CN110616471B - Polyamide 5X medium-strength yarn and preparation method thereof - Google Patents

Polyamide 5X medium-strength yarn and preparation method thereof Download PDF

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CN110616471B
CN110616471B CN201910950609.8A CN201910950609A CN110616471B CN 110616471 B CN110616471 B CN 110616471B CN 201910950609 A CN201910950609 A CN 201910950609A CN 110616471 B CN110616471 B CN 110616471B
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polyamide
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temperature
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CN110616471A (en
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孙朝续
徐晓辰
秦兵兵
刘修才
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Cathay R&D Center Co Ltd
CIBT America Inc
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/28Preparatory processes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02Heat treatment
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/16Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Polyamides (AREA)

Abstract

The invention provides a polyamide 5X medium-strength yarn and a preparation method thereof, wherein the raw materials for producing the polyamide 5X medium-strength yarn at least comprise 1, 5-pentanediamine and dicarboxylic acid; or polyamide 5X obtained by polymerizing 1, 5-pentanediamine and dicarboxylic acid serving as monomers; the breaking strength of the polyamide 5X medium-strength filaments is 6.0-8.0cN/dtex. The preparation method comprises the following steps: (1) Polymerizing 1, 5-pentanediamine and dicarboxylic acid to form a polyamide 5X melt; alternatively, the polyamide 5X resin is heated to a molten state to form a polyamide 5X melt; (2) Spinning the polyamide 5X melt to form primary yarn; (3) And processing the primary raw silk to obtain the polyamide 5X medium-strength silk. The polyamide 5X medium-strength yarn has the characteristics of high strength, low elongation, low thermal shrinkage and the like; in addition, the wear-resistant and alkali-resistant composite material also has the advantages of good wear resistance, good alkali resistance, dimensional stability and the like, so that the material can be widely applied to the fields of sewing threads, safety belts, ropes, fishing nets, filter cloth and the like.

Description

Polyamide 5X medium-strength yarn and preparation method thereof
The application is a divisional application of an invention application of 'a polyamide 5X medium-strength yarn and a preparation method thereof', wherein the application date is 2017, 2, 24 and the application number is 201710102934. X.
Technical Field
The invention belongs to the technical field of polyamide materials, and relates to a polyamide 5X medium-strength yarn and a preparation method thereof.
Background
Medium strength yarn is a fiber having a breaking strength between that of civil yarn and that of low denier industrial yarn, and is used for the manufacture of fishing nets, industrial sewing threads, and the like. In the prior art, the strong yarn is generally produced by processing polyester serving as a raw material on spinning equipment of civil yarn. The orientation degree, crystallinity degree and breaking strength of the strong yarn in the polyester prepared by the method are low, and the dimensional stability is poor; and in the strand silk forming process, the stretching and setting temperature is low, the stretching multiplying power is small, and the method is difficult to be applied to the industrial field with higher requirements on the breaking strength and the dimensional stability.
Chinese patent CN 101205632A provides a process for producing medium-strength polyester filament by melt direct spinning, chinese patent CN 105369375A provides medium-strength yarn and a processing method, the medium-strength yarn materials reported in the 2 patents are all polyester, and the obtained polyester medium-strength yarn has not high mechanical property, but also poor wear resistance and alkali resistance. Therefore, a material having both good wear resistance and good alkali resistance is needed.
Polyamide 5X is a novel polyamide obtained by polymerizing 1, 5-pentanediamine and a dibasic acid, and has not only excellent mechanical properties but also special properties not possessed by conventional polyesters. Due to the special structure of the polyamide 5X, the spinning process can not be carried out by carrying out the existing polyester process, on the basis, various properties of the polyamide 5X are further adjusted, and particularly, on the basis of meeting various mechanical strengths, the requirements of the existing market on the wear resistance and alkali resistance of the fiber can be met, so that the polyamide 5X has very important significance and value.
Disclosure of Invention
The first purpose of the invention is to provide a polyamide 5X medium-strength yarn which has high strength, low elongation and low heat shrinkage performance, and is excellent in abrasion resistance and alkali resistance.
The second purpose of the invention is to provide a preparation method of the polyamide 5X medium-strength yarn.
In order to achieve the purpose, the solution of the invention is as follows:
the production raw materials of the polyamide 5X medium-strength yarn at least comprise 1, 5-pentanediamine and dicarboxylic acid; or,
polyamide 5X obtained by polymerizing 1, 5-pentanediamine and dicarboxylic acid serving as monomers.
The breaking strength of the filaments in polyamide 5X may be 6.0-8.0cN/dtex.
Preferably, the titer of the polyamide 5X medium-strength filaments can be 110 to 1100dtex, and can be preferably 220 to 990dtex, and can be further preferably 220 to 880dtex, and can be further preferably 220 to 550dtex.
Preferably, the breaking strength of the strong filaments in the polyamide 5X can be preferably 6.3-7.6cN/dtex, can be further preferably 6.5-7.2cN/dtex, and can be further preferably 6.7-7.0cN/dtex.
Preferably, the elongation at break of the filaments in the polyamide 5X may be 14 to 25%, and may be preferably 14 to 16%.
