamide 5X fully drawn yarn may be 27 to 34%.
In one embodiment, the polyamide 5X fully drawn yarn has an initial modulus of 15 to 40cN/dtex, further 18 to 35cN/dtex, still further 20 to 30cN/dtex, still further 23 to 28cN/dtex, e.g. 16cN/dtex, 16.1cN/dtex, 18cN/dtex, 18.2cN/dtex, 18.5cN/dtex, 19cN/dtex, 19.5cN/dtex, 20cN/dtex, 20.2cN/dtex, 20.5cN/dtex, 21cN/dtex, 22cN/dtex, 23.2cN/dtex, 23.5cN/dtex, 24cN/dtex, 25cN/dtex, 25.8cN/dtex, 26cN/dtex.
In one embodiment, the dyeing uniformity (gray card) of the polyamide 5X fully drawn yarn may be 3.5 or more, further 4.0 or more, still further 4.5 or more, and still further 5.0 or more.
In one embodiment, the polyamide 5X fully drawn yarn may have a degree of dyeing uniformity (gray card) of 4.5 to 5.0.
In one embodiment, the dyed double a ratio of the polyamide 5X fully drawn yarn may be greater than or equal to 92%, further may be greater than or equal to 94%, still further may be greater than or equal to 96%, still further may be greater than or equal to 98%, such as 97.0%, 97.2%, 97.5%, 97.8%, 98.0%, 98.2%, 98.4%, 98.5%, 99.0%.
In one embodiment, the dyed double a ratio of the polyamide 5X fully drawn yarn may be 97 to 99%.
In one embodiment, the polyamide 5X fully drawn yarn may have a yield of 94% or more, more preferably 95% or more, still more preferably 96% or more, still more preferably 98% or more, such as 97.0%, 98.0%, 98.5%, 98.6%, 98.7%, 98.8%, 98.9%, 99.0%, 99.2%, 99.3%, 99.5%.
In one embodiment, the polyamide 5X fully drawn yarn may have a yield of 98.5 to 99.5%, where the yield = (mass of finished fiber produced/mass of total resin input) ×100%.
In one embodiment, the polyamide 5X fully drawn yarn comprises an additive.
In one embodiment, the additive comprises 0.001 to 5% by mass, for example 0.005%, 0.01%, 0.05%, 0.1%, 0.2%, 0.5%, 1%, 2%, 2.5%, 3% by mass of the total mass of the polyamide 5X fully drawn yarn production stock.
In one embodiment, the additive includes any one or more of a matting agent, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a crystallization nucleating agent, a fluorescent whitening agent, and an antistatic agent.
The polyamide 5X fully drawn yarn of one embodiment of the invention has the characteristics of high strength, low shrinkage and good dyeing property.
The polyamide 5X fully drawn yarn of the embodiment of the invention has good softness and dyeing property, so that the polyamide 5X fully drawn yarn can be widely applied to the field of knitting and tatting fabrics.
An embodiment of the invention provides a preparation method of polyamide 5X fully drawn yarn, which can be used for preparing the polyamide 5X fully drawn yarn.
The embodiment of the invention provides a preparation method of polyamide 5X fully drawn yarn, which comprises the steps of carrying out drawing treatment on primary yarn formed by polyamide 5X melt to obtain the polyamide 5X fully drawn yarn, wherein the drawing treatment comprises two-stage drawing by using three pairs of hot rollers, and the speed of the hot rollers is 300-5500 m/min.
The preparation method of the polyamide 5X fully drawn yarn in one embodiment of the invention comprises the following steps:
(1) Providing a polyamide 5X melt;
(2) Spraying polyamide 5X melt through a spinneret plate of a spinning box body to form primary filaments;
(3) And (3) cooling, oiling, two-stage drafting, heat setting and winding forming are carried out on the primary yarn to obtain the polyamide 5X fully-drawn yarn.
In one embodiment, step (1) comprises: forming a polyamide 5X melt by polymerizing 1, 5-pentanediamine and a dicarboxylic acid; alternatively, the polyamide 5X melt is formed by heating the polyamide 5X resin to a molten state.
In one embodiment, the polymerization process of 1, 5-pentanediamine and dicarboxylic acid comprises the steps of:
(1-1) mixing 1, 5-pentanediamine, dicarboxylic acid and water under the condition of inert gas to prepare a polyamide 5X salt solution;
(1-2) heating the polyamide 5X salt solution, increasing the pressure in the reaction system to 0.3-2.5 MPa, exhausting, maintaining pressure, reducing the pressure in the reaction system to 0-0.2 MPa, vacuumizing to the vacuum degree of-0.01 to-0.08 MPa, wherein the pressure is gauge pressure, and obtaining the polyamide 5X melt.
In one embodiment, the inert gas of step (1-1) comprises one, two or three of nitrogen, argon or helium.
In one embodiment, the molar ratio of 1, 5-pentanediamine to dicarboxylic acid of step (1-1) is from (1 to 1.08): 1.
In one embodiment, the temperature of the reaction system at the end of the pressure maintaining in step (1-2) is 230 to 260 ℃, for example 235 ℃, 240 ℃, 245 ℃, 250 ℃, 255 ℃.