Preferably, the dry heat shrinkage of the strong yarn in the polyamide 5X may be 3.0 to 8.0%, may be preferably 3.5 to 7.5%, and may be further preferably 4.0 to 6.0%.
Preferably, the boiling water shrinkage of the filaments in the polyamide 5X may be 2.0 to 7.0%, may be preferably 3.0 to 6.0%, and may be more preferably 4.0 to 5.0%.
Preferably, the crystallinity of the strong yarn in the polyamide 5X may be 60 to 70%, may be preferably 61 to 69%, may be more preferably 62 to 68%, and may be more preferably 64 to 67%.
Preferably, the degree of orientation of the filaments in the polyamide 5X may be 70 to 80%, may be preferably 71 to 79%, may be further preferably 72 to 77%, and may be further preferably 73 to 76%.
Preferably, the 1, 5-pentanediamine is prepared from bio-based raw materials by a fermentation method or an enzymatic conversion method.
Preferably, the dicarboxylic acid has a carbon number of 4 to 18. 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, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid and Δ 9-1,18 octadecenedioic acid.
The raw material for producing the polyamide 5X medium-strength yarn can also comprise a comonomer.
The comonomers may include: any one or more of aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic dicarboxylic acid, ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, epsilon-caprolactam and omega-laurolactam.
The raw materials for producing the polyamide 5X medium-strength yarn can also comprise additives.
The additives may include: any one or more of a delustering agent, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a crystallization nucleating agent, a fluorescent brightener and an antistatic agent. The additive can be added in an amount of 0.001-10% of the total weight of the raw materials.
The preparation method of the polyamide 5X medium-strength yarn comprises the following steps:
(1) Polymerizing 1, 5-pentanediamine and dicarboxylic acid to form a polyamide 5X melt; or,
heating polyamide 5X (polyamide 5X resin) to a molten state to form a polyamide 5X melt;
(2) Spinning the polyamide 5X melt to form primary yarns;
(3) And treating the nascent fiber to obtain the polyamide 5X medium-strength fiber.
When the raw material for producing the filament in the polyamide 5X further comprises a comonomer, the comonomer is added in the step (1).
When the raw material for producing the filament in the polyamide 5X further comprises an additive, the additive is added in the step (1).
Preferably, in step (1), the polymerization comprises the steps of:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, dicarboxylic acid and water to prepare a salt solution of polyamide; wherein, the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.05): 1;
(1-2) heating the salt solution of the polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure, then reducing the pressure to 0-0.2Mpa, vacuumizing to-0.08-0.01 Mpa of vacuum degree, wherein the pressure is gauge pressure, and obtaining the polyamide 5X melt.
When the raw material for producing the filament in the polyamide 5X further includes a comonomer, the comonomer is added in the step (1-1).
When the raw material for producing the filament in the polyamide 5X further comprises an additive, the additive is added in the step (1-1).
Preferably, the temperature of the reaction system at the end of the dwell pressure is 232 to 265 ℃.
Preferably, the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
Preferably, the temperature after the vacuum pumping is 260-280 ℃.
In the step (1), the polyamide 5X resin is a polyamide 5X resin chip.
Preferably, the polyamide 5X resin may have a relative viscosity of 2.5 to 3.0, preferably 2.6 to 2.9, more preferably 2.7 to 2.8 in 96% sulfuric acid.
The polyamide 5X resin has a water content of 50 to 1500ppm, preferably 200 to 800ppm, more preferably 300 to 700ppm, and still more preferably 400 to 600ppm.
In the step (1), the heating is carried out in a screw extruder which is divided into five zones for heating.
Wherein, the temperature of the first zone is preferably 200-300 ℃; and/or the temperature of the second zone is 230-320 ℃; and/or, the temperature of the three zones is 240-350 ℃; and/or the temperature of the four zones is 270-360 ℃; and/or the temperature of the five zones is 270-400 ℃.
Preferably, the two-zone temperature is greater than the one-zone temperature.
Preferably, the three, four or five zone temperatures are greater than the one or two zone temperatures.
Preferably, when the raw material for producing the filament in the polyamide 5X further comprises an additive, the polyamide 5X is heated to a molten state to form a polyamide 5X melt, and then mixed with the additive.
Preferably, in the step (2), the spinning comprises the following steps:
and (3) spraying the polyamide 5X melt through a spinneret plate of a spinning manifold to form the primary yarn.
The temperature of the spinning beam may be 200 to 350 ℃, more preferably 210 to 330 ℃, even more preferably 220 to 310 ℃, and even more preferably 240 to 300 ℃.
Preferably, the pressure of the spin pack of the spinning beam may be 10 to 30MPa, may preferably be 15 to 25MPa, and may further preferably be 17 to 24MPa.
Preferably, the number of holes of the spinneret plate may be 48 to 576f, preferably 64 to 480f, more preferably 96 to 288f, and still more preferably 96 to 192f.
Preferably, the spinneret draw ratio of the spinneret may be in the range of 50 to 300, may preferably be in the range of 70 to 140, may further preferably be in the range of 80 to 110, and may further preferably be in the range of 90 to 100.
Preferably, in the step (3), the processing includes the steps of:
and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 5X medium-strength yarn.
Wherein the cooling is by cross-air blowing.
Preferably, the wind speed of the cross-blown air may be preferably 0.5 to 0.9m/s, and may be more preferably 0.6 to 0.8m/s.
Preferably, the air temperature of the cross-air blast may be preferably 15 to 32 ℃, may be more preferably 20 to 28 ℃, and may be further preferably 23 to 26 ℃.
Preferably, the humidity of the side blow may be 60 to 80%, and may be preferably 65 to 78%.
Preferably, the winding tension at the time of the winding formation may be 50 to 150cN, may be preferably 70 to 120cN, may be further preferably 75 to 110cN, and may be further preferably 80 to 100cN.
Preferably, the winding speed may be 2000 to 3500m/min, may preferably be 2200 to 3000m/min, and may further preferably be 2200 to 2800m/min.
Preferably, the stretching is two-stage or more stretching.
Preferably, the stretching process is: feeding the oiled nascent yarn into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting.
Preferably, the first stage drawing may have a drawing ratio of 3.0 to 4.5 and a drawing temperature of 60 to 180 ℃.
Preferably, the stretching ratio of the secondary stretching may be-1.0 to 2.0, and the stretching temperature may be 140 to 200 ℃.
Preferably, the total draw ratio is 3.0 to 9.0, preferably 4.0 to 6.0.
Preferably, the heat-setting temperature may be 180 to 240 ℃ and may preferably be 200 to 230 ℃.
Preferably, the speed of the godet rolls may be from 200 to 800m/min, and may preferably be from 400 to 600m/min.
Preferably, the speed of the first hot roll pair may be 300 to 900m/min, and may preferably be 500 to 700m/min.
Preferably, the speed of the second pair of thermo rolls may be 1500 to 2200m/min, and may preferably be 1600 to 2000m/min.
Preferably, the speed of the third pair of thermo rolls may be 2200 to 3000m/min, and may preferably be 2200 to 2800m/min.
Preferably, the number of turns of the polyamide 5X fiber of the first thermo roll may be 4 to 8, and may preferably be 5 to 7.
Preferably, the number of windings of the polyamide 5X fibers of the second pair of heated rolls can be from 6 to 12, and can preferably be from 7 to 10.
Preferably, the number of turns of the polyamide 5X fiber of the third pair of heated rolls can be from 5 to 10, and can preferably be from 6 to 8.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the polyamide 5X medium-strength yarn has the characteristics of high strength, low elongation, low thermal shrinkage and the like.
Secondly, the polyamide 5X medium-strength yarn also has the advantages of good wear resistance, good alkali resistance, dimensional stability and the like, so that the polyamide 5X medium-strength yarn is widely applied to the fields of sewing threads, safety belts, ropes, fishing nets or filter cloth and the like.
Thirdly, the invention prepares the polyamide 5X medium-strength filament by carrying out primary and secondary stretching and high-temperature tension heat setting processes through three pairs of hot rollers, thereby reducing the stretching path and saving the production cost compared with the process using four pairs of hot rollers (application number: 201510881321.1).
Detailed Description
The invention relates to a polyamide 5X medium-strength yarn and a preparation method thereof.
< Polyamide 5X Medium Strength yarn >
The raw materials for producing polyamide 5X of the present invention at least include: 1, 5-pentanediamine and a dicarboxylic acid; or polyamide 5X obtained by polymerizing 1, 5-pentanediamine and dicarboxylic acid as monomers.
The dicarboxylic acids may include short chain dicarboxylic acids and/or long chain dicarboxylic acids. The short-chain dibasic acid can be any one selected from succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid or sebacic acid. The long-chain dicarboxylic acid may be any one selected from undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid, and Δ 9-1, 18-octadecenedioic acid.
In the polyamide 5X, X may take an integer of 2 to 18, for example, the polyamide 5X may include: polyamide 52, polyamide 54, polyamide 56, polyamide 510, polyamide 511, polyamide 512, polyamide 513, polyamide 514, polyamide 515, polyamide 516, polyamide 517, polyamide 518, and the like.
The above-mentioned 1, 5-pentanediamine may be produced by a biological fermentation method or may be produced by a chemical method, and is preferably produced by a biological fermentation method in view of environmental influences.
The polyamide 5X medium strength yarn of the present invention may contain a copolymerized component or a mixed second component or third component in addition to the main component (the dibasic acid and the diamine) within a range not deviating from the object of the present invention. As the copolymerization component, for example: structural units derived from aliphatic dicarboxylic acids, alicyclic dicarboxylic acids, and aromatic dicarboxylic acids. Further, the resin composition may contain a structural unit derived from a structural unit of an aliphatic diamine such as ethylenediamine or hexamethylenediamine, for example, an alicyclic diamine structural unit of cyclohexanediamine, an aromatic diamine structural unit of xylylenediamine, an amino acid such as 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, or p-aminomethylbenzoic acid, or a lactam such as e-caprolactam or ω -laurolactam.