In one embodiment, the temperature of the reaction system after the completion of the depressurization in step (1-2) is 240 to 280℃such as 245℃250℃255℃260℃265℃270℃275℃278 ℃.
In one embodiment, the temperature after the evacuation of step (1-2) is 260 to 285 ℃, e.g., 270 ℃, 275 ℃, 280 ℃, 283 ℃.
In one embodiment, the polyamide 5X resin 96% sulfuric acid of step (1) has a relative viscosity of 2.4 to 3.0, further may be 2.5 to 2.9, still further may be 2.6 to 2.8, such as 2.45, 2.5, 2.6, 2.7, 2.8, 2.9, etc.; the water content of the polyamide 5X resin may be 200 to 1000ppm, more preferably 300 to 900ppm, still more preferably 400 to 800ppm, still more preferably 500 to 600ppm, for example 400ppm, 450ppm, 500ppm, 520ppm, 600ppm, 700ppm.
In one embodiment, the heating of the polyamide 5X resin to the molten state of step (1) is performed in a screw extruder, the screw being divided into five zones, wherein one zone may be heated at a temperature of 200-260 ℃, such as 220 ℃, 225 ℃, 240 ℃, 245 ℃, 250 ℃, 255 ℃, 260 ℃; the temperature of the second zone may be 230-280 ℃, such as 235 ℃, 240 ℃, 245 ℃, 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃; the temperature of the three zones may be 240 to 290 ℃, such as 245 ℃, 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃, 275 ℃, 280 ℃; the temperature of the four zones may be 240 to 300 ℃, such as 245 ℃, 250 ℃, 260 ℃, 270 ℃, 275 ℃, 280 ℃, 285 ℃, 290 ℃; the five zone temperature may be 250 to 290 ℃, such as 255 ℃, 260 ℃, 270 ℃, 280 ℃, 283 ℃, 285 ℃, 290 ℃.
In one embodiment, the temperature of the spinning beam of step (2) may be 250 to 295 ℃, further 255 to 290 ℃, still further 260 to 288 ℃, still further 265 to 285 ℃, such as 250 ℃, 255 ℃, 258 ℃, 260 ℃, 270 ℃, 280 ℃, 282 ℃, 284 ℃, 285 ℃, 286 ℃, 288 ℃, 290 ℃; the pressure of the spinning pack of the spinning beam may be 10 to 25MPa, more preferably 12 to 23MPa, still more preferably 14 to 20MPa, for example 13MPa, 15MPa, 16MPa, 17MPa, 19MPa, 20MPa.
In one embodiment, the cooling in step (3) is a side or circular air-cooling, and the air speed of the side or circular air-cooling may be 0.4-0.9 m/s, and further may be 0.5-0.8 m/s, such as 0.45m/s, 0.47m/s, 0.48m/s, 0.5m/s, 0.52m/s, 0.55m/s, 0.6m/s, 0.65m/s, 0.7m/s, 0.75m/s, 0.8m/s; the air temperature of the side air blower or the circular air blower can be 15-25 ℃, further can be 16-22 ℃, and still further can be 18-20 ℃, such as 19 ℃, 20 ℃ and 21 ℃; the humidity of the side air or the circular air may be 60 to 85%, and further may be 65 to 75%, for example 76%, 78%, 80%, 82%, 83%.
In one embodiment, the drawing of step (3) is: the primary yarn after oiling is fed into a first pair of hot rolls through a godet, first-stage drafting is carried out between the first pair of hot rolls and a second pair of hot rolls, and then second-stage drafting is carried out between the second pair of hot rolls and a third pair of hot rolls, and tension heat setting is preferably carried out.
In one embodiment, the first pair of hot rolls has a speed of 300-3500 m/min, the second pair of hot rolls has a speed of 1200-5000 m/min, and the third pair of hot rolls has a speed of 2000-5500 m/min.
In one embodiment, the speeds of the three pairs of hot rolls are 500-3500 m/min respectively.
In one embodiment, the speeds of the three pairs of hot rolls are 2800 to 4900m/min, respectively.
In one embodiment, the first pair of heated rolls may have a temperature of 50 to 100 ℃, further 55 to 90 ℃, still further 60 to 80 ℃, such as 65 ℃, 70 ℃, 75 ℃, 85 ℃, 95 ℃; the number of windings of the first pair of heat rollers may be 4 to 8, further may be 4 to 7, and still further may be 4 to 6, for example 5.
In one embodiment, the temperature of the second pair of heated rolls may be 130 to 180 ℃, further 140 to 170 ℃, still further 150 to 160 ℃, such as 135 ℃, 145 ℃, 155 ℃, 165 ℃; the number of windings of the second pair of heat rollers may be 5 to 10, further may be 5 to 8, and still further may be 5 to 7, for example 6.
In one embodiment, the temperature of the third pair of hot rolls may be 150 to 220 ℃, further 160 to 190 ℃, still further 170 to 180 ℃, such as 175 ℃ and 185 ℃; the number of windings of the third pair of hot rolls can be 4-10, more can be 5-7, still more can be 5-6.
In one embodiment, the speed of the first pair of hot rolls is 550-1700 m/min, and further may be 600-1600 m/min, such as 600m/min, 700m/min, 800m/min, 900m/min, 1500m/min; the speed of the second pair of hot rolls is 1500-2400 m/min, and further may be 1600-2300 m/min, such as 1700m/min, 1800m/min, 1900m/min, 2000m/min; the third pair of heat roller speed is 2300-3300 m/min, further 2400-3200 m/min, such as 2500m/min, 2700m/min, 2800m/min, 3000m/min.
In one embodiment, the speed of the first pair of hot rolls is 2900-3400 m/min, and further may be 2950-3300 m/min; for example 3000m/min, 3150m/min, 3200m/min; the speed of the second pair of heat rollers is 3600-4900 m/min, and can be 4000-4850 m/min, such as 3700m/min, 3800m/min, 4000m/min, 4500m/min, 4700m/min, 4750m/min, 4800m/min; the speed of the third pair of heat rollers is preferably 3750 to 4850m/min, and may further be 3800 to 4800m/min, for example 3800m/min, 4000m/min, 4500m/min, 4700m/min, 4750m/min, 4800m/min.
In an embodiment, when the speed of the third pair of hot rolls is less than or equal to 3300m/min, the winding speed of the winding forming is 2200-3200 m/min, more preferably 2300-3000 m/min, still more preferably 2350-2800 m/min, such as 2300m/min, 2350m/min, 2480m/min, 2500m/min, 2650m/min, 2750m/min, 2780m/min, 2800m/min.
In one embodiment, when the speed of the third pair of hot rolls is greater than or equal to 3300m/min, the winding speed of the winding forming is 3600 to 4950m/min, further may be 3650 to 4900m/min, and still further may be 3700 to 4850m/min, for example 3700m/min, 4700m/min, 4720m/min, 4730m/min.
According to the method, high-power drafting and high-temperature setting are achieved through two-stage drafting of three pairs of hot rolls, fine denier, high-strength and low-shrinkage polyamide 5X civil filaments can be prepared, and the problems of low strength and large boiling water shrinkage of fine denier polyamide 5X fibers are solved.
According to one embodiment of the invention, the fiber yield is improved through polyamide 5X resin quality optimization (such as adjusting the viscosity and the water content of the polyamide 5X resin), spinning process optimization and the like.
The embodiment of the invention provides an application of the polyamide 5X fully drawn yarn in knitting and tatting fabrics.
In one embodiment, the knitted fabric wicking height (30 min): the length direction is more than or equal to 150mm, and the width direction is more than 160mm; the fabric width shrinkage is less than 8%, and is preferably less than or equal to 4%; the washing color fastness of the fabric is more than 3.5 grade, and is more preferably more than or equal to 4 grade; the fabric has a light fastness of > 3.0 grade, and preferably more than or equal to 4 grade.
In one embodiment, the polyamide 5X fully drawn yarn may be used in the field of undergarments, shirts, business wear, yoga gowns, down jackets, jacket, socks, luggage, curtains, shoes, embroidery threads, brands, sofa cloths, elastic bands, combat uniform, wedding dress, leisure jackets, outdoor tents, tools, sportswear, sleeping bags, mountain climbing bags.
The polyamide 5X fully drawn yarn according to one embodiment of the present invention and its preparation are further described below with reference to specific examples. Wherein the relevant tests involved are as follows:
1) Denier, monofilament dpf: denier is measured according to GB/T14343, monofilament dpf = total denier per number of fibers in the multifilament.
2) Breaking strength, elongation, initial modulus: the determination of the breaking strength and the elongation can be referred to a GB/T14344-2008 chemical fiber tensile property test method; applying a pretension of 0.05+/-0.005 cN/dtex, holding a distance of 500mm and a stretching speed of 500mm/min; modulus = breaking elongation at 1% corresponding breaking strength x 100.
3) Shrinkage in boiling water: the pretension was 0.05.+ -. 0.005cN/dtex as measured in accordance with GB/6505.
4) Dyeing uniformity (gray card)/grade: the FZ/T50008 nylon filament dyeing uniformity test method is kept at 98 ℃ for 30min, and the dyeing uniformity is judged.
5) Water content: the measurement was carried out by a Karl Fischer water titration apparatus.
6) Resin relative viscosity of 96% sulfuric acid: concentrated sulfuric acid method by Ubbelohde viscometer: accurately weighing 0.25+/-0.0002 g of dried polyamide resin slice, and adding 50mL of concentrated sulfuric acid (96 wt%) for dissolution; measurement and recording of the flow-through time t of concentrated sulfuric acid in a constant temperature water bath at 25 DEG C 0 And polyamide sample solution flow-through time t. The viscosity number calculation formula: relative viscosity = t/t 0 The method comprises the steps of carrying out a first treatment on the surface of the t-time of solution flow; t is t 0 Solvent flow-through time.
7) Dyeing double a rate: dyeing double A rate= ((dyeing pickup uniformity is not less than 4.5 grade fiber weight)/total weight of all dyed fibers) ×100%.
8) The preparation rate is as follows: yield = (mass of finished fibers prepared/mass of total resin input) ×100%.
9) Fastness to washing: reference is made to standard ISO 105 c06 a1s. The color fastness to light is referred to the standard ISO 105B 02.