Further, in the present invention, the raw material for producing the strong yarn in polyamide 5X may include various additives in addition to the above-mentioned 1, 5-pentanediamine and dicarboxylic acid according to the actual use requirements. Various additives including, but not limited to, delusterants, flame retardants, antioxidants, ultraviolet absorbers, infrared absorbers, crystal nucleating agents, fluorescent brighteners, antistatic agents, or the like may be copolymerized or mixed as needed in a total additive content of 0.001 to 10 wt%. The above additives may be added in the alternative or in any combination.
[ Properties of Polyamide 5X Medium Strength yarn ]
The properties of the filaments in the above polyamide 5X are as follows:
(1) Fineness:
the titer of the polyamide 5X medium-strength filaments can be 110 to 1100dtex, can be preferably 210 to 990dtex, can be further preferably 220 to 880dtex, and can be further preferably 220 to 550dtex.
(2) And breaking strength:
the breaking strength of the filaments in polyamide 5X may be 6.0 to 8.0cN/dtex, and may preferably be 6.3 to 7.6cN/dtex, and may more preferably be 6.5 to 7.2cN/dtex, and still more preferably be 6.7 to 7.0cN/dtex.
(3) Elongation at break:
the elongation at break of the filaments in polyamide 5X may be 14 to 25%, and may preferably be 14 to 16%.
The breaking strength and breaking elongation are measured according to GB/T14344-2008.
(4) Dry heat shrinkage ratio:
the dry heat shrinkage of the filament in the polyamide 5X may be 3.0 to 8.0%, may be preferably 3.5 to 7.5%, and may be more preferably 4.0 to 6.0%.
Wherein the dry heat shrinkage is performed according to FZ/T50004, and the heat treatment temperature is 180 ℃.
(5) Boiling water shrinkage ratio:
the boiling water shrinkage of the polyamide 5X medium filament may be 2.0 to 7.0%, preferably 3.0 to 6.0%, and more preferably 4.0 to 5.0%.
Wherein, the boiling water shrinkage rate is measured by reference to GB/6505-2008 'test method for chemical fiber filament thermal shrinkage rate', which comprises the following specific steps: taking a section of polyamide 5X medium-strength fiber, pre-tensioning by 0.05 +/-0.005 cN/dtex, marking 50.00cm at the two ends of the middle of the section of polyamide 5X medium-strength fiber, wrapping the section of polyamide 5X medium-strength fiber with gauze, putting the section of polyamide 5X medium-strength fiber into boiling water to boil for 30min, drying a sample, measuring the length between two marked points, and calculating the boiling water shrinkage by adopting the following formula:
boiling water shrinkage = ((initial length-length after shrinkage)/length after shrinkage) X100%.
(6) And crystallinity:
the crystallinity of the filament in polyamide 5X may be 60 to 70%, may be preferably 61 to 69%, may be more preferably 62 to 68%, and may be more preferably 64 to 67%.
(7) Degree of orientation:
the orientation degree of the filaments in the polyamide 5X may be 70 to 80%, may preferably be 71 to 79%, may more preferably be 72 to 77%, and may more preferably be 73 to 76%.
Fiber samples were analyzed using a D/max-2550PC X-ray diffractometer manufactured by Rigaku Corporation, japan, at a Cu target wavelength
Figure BDA0002225673650000081
The voltage is 20-40kV, the current is 10-450mA, and the range of the measurement angle 2 theta is 5-40 degrees. Fully shearing a polyamide 5X medium-strength fiber sample for testing crystallization, wherein the mass of the sample is more than 0.2g; the polyamide 5X medium strength fiber samples used for testing the crystallite orientation were carded in order, with a strand length of 30mm, and tested. And (4) performing data processing by using origin software and the like, and analyzing and calculating the crystallinity and the orientation of the fiber.
Formula for calculating crystallinity:
Figure BDA0002225673650000082
wherein, sigma IcIntegrated intensity of total diffraction for crystalline fraction; sigma IaThe integrated intensity of scattering of the amorphous fraction.
Formula for calculating degree of orientation:
Figure BDA0002225673650000083
wherein HiThe peak width at half maximum of the ith peak.
(8) And wear resistance:
the abrasion resistance of the fiber is tested by an LFY-109 type computer yarn abrasion resistance tester. And judging the wear resistance index by the wear resistance times of the fiber. The larger the number of times the fiber is resistant to abrasion, the better the resistance to abrasion.
(9) And alkali resistance:
the alkali resistance test method of the polyamide 5X medium-strength yarn is a sodium hydroxide solution soaking method. The polyamide 5X medium-strength yarn is soaked in a 5% sodium hydroxide solution for the same time (for example, 168 hours), and the mechanical properties (breaking strength) before and after soaking are measured to evaluate the alkali resistance.
< preparation method of Polyamide 5X Medium-Strength yarn >
A preparation method of polyamide 5X medium-strength yarn comprises the following steps:
(1) Polymerizing 1, 5-pentanediamine and dicarboxylic acid to form a polyamide 5X melt; or,
heating polyamide 5X (polyamide 5X resin) to a molten state to form a polyamide 5X melt;
(2) Spinning the polyamide 5X melt to form primary yarn;
(3) And treating the primary yarn to obtain the polyamide 5X medium-strength yarn.