10 Fabric width shrinkage: shrinkage= (fabric width before dyeing-fabric width after dyeing)/fabric width before dyeing.
11 Wicking height): reference standard AATCC-197.
The raw materials 1, 5-pentanediamine, polyamide 56 resin, polyamide 510 resin, polyamide 512 resin used in the following examples were all purchased from Kaiser (Kingxiang) biological materials Co., ltd.
Example 1
(1) 1, 5-pentanediamine and adipic acid were polymerized to form a melt of polyamide 56 having a 96% sulfuric acid relative viscosity of 2.7. The specific process is as follows:
(1-1) uniformly mixing 1, 5-pentanediamine, adipic acid and water under the condition of nitrogen to prepare a polyamide salt solution; wherein, the mol ratio of the 1, 5-pentanediamine to the adipic acid is 1.05:1;
(1-2) heating a polyamide salt solution, increasing the pressure in a reaction system to 2.2MPa, exhausting, maintaining pressure, reducing the pressure in the reaction system to 0MPa, and vacuumizing to the vacuum degree of-0.05 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system is 250 ℃ at the end of pressure maintaining, 275 ℃ at the end of depressurization, and 280 ℃ after vacuumizing.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 285 ℃, and the pressure of the spinning component is 16MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain a fine denier high-strength low-shrinkage polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.5m/s, the wind temperature is 19 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 800m/min, the temperature is 65 ℃, and the winding number of turns is 4; the speed of the second pair of hot rollers is 1800m/min, the temperature is 150 ℃, and the winding number of turns is 6; the speed of the third pair of hot rollers is 2500m/min, the temperature is 180 ℃, and the winding number of turns is 5 turns;
the winding speed was 2480m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
And (3) preparing polyamide 56 fiber spun yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through the spinning process. The parameters of the prepared polyamide 56 fabric are shown in Table 2.
Example 2
(1) 1, 5-pentanediamine and adipic acid were polymerized to form a melt of polyamide 56 having a 96% sulfuric acid relative viscosity of 2.8. The specific process is as follows:
(1-1) uniformly mixing 1, 5-pentanediamine, adipic acid and water under the condition of nitrogen to prepare a polyamide salt solution; wherein, the mol ratio of the 1, 5-pentanediamine to the adipic acid is 1.08:1;
(1-2) heating a polyamide salt solution, increasing the pressure in a reaction system to 2.4MPa, exhausting, maintaining pressure, reducing the pressure in the reaction system to 0MPa, and vacuumizing to the vacuum degree of-0.04 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system is 255 ℃ at the end of pressure maintaining, 278 ℃ at the end of depressurization, and 283 ℃ after vacuumizing.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 280 ℃, and the pressure of the spinning component is 13MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain a fine denier high-strength low-shrinkage polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.52m/s, the wind temperature is 20 ℃, and the humidity is 76%;
The drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 3100m/min, the temperature is 65 ℃, and the winding number of turns is 4; the speed of the second pair of hot rollers is 4800m/min, the temperature is 160 ℃, and the winding number of turns is 5 turns; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the winding number of turns is 5;
the winding speed was 4700m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
And (3) preparing polyamide 56 fiber spun yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through the spinning process. The parameters of the prepared polyamide 56 fabric are shown in Table 2.
Example 3
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.6, and the water content is 520ppm; the screw was heated in five zones, the first zone temperature was 240 ℃, the second zone temperature was 250 ℃, the third zone temperature was 260 ℃, the fourth zone temperature was 270 ℃, and the fifth zone temperature was 280 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 282 ℃, and the pressure of the spinning component is 17MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.48m/s, the wind temperature is 18 ℃, and the humidity is 82%;
the drawing process is drawing, and specifically comprises the following steps: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 600m/min, the temperature is 70 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 1700m/min, the temperature is 145 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 2400m/min, the temperature is 190 ℃, and the winding number of turns is 6;
the winding speed was 2350m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Example 4
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.7, and the water content is 600ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 285 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 286 ℃, and the pressure of the spinning component is 14MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.47m/s, the wind temperature is 19 ℃, and the humidity is 78%;
the drafting process is two-stage drafting, and concretely comprises the following steps: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 900m/min, the temperature is 70 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 1800m/min, the temperature is 160 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 2800m/min, the temperature is 185 ℃, and the winding number of turns is 6;
the winding speed was 2750m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Example 5
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.9, and the water content is 400ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 260 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 290 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 285 ℃, and the pressure of the spinning component is 17MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.52m/s, the wind temperature is 21 ℃, and the humidity is 83%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 1500m/min, the temperature is 65 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 3500m/min, the temperature is 150 ℃, and the winding number of turns is 6; the speed of the third pair of hot rollers is 3800m/min, the temperature is 170 ℃, and the winding number of turns is 6;
the winding speed was 3700m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Example 6
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.8, and the water content is 500ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 285 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 284 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.55m/s, the wind temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 3000m/min, the temperature is 70 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 4800m/min, the temperature is 150 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the winding number of turns is 7;
the winding speed was 4730m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Example 7
(1) Heating the polyamide 510 resin to a molten state in a screw extruder to form a polyamide 510 melt; wherein, the relative viscosity of the polyamide 510 resin 96% sulfuric acid is 2.45, and the water content is 400ppm; the screw is divided into five zones for heating, wherein the temperature of the first zone is 220 ℃, the temperature of the second zone is 240 ℃, the temperature of the third zone is 250 ℃, the temperature of the fourth zone is 260 ℃, and the temperature of the fifth zone is 260 ℃.
(2) Spraying the melt of the polyamide 510 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 260 ℃, and the pressure of the spinning component is 15MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 510 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.5m/s, the wind temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 800m/min, the temperature is 55 ℃, and the winding number of turns is 4; the speed of the second pair of hot rollers is 1800m/min, the temperature is 140 ℃, and the winding number of turns is 8; the speed of the third pair of hot rollers is 2700m/min, the temperature is 160 ℃, and the winding number of turns is 5;
the speed of winding was 2650m/min.
The parameters of the resulting polyamide 510 fully drawn yarn are shown in Table 1.
Example 8
(1) Heating the polyamide 510 resin to a molten state in a screw extruder to form a polyamide 510 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 510 resin is 2.6, and the water content is 300ppm; the screw was heated in five zones, the first zone temperature was 225 ℃, the second zone temperature was 240 ℃, the third zone temperature was 255 ℃, the fourth zone temperature was 260 ℃, and the fifth zone temperature was 255 ℃.
(2) Spraying the melt of the polyamide 510 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 258 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 510 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.45m/s, the wind temperature is 18 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 3000m/min, the temperature is 50 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 4800m/min, the temperature is 145 ℃, and the winding number of turns is 6; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the winding number of turns is 7;
the winding speed was 4720m/min.
The parameters of the resulting polyamide 510 fully drawn yarn are shown in Table 1.
Example 9
(1) Heating the polyamide 512 resin to a molten state in a screw extruder to form a polyamide 512 melt; wherein, the relative viscosity of the polyamide 512 resin 96% sulfuric acid is 2.6, and the water content is 450ppm; the screw is divided into five zones for heating, wherein the temperature of the first zone is 220 ℃, the temperature of the second zone is 230 ℃, the temperature of the third zone is 240 ℃, the temperature of the fourth zone is 245 ℃, and the temperature of the fifth zone is 250 ℃.
(2) Spraying the melt of the polyamide 512 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 250 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 512 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.48m/s, the wind temperature is 22 ℃, and the humidity is 80%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 700m/min, the temperature is 50 ℃, and the winding number of turns is 4; the speed of the second pair of hot rollers is 1900m/min, the temperature is 135 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 2800m/min, the temperature is 180 ℃, and the winding number of turns is 5;
the winding speed was 2780m/min.
The parameters of the polyamide 512 fully drawn yarn produced are shown in table 1.
Example 10
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.8, and the water content is 500ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 285 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 284 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.55m/s, the wind temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 3000m/min, the temperature is 70 ℃, and the winding number of turns is 3; the speed of the second pair of hot rollers is 4800m/min, the temperature is 150 ℃, and the winding number of turns is 4; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the winding number of turns is 3; the winding speed was 4730m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Example 11
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.8, and the water content is 500ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 285 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 284 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.55m/s, the wind temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 3000m/min, the temperature is 40 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 4800m/min, the temperature is 100 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 4750m/min, the temperature is 130 ℃, and the winding number of turns is 7; the winding speed was 4730m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Comparative example 1
(1) 1, 5-pentanediamine and adipic acid were polymerized to form a melt of polyamide 56 having a 96% sulfuric acid relative viscosity of 2.8. The specific process is as follows:
(1-1) uniformly mixing 1, 5-pentanediamine, adipic acid and water under the condition of nitrogen to prepare a polyamide salt solution; wherein, the mol ratio of the 1, 5-pentanediamine to the adipic acid is 1.08:1;
(1-2) heating a polyamide salt solution, increasing the pressure in a reaction system to 2.4MPa, exhausting, maintaining pressure, reducing the pressure in the reaction system to 0MPa, and vacuumizing to the vacuum degree of-0.04 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system is 255 ℃ at the end of pressure maintaining, 278 ℃ at the end of depressurization, and 283 ℃ after vacuumizing.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 280 ℃, and the pressure of the spinning component is 13MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.52m/s, the wind temperature is 20 ℃, and the humidity is 76%;
the drafting is primary drafting, and concretely comprises the following steps: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, and carrying out primary drafting and tension heat setting between the first pair of hot rollers and a second pair of hot rollers;
The speed of the first pair of hot rollers is 3100m/min, the temperature is 65 ℃, and the winding number of turns is 4; the speed of the second pair of hot rollers is 4800m/min, the temperature is 160 ℃, and the winding number of turns is 5 turns;
the winding speed was 4700m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
And (3) preparing polyamide 56 fiber spun yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through the spinning process. The parameters of the prepared polyamide 56 fabric are shown in Table 2.