When the raw material for producing the strong yarn in polyamide 5X further includes a comonomer, the comonomer is added in step (1).
When the raw material for producing the strong yarn in polyamide 5X further includes an additive, the additive is added in step (1).
In the step (1), the polymerization comprises the following steps:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, dicarboxylic acid and water to prepare a salt solution of polyamide; wherein, the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.05): 1;
(1-2) heating the salt solution of the polyamide, raising the pressure in the reaction system to 0.3-2.0Mpa, exhausting, maintaining the pressure, reducing the pressure to reduce the pressure in the reaction system to 0-0.2Mpa in gauge pressure, and vacuumizing to-0.08-0.01 Mpa in vacuum degree to obtain the polyamide 5X melt.
When the raw material for producing the filament in polyamide 5X further comprises a comonomer, the comonomer is added in step (1-1).
When the raw material for producing the strong yarn in polyamide 5X further includes an additive, the additive is added in step (1-1).
The temperature of the reaction system at the end of the pressure maintaining is 232-265 ℃.
The temperature of the reaction system after the pressure reduction is finished is 245-280 ℃.
The temperature after vacuum pumping is 260-280 ℃.
In step (1), the polyamide 5X resin is a polyamide 5X chip, which is prepared according to the preparation method disclosed in CN 104031263A.
Among them, since polyamide 5X resin has a strong water absorption property, it is necessary to dry it before melting by heating, and it is preferable to dry it at 80 to 130 ℃ for 10 to 30 hours, if necessary, and then melt it by heating in a single-screw extruder after drying.
The polyamide 5X resin has a water content of 50 to 1500ppm, preferably 200 to 800ppm, more preferably 300 to 700ppm, and still more preferably 400 to 600ppm.
The polyamide 5X resin may have a relative viscosity of 96% sulfuric acid of 2.5 to 3.0, may preferably be 2.6 to 2.9, and may more preferably be 2.7 to 2.8.
The relative viscosity was measured as follows:
the relative viscosity of the polyamide 5X resin is measured by a Ubbelohde viscometer concentrated sulfuric acid method, and the method comprises the following steps: the dried polyamide 5X chips or staple fiber samples thereof were accurately weighed at 0.25. + -. 0.0002g, dissolved in 50mL of concentrated sulfuric acid (96%), and the flow-through time t of the concentrated sulfuric acid was measured and recorded in a thermostatic water bath at 25 ℃0And the flow-through time t of the polyamide 5X-chip or its staple fiber sample solution.
The relative viscosity is calculated by the formula: relative viscosity VN = t/t0
t-solution flow time;
t0-solvent flow time.
The heating in the step (1) is carried out in a screw extruder, the screw extruder is divided into five zones for heating, the temperature of the first zone is 200-300 ℃, the temperature of the second zone is 230-320 ℃, the temperature of the third zone is 240-350 ℃, the temperature of the fourth zone is 270-360 ℃, and the temperature of the fifth zone is 270-400 ℃.
Preferably, the second zone temperature is greater than the first zone temperature; the temperature of the three zone, the temperature of the four zone or the temperature of the five zone is higher than the temperature of the first zone or the temperature of the second zone.
When the raw material for producing the filament in the polyamide 5X also comprises the additive, the polyamide 5X is heated to a molten state to form a polyamide 5X melt, and then the polyamide 5X melt is mixed with the additive.
In the step (2), the spinning comprises the following steps:
and (3) spraying the polyamide 5X melt through a spinneret plate of a spinning manifold to form the primary yarn.
Among them, the temperature of the spinning beam may be 200 to 350 ℃, more preferably 210 to 330 ℃, still more preferably 220 to 310 ℃, and still more preferably 240 to 300 ℃.
The pressure of the spin pack of the spinning beam may be 10 to 30MPa, preferably 15 to 25MPa, and more preferably 17 to 24MPa.
The number of holes of the spinneret may be 48 to 576f, may preferably be 64 to 480f, may more preferably be 96 to 288f, and may more preferably be 96 to 192f.
The spinneret has a spinneret draw ratio of 50 to 300, preferably 70 to 140, more preferably 80 to 110, even more preferably 90 to 100.
In the step (3), the processing includes the steps of:
and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 5X medium-strength yarn.
Wherein the cooling is performed by cross air blow; the wind speed of the cross air blow can be preferably 0.5-0.9m/s, and can be more preferably 0.6-0.8m/min; the air temperature of the cross air blower is preferably 15-32 ℃, more preferably 20-28 ℃, and further preferably 23-26 ℃; the humidity of the cross-air may be 60 to 80%, and may preferably be 65 to 78%.
The winding speed may be 2000 to 3500m/min, and may preferably be 2200 to 3000m/min, and may more preferably be 2200 to 2800m/min.
The stretching process is more than two-stage stretching, and specifically comprises the following steps: the oiled nascent yarn enters a winding room through a spinning channel, is fed into a first pair of hot rollers through a godet roller, is subjected to primary stretching between the first pair of hot rollers and a second pair of hot rollers, is subjected to secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and is subjected to tension heat setting.