Comparative example 2
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.3, and the water content is 600ppm; the screw was heated in five zones, the first zone temperature was 245 ℃, the second zone temperature was 265 ℃, the third zone temperature was 275 ℃, the fourth zone temperature was 285 ℃, and the fifth zone temperature was 285 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 286 ℃, and the pressure of the spinning component is 14MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
The cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.47m/s, the wind temperature is 19 ℃, and the humidity is 78%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 900m/min, the temperature is 70 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 1800m/min, the temperature is 160 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 2800m/min, the temperature is 185 ℃, and the winding number of turns is 6; the winding speed was 2750m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
And (3) preparing polyamide 56 fiber spun yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through the spinning process. The parameters of the prepared polyamide 56 fabric are shown in Table 2.
Comparative example 3
(1) Heating the polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 56 resin is 2.6, and the water content is 1300ppm; the screw was heated in five zones, the first zone temperature was 240 ℃, the second zone temperature was 250 ℃, the third zone temperature was 260 ℃, the fourth zone temperature was 270 ℃, and the fifth zone temperature was 280 ℃.
(2) Spraying the melt of the polyamide 56 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 282 ℃, and the pressure of the spinning component is 17MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 56 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.48m/s, the wind temperature is 18 ℃, and the humidity is 82%;
the drafting is two-stage drafting, specifically: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, carrying out primary drafting between the first pair of hot rollers and a second pair of hot rollers, and then carrying out secondary drafting between the second pair of hot rollers and a third pair of hot rollers and carrying out tension heat setting;
the speed of the first pair of hot rollers is 600m/min, the temperature is 70 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 1700m/min, the temperature is 145 ℃, and the winding number of turns is 7; the speed of the third pair of hot rollers is 2400m/min, the temperature is 190 ℃, and the winding number of turns is 6; the winding speed was 2350m/min.
The parameters of the polyamide 56 fully drawn yarn produced are shown in Table 1.
Comparative example 4
(1) Heating the polyamide 510 resin to a molten state in a screw extruder to form a polyamide 510 melt; wherein the relative viscosity of 96% sulfuric acid of the polyamide 510 resin is 2.6, and the water content is 300ppm; the screw was heated in five zones, the first zone temperature was 225 ℃, the second zone temperature was 240 ℃, the third zone temperature was 255 ℃, the fourth zone temperature was 260 ℃, and the fifth zone temperature was 255 ℃.
(2) Spraying the melt of the polyamide 510 obtained in the step (1) through a spinneret plate of a spinning box body to form primary filaments; wherein the temperature of the spinning box body is 258 ℃, and the pressure of the spinning component is 12MPa.
(3) Cooling, oiling, drafting, heat setting and winding the nascent yarn obtained in the step (2) to obtain polyamide 510 fully-drawn yarn;
the cooling in the step (3) is to cool side blowing air, wherein the wind speed of the side blowing air is 0.45m/s, the wind temperature is 18 ℃, and the humidity is 75%;
the drafting is primary drafting, and concretely comprises the following steps: feeding the primary yarn after oiling into a first pair of hot rollers through a godet, and carrying out primary drafting and tension heat setting between the first pair of hot rollers and a second pair of hot rollers;
the speed of the first pair of hot rollers is 2800m/min, the temperature is 50 ℃, and the winding number of turns is 5 turns; the speed of the second pair of hot rollers is 4200m/min, the temperature is 145 ℃, and the winding number of turns is 6;
the winding speed was 4720m/min.
The parameters of the resulting polyamide 510 fully drawn yarn are shown in Table 1.
Table 1 parameters of polyamide 5X fully drawn yarn prepared in examples and comparative examples
As can be seen from Table 1, the three pairs of hot rolls are adopted for two-stage drafting, parameters such as speed, temperature and the like of the hot rolls are controlled, high-power drafting and high-temperature heat setting are realized, the fine denier, high-strength and low-shrinkage polyamide 5X civil filaments are prepared, the problems of low strength and large boiling water shrinkage of the fine denier polyamide 5X fibers are solved, and meanwhile, the fiber yield is improved through the optimization of a spinning process.
Table 2 parameters of polyamide 5X fabric prepared in examples and comparative examples
As can be seen from Table 2, the color fastness of the application example 1 and the application example 2 is higher than that of the application example 1 and the application example 2, and the higher color fastness can lead the fabric product to touch rainwater and sweat or not easily cause pigment on the fabric to fall off and fade when being exposed to light in the wearing process. The low shrinkage of the fabric width indicates that the shrinkage degree of the fabric after high-temperature dyeing is small, and the production cost is greatly reduced. The high wicking height in the length and width directions indicates that the fabric product has excellent moisture absorption and sweat release functions, and is particularly suitable for applications such as underwear, shirts, western-style clothes, yoga jackets, down jackets, jacket-coats, socks and the like.
Unless otherwise defined, all terms used herein are intended to have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are intended to be illustrative only and not to limit the scope of the invention, and various other alternatives, modifications, and improvements may be made by those skilled in the art within the scope of the invention, and therefore the invention is not limited to the above embodiments but only by the claims.