Tension heat setting means heat setting in a state where the fibers are tensioned, and tension heat setting is mainly performed between the second pair of hot rolls and the third pair of hot rolls.
Wherein the stretching ratio of the first-stage stretching can be 3.0-4.5, the stretching temperature can be 60-180 ℃, and the first-stage stretching is the main stretching.
The stretching ratio of the secondary stretching may be 1.0-2.0, and the stretching temperature may be 140-200 ℃.
The total stretching ratio may be 3.0 to 9.0, and may preferably be 4.0 to 6.0.
Actually, the stretching process may be three-stage stretching, four-stage stretching, five-stage stretching or six-stage stretching, and the two-stage stretching is preferable in the embodiment; the stretching ratio may preferably be 4.0 to 6.0, and the stretching temperature may preferably be 60 to 150 ℃.
The heat-setting temperature may be 180 to 240 ℃ and may preferably be 200 to 230 ℃.
The speed of the godet rolls may be from 200 to 800m/min, and may preferably be from 400 to 600m/min.
The speed of the first pair of hot rolls may be in the range of 300 to 900m/min, and may preferably be in the range of 500 to 700m/min.
The speed of the second thermo roll can be 1500-2200m/min, and can preferably be 1600-2000m/min.
The speed of the third pair of thermo rolls may be 2200 to 3000m/min, and may preferably be 2200 to 2800m/min.
The number of windings of the polyamide 5X fibers of the first thermo roll may be 4-8 and may preferably be 5-7.
The number of windings of the polyamide 5X fibers of the second pair of hot rolls may be 6 to 12 and may preferably be 7 to 10.
The number of wraps of the polyamide 5X fibers of the third pair of heated rolls can be from 5 to 10 and can preferably be from 6 to 8.
The present invention will be further described with reference to examples and comparative examples.
The first embodiment is as follows: polyamide 56 medium strength yarn (550 dtex/96 f)
The embodiment provides a preparation method of a polyamide 56 medium-strength filament, which comprises the following steps:
(1) Heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
(2) Spinning the polyamide 56 melt to form primary yarn;
(3) And treating the primary yarn to obtain the polyamide 56 medium-strength yarn.
Wherein, in the step (1), the relative viscosity of the polyamide 56 resin (in a slice form) is 2.7, and the polyamide resin is prepared by a biological fermentation method.
The heating in step (1) is carried out in a single screw extruder, which is divided into five zones for heating, wherein the temperature of the first zone is 250 ℃, the temperature of the second zone is 260 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 280 ℃.
The spinning in the step (2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 280 ℃, and the pressure of the spinning assembly of the spinning beam is 18.0MPa.
The processing in the step (3) comprises the following steps: and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 56 medium-strength yarn. Wherein the cooling is carried out by cross-air blowing, the air speed is 0.55m/s, the air temperature is 22 ℃, and the humidity is 73%. The winding tension was 50cN.
The properties of the filaments in the polyamide 56 obtained in this example are shown in tables 6 and 7.
The parameters of the winding process in this embodiment are shown in table 1.
TABLE 1 winding Process for the filaments (550 dtex/96 f) in the polyamide 56 of this example
Device Temperature (. Degree.C.) Speed (m/min) Number of turns of wire hanging
Godet roller / 450 /
First hot roller pair 100 500 6
Second pair of hot rollers 180 1700 9
Third heat roller pair 230 2560 7
Winding of / 2500 /
The second embodiment: polyamide 56 medium strength yarn (830 dtex/192 f)
The embodiment provides a preparation method of a polyamide 56 medium-strength wire, which comprises the following steps:
(1) Heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
(2) Spinning the polyamide 56 melt to form primary yarn;
(3) And treating the primary yarn to obtain the polyamide 56 medium-strength yarn.
In the step (1), the polyamide 56 resin (in the form of chips) had a relative viscosity of 2.8 and was prepared by a biological fermentation method.
The heating in the step (1) is carried out in a single screw extruder, the screw extruder is divided into five zones for heating, the temperature of the first zone is 255 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 285 ℃.
The spinning in the step (2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly of the spinning manifold is 18.5MPa.
The processing in the step (3) comprises the following steps: and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 56 medium-strength yarn. Wherein the cooling is carried out by cross air blow, the air speed is 0.65m/s, the air temperature is 20 ℃, and the humidity is 72%. The winding tension was 80cN.
The properties of the filaments in the polyamide 56 obtained in this example are shown in tables 6 and 7.
The parameters of the winding process in this embodiment are shown in table 2.
TABLE 2 winding process of the strength yarn (830 dtex/192 f) in the polyamide 56 of this example.
Device Temperature (. Degree.C.) Speed (m/min) Number of turns of wire hanging
Godet roller / 500 /
First pair of hot rollers 90 550 5
Second pair of hot rollers 200 1900 8
Third pair of hot rollers 220 2650 8
Winding of / 2600 /
Example three: polyamide 56 medium-strength yarn (300 dtex/60 f)
The embodiment provides a preparation method of a polyamide 56 medium-strength wire, which comprises the following steps:
(1) Heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
(2) Spinning the polyamide 56 melt to form primary yarn;
(3) And treating the primary yarn to obtain the polyamide 56 medium-strength yarn.