Claims (41)

1. A polyamide 5X fully drawn yarn for knitting or tatting fabric has a monofilament dpf of less than or equal to 4;
The fineness is 22-78dtex;
the breaking elongation is 27-34%;
the initial modulus is 15-40 cN/dtex;
the dyeing uniformity (gray card) is more than or equal to 3.5 grade;
the dyeing double A rate is more than or equal to 94%;
the preparation rate is more than or equal to 94%;
the preparation method of the polyamide 5X fully drawn yarn comprises the steps of carrying out stretching treatment on a nascent yarn formed by a polyamide 5X melt to obtain the polyamide 5X fully drawn yarn;
the stretching treatment comprises two-stage drafting by using three pairs of hot rolls;
the speed of the first pair of hot rollers is 2900-3400 m/min, the speed of the second pair of hot rollers is 3600-4900 m/min, and the speed of the third pair of hot rollers is 3750-4850 m/min;
the temperature of the first pair of hot rollers is 50-70 ℃; the winding number of the first pair of hot rollers is 4-6;
the temperature of the second pair of hot rollers is 135-180 ℃; the winding number of the second pair of hot rolls is 6-8;
the temperature of the third pair of hot rollers is 160-190 ℃; the winding number of the third pair of hot rollers is 5-7.
2. The polyamide 5X fully drawn yarn of claim 1 wherein its monofilament dpf is 3 or less;
the initial modulus is 18-35 cN/dtex;
the dyeing uniformity (gray card) is more than or equal to 4.0 level;
the dyeing double A rate is more than or equal to 96 percent;
The preparation rate is more than or equal to 95 percent.
3. The polyamide 5X fully drawn yarn of claim 2 wherein its monofilament dpf is 2 or less;
the initial modulus is 20-30 cN/dtex;
the dyeing uniformity (gray card) is more than or equal to 4.5 grade;
the dyeing double A rate is more than or equal to 98 percent;
the preparation rate is more than or equal to 96 percent.
4. The polyamide 5X fully drawn yarn of claim 3 wherein the filaments have a dpf of from 0.5 to 2;
the initial modulus is 23-28 cN/dtex;
the dyeing uniformity (gray card) is more than or equal to 5.0 level;
the dyeing double A rate is more than or equal to 99 percent;
the preparation rate is more than or equal to 98 percent.
5. The polyamide 5X fully drawn yarn according to claim 1, wherein the breaking strength thereof is from 5.5 to 8.5cN/dtex.
6. The polyamide 5X fully drawn yarn of claim 5 having a tenacity at break of from 5.8 to 8.3cN/dtex.
7. The polyamide 5X fully drawn yarn according to claim 6, wherein the breaking strength thereof is from 6.0 to 7.8cN/dtex.
8. The polyamide 5X fully drawn yarn of claim 7 having a tenacity at break of 6.3 to 7.5cN/dtex.
9. The polyamide 5X fully drawn yarn of claim 1 wherein the boiling water shrinkage is 10% or less.
10. The polyamide 5X fully drawn yarn of claim 9 wherein the boiling water shrinkage is 8% or less.
11. The polyamide 5X fully drawn yarn of claim 10 having a boiling water shrinkage of 7% or less.
12. The polyamide 5X fully drawn yarn of claim 11 wherein the boiling water shrinkage is 6% or less.
13. The polyamide 5X fully drawn yarn of claim 1 wherein the polyamide 5X is prepared from polymerization of 1, 5-pentanediamine and dicarboxylic acid; the dicarboxylic acid is saturated or unsaturated linear aliphatic dicarboxylic acid and contains 4-18 carbon atoms.
14. The polyamide 5X fully drawn yarn of claim 13, wherein the dicarboxylic acid comprises one or more of succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanoic acid, hexadecanedioic acid, heptadecanoic acid, octadecanedioic acid, maleic acid, and Δ9-1, 18-octadecenoic acid.
15. The polyamide 5X fully drawn yarn of claim 1 comprising an additive comprising any one or more of a matting agent, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a crystallization nucleating agent, a fluorescent whitening agent, and an antistatic agent; and/or the number of the groups of groups,
The mass of the additive accounts for 0.001-5% of the total mass of the polyamide 5X fully drawn yarn production raw material.
16. A preparation method of polyamide 5X fully drawn yarn comprises the steps of carrying out stretching treatment on primary yarn formed by polyamide 5X melt to obtain polyamide 5X fully drawn yarn;
the stretching treatment comprises two-stage drafting by using three pairs of hot rolls, wherein the speed of the first pair of hot rolls is 2900-3400 m/min, the speed of the second pair of hot rolls is 3600-4900 m/min, and the speed of the third pair of hot rolls is 3750-4850 m/min.
17. The method of claim 16, the stretching process comprising sequentially cooling, oiling, the two-stage drawing, heat setting, and coil forming.
18. The method of claim 16, comprising polymerizing 1, 5-pentanediamine and dicarboxylic acid to form the polyamide 5X melt.
19. The method of claim 16, comprising heating a polyamide 5X resin to a molten state to form the polyamide 5X melt.
20. The process of claim 19 wherein the polyamide 5X resin is heated to a molten state in a screw extruder divided into five zones, heated at a first zone temperature of 200 to 260 ℃, a second zone temperature of 230 to 280 ℃, a third zone temperature of 240 to 290 ℃, a fourth zone temperature of 240 to 300 ℃, and a fifth zone temperature of 250 to 290 ℃.
21. The method of claim 19, wherein the polyamide 5X resin has a relative viscosity of 2.4 to 3.0 with 96% sulfuric acid; the water content is 200-1000 ppm.
22. The method of claim 21, wherein the polyamide 5X resin has a relative viscosity of 2.5 to 2.9 with 96% sulfuric acid; the water content is 300-900 ppm.
23. The method of claim 22, wherein the polyamide 5X resin has a relative viscosity of 2.6-2.8 with 96% sulfuric acid; the water content is 400-800 ppm.
24. The method of claim 23, wherein the polyamide 5X resin has a water content of 96% sulfuric acid of 500 to 600ppm.
25. The method of claim 16, wherein the polyamide 5X melt is ejected through a spinneret of a spinning beam to form the nascent filaments; the temperature of the spinning box body is 250-295 ℃; the pressure of the spinning component of the spinning box body is 10-25 MPa.
26. The method of claim 25, wherein the temperature of the spinning beam is 255-290 ℃; the pressure of the spinning component of the spinning box body is 12-23 MPa.
27. The method of claim 26, wherein the temperature of the spin beam is 260-288 ℃; the pressure of the spinning component of the spinning box body is 14-20 Mpa.
28. The method of claim 27, wherein the spinning beam has a temperature of 265 to 285 ℃.
29. The method of claim 18, comprising: mixing 1, 5-pentanediamine, dicarboxylic acid and water to prepare a polyamide 5X salt solution; and
heating the polyamide 5X salt solution, increasing the pressure in the system to 0.3-2.5 MPa, exhausting, maintaining pressure, reducing the pressure in the system to 0-0.2 MPa, and vacuumizing to the vacuum degree of-0.01-0.08 MPa to obtain a polyamide 5X melt; the pressure is gauge pressure;
wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.08): 1;
the temperature of the system is 230-260 ℃ when the pressure maintaining is finished;
the temperature of the system after the depressurization is finished is 240-280 ℃;
the temperature of the system after vacuumizing is 260-285 ℃.
30. The method of claim 16, wherein the two-stage drawing comprises feeding the raw filament first through a godet into the first pair of heated rolls, one-stage drawing between the first pair of heated rolls and the second pair of heated rolls, and then two-stage drawing between the second pair of heated rolls and the third pair of heated rolls.
31. The method of claim 30, wherein the first pair of heated rolls has a speed of 2900-3400 m/min, the second pair of heated rolls has a speed of 3600-4900 m/min, and the third pair of heated rolls has a speed of 3750-4850 m/min;
The temperature of the first pair of hot rollers is 50-70 ℃; the winding number of the first pair of hot rollers is 4-6;
the temperature of the second pair of hot rollers is 135-180 ℃; the winding number of the second pair of hot rolls is 6-8;
the temperature of the third pair of hot rollers is 160-190 ℃; the winding number of the third pair of hot rollers is 5-7.
32. The method of claim 31, wherein the first pair of heated rolls has a speed of 2950 to 3300m/min, the second pair of heated rolls has a speed of 4000 to 4850m/min, and the third pair of heated rolls has a speed of 3800 to 4800m/min.
33. The method of claim 31, wherein the temperature of the second pair of heated rolls is 140-170 ℃;
the temperature of the third pair of hot rollers is 170-180 ℃, and the winding number of the third pair of hot rollers is 5-6.
34. The method of claim 33, wherein the temperature of the second pair of heated rolls is 150-160 ℃.
35. The method of claim 17, wherein the cooling is performed by air cooling with a side air blower or a circular air blower, and the air speed of the side air blower or the circular air blower is 0.4-0.9 m/s; the air temperature of the side air blowing or the annular air blowing is 15-25 ℃; the humidity of the lateral air blowing or the circular air blowing is 60-85%.
36. The method of claim 35, wherein the air velocity of the side or ring air is 0.5-0.8 m/s; the air temperature of the side air blowing or the annular air blowing is 16-22 ℃; the humidity of the lateral air blowing or the circular air blowing is 65-75%.
37. The method of claim 36, wherein the cross-air or loop-air has an air temperature of 18-20 ℃.
38. Use of the polyamide 5X fully drawn yarn of any one of claims 1 to 15 or the polyamide 5X fully drawn yarn produced by the method of any one of claims 16 to 37 in a knitted or woven fabric.
39. Use according to claim 38, the knitted fabric wicking height (30 min): the length direction is more than or equal to 150mm, and the width direction is more than 160mm; the fabric width shrinkage rate is less than 8%; the washing color fastness of the fabric is more than 3.5 grades; the color fastness to sunlight of the fabric is more than 3.0 grade.
40. Use according to claim 39, said knitted fabric wicking height (30 min): the fabric width shrinkage rate is less than or equal to 4%; the washing color fastness of the fabric is more than or equal to level 4; the color fastness to sunlight of the fabric is more than or equal to level 4.
41. The use according to claim 40 of knitted and woven fabric for undergarments, shirts, western-style clothes, yoga clothes, down jackets, jacket, bags, curtains, shoes, embroidery threads, brands, sofa cloths, elastic bands, combat uniform, wedding dress, leisure jackets, outdoor tents, tools, sports wear, sleeping bags or mountain climbing bags.
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