Wherein, in the step (1), the relative viscosity of the polyamide 56 resin (in a slice form) is 3.0, and the polyamide resin is prepared by a biological fermentation method.
The heating in step (1) is carried out in a single screw extruder, which is divided into five zones with a first zone temperature of 265 ℃, a second zone temperature of 275 ℃, a third zone temperature of 295 ℃, a fourth zone temperature of 295 ℃ and a fifth zone temperature of 290 ℃.
The spinning in the step (2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 290 ℃, and the pressure of the spinning assembly of the spinning beam is 19.0MPa.
The processing in the step (3) comprises the following steps: and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 56 medium-strength yarn. Wherein the cooling is carried out by cross-air blowing, the air speed is 0.85m/s, the air temperature is 18 ℃, and the humidity is 68%. The winding tension was 50cN.
The properties of the filaments in the polyamide 56 obtained in this example are shown in tables 6 and 7.
The parameters of the winding process in this embodiment are shown in table 3.
TABLE 3 winding Process for the filaments (300 dtex/60 f) in the polyamide 56 of this example.
Device Temperature (. Degree.C.) Speed (m/min) Number of turns of wire hanging
Godet roller / 560 /
First hot roller pair 105 600 6
Second pair of hot rollers 210 1850 9
Third pair of hot rollers 235 2850 8
Winding of / 2800 /
Example four: polyamide 56 medium strength yarn (833 dtex/192 f)
The embodiment provides a preparation method of a polyamide 56 medium-strength wire, which comprises the following steps:
(1) Heating the polyamide 56 resin to a molten state to form a polyamide 56 melt;
(2) Spinning the polyamide 56 melt to form primary yarn;
(3) And treating the primary yarn to obtain the polyamide 56 medium-strength yarn.
Wherein, in the step (1), the relative viscosity of the polyamide 56 resin (in a slice form) is 2.5, and the polyamide resin is prepared by a biological fermentation method.
The heating in step (1) is carried out in a single screw extruder, which is divided into five zones for heating, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 255 ℃, the temperature of the third zone is 265 ℃, the temperature of the fourth zone is 270 ℃, and the temperature of the fifth zone is 270 ℃.
The spinning in the step (2) comprises the following steps: and (3) feeding the polyamide 56 melt into a metering pump through a melt pipeline, accurately metering by the metering pump, feeding into a spinning box, and spraying out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 270 ℃, and the pressure of the spinning assembly of the spinning beam is 16.5MPa.
The processing in the step (3) comprises the following steps: and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyamide 56 medium-strength yarn. Wherein the cooling is carried out by cross air blow, the air speed is 0.8m/s, the air temperature is 16 ℃, and the humidity is 65%. The winding tension was 82cN.
The properties of the filaments in the polyamide 56 obtained in this example are shown in tables 6 and 7.
The parameters of the winding process in this embodiment are shown in table 4.
Table 4 winding process of the strong yarn (833 dtex/192 f) in the polyamide 56 of this example.
Device Temperature (. Degree. C.) Speed (m/min) Number of turns of wire hanging
Godet roller / 520 /
First hot roller pair 110 550 7
Second pair of hot rollers 205 1950 9
Third pair of hot rollers 225 2700 6
Winding of / 2680 /
Comparative example one: polyester medium strength yarn (830 dtex/192 f)
The comparative example provides a preparation method of polyester medium strength yarn, which comprises the following steps:
(1) Heating the polyester resin to a molten state to form a polyester melt;
(2) Spinning the polyester melt to form primary raw silk;
(3) And treating the nascent fiber to obtain the polyester medium-strength fiber.
Wherein, in the step (1), the intrinsic viscosity of the polyester resin (in the form of chips) was 0.7dL/g.
The heating in the step (1) is carried out in a single screw extruder, the screw extruder is divided into five zones for heating, the temperature of the first zone is 255 ℃, the temperature of the second zone is 275 ℃, the temperature of the third zone is 295 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 290 ℃.
The spinning in the step (2) comprises the following steps: and (3) feeding the polyester melt into a metering pump through a melt pipeline, accurately metering the polyester melt by the metering pump, feeding the polyester melt into a spinning box, and spraying the polyester melt out through a spinneret orifice of a spinneret plate to form the nascent fiber. Wherein the temperature of the spinning beam is 290 ℃, and the pressure of the spinning assembly of the spinning beam is 15.5MPa.
The processing in the step (3) comprises the following steps: and cooling, oiling, stretching, heat setting and winding the as-spun yarn to obtain the polyester medium-strength yarn. Wherein the cooling is carried out by cross-air blowing, the air speed is 0.6m/s, the air temperature is 18 ℃, and the humidity is 75%. The winding tension was 85cN.
The properties of the filaments in the polyester obtained in this comparative example are shown in tables 6 and 7.
Wherein, the parameters of the winding process in this comparative example are shown in table 5.
TABLE 5 winding process of the reinforcing filaments (830 dtex/192 f) in the polyester of this comparative example.
Device Temperature (. Degree.C.) Speed (m/min) Number of turns of wire
Godet roller / 520 /
First pair of hot rollers 130 550 6
Second pairHot roller 200 1750 7
Third pair of hot rollers 240 2650 7
Winding of / 2620 /
TABLE 6 partial Performance of the products of the examples and comparative examples Table I
Figure BDA0002225673650000161
TABLE 7 partial Performance of the products of the examples and comparative examples TABLE II
Figure BDA0002225673650000162
Figure BDA0002225673650000171
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.

Claims (26)

1. A polyamide 5X medium-strength yarn is characterized in that: raw materials for producing the polyamide 5X medium-strength filament at least comprise 1, 5-pentanediamine and dicarboxylic acid; the breaking strength of the polyamide 5X medium-strength filaments is 6.0-8.0cN/dtex; the dry heat shrinkage rate of the polyamide 5X medium-strength filament is 3.0-8.0%;
the titer of the polyamide 5X medium-strength fiber is 110-1100dtex;
the boiling water shrinkage of the polyamide 5X medium-strength fiber is 2.0-7.0%;
the crystallinity of the polyamide 5X medium-strength fiber is 60-70%;
the orientation degree of the strong filaments in the polyamide 5X is 70-80%;
the polyamide 5X medium-strength filament is prepared by a preparation method comprising the following steps of:
(1) Polymerizing 1, 5-pentanediamine and dicarboxylic acid to form a polyamide 5X melt; or,
heating polyamide 5X resin to a molten state to form a polyamide 5X melt;
(2) Spinning the polyamide 5X melt to form primary yarns;
(3) Treating the primary raw silk to obtain the polyamide 5X medium-strength silk;
in the step (3), the processing includes the steps of:
cooling, oiling, stretching, heat setting and winding the primary raw silk to obtain the polyamide 5X medium-strength silk;
the stretching process is two-stage stretching:
the stretching process comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, and performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers and performing heat setting;
wherein the stretching multiple of the primary stretching is 3.0-4.5, and the stretching temperature is 60-180 ℃;
the stretching multiple of the secondary stretching is 1.0-2.0, and the stretching temperature is 140-200 ℃;
the heat setting temperature is 180-240 ℃;
the number of winding turns of the polyamide 5X fiber of the second pair of hot rollers is 6-12;
the number of winding turns of the polyamide 5X fiber of the third pair of hot rollers is 5-10;
the winding speed is 2000-3500m/min.
2. The polyamide 5X medium strength yarn of claim 1, wherein:
the titer of the polyamide 5X medium-strength filament is 220-990dtex; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 5X medium-strength filaments is 6.3-7.6cN/dtex.
3. The polyamide 5X medium strength yarn of claim 2, wherein:
the titer of the polyamide 5X medium-strength filament is 220-880dtex; and/or the presence of a gas in the gas,
the breaking strength of the strong filaments in the polyamide 5X is 6.5-7.2cN/dtex.
4. Polyamide 5X medium strength yarn according to claim 2 or 3, characterized in that:
the titer of the polyamide 5X medium-strength fiber is 220-550dtex; and/or the presence of a gas in the gas,
the breaking strength of the polyamide 5X medium-strength filaments is 6.7-7.0cN/dtex.
5. The polyamide 5X medium strength yarn of claim 1, wherein: the elongation at break of the polyamide 5X medium-strength filaments is 14-25%; and/or the presence of a gas in the atmosphere,
the dry heat shrinkage rate of the polyamide 5X medium-strength fiber is 3.5-7.5%; and/or the presence of a gas in the atmosphere,
the boiling water shrinkage of the polyamide 5X medium-strength fiber is 3.0-6.0%; and/or the presence of a gas in the gas,
the crystallinity of the polyamide 5X medium-strength fiber is 61-69%; and/or the presence of a gas in the gas,
the orientation degree of the strong filaments in the polyamide 5X is 71-79%.
6. The polyamide 5X medium strength yarn of claim 5, wherein: the elongation at break of the polyamide 5X medium-strength filaments is 14-16%; and/or the presence of a gas in the gas,
the dry heat shrinkage rate of the polyamide 5X medium-strength filament is 4.0-6.0%; and/or the presence of a gas in the gas,
the boiling water shrinkage of the polyamide 5X medium-strength fiber is 4.0-5.0%; and/or the presence of a gas in the gas,
the crystallinity of the polyamide 5X medium-strength yarn is 62-68%; and/or the presence of a gas in the atmosphere,
the orientation degree of the strong filaments in the polyamide 5X is 72-77%.
7. Polyamide 5X medium strength yarn according to claim 5 or 6, characterized in that:
the crystallinity of the polyamide 5X medium-strength yarn is 64-67%; and/or the presence of a gas in the atmosphere,
the orientation degree of the strong filaments in the polyamide 5X is 73-76%.
8. The polyamide 5X medium strength yarn of claim 1, wherein: the 1, 5-pentanediamine is prepared from bio-based raw materials by a fermentation method or an enzyme conversion method; and/or the presence of a gas in the atmosphere,
the number of carbon atoms of the dicarboxylic acid is 4-18; the dicarboxylic acids include succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid and Δ9-one or more of 1,18 octadecenedioic acid; and/or the presence of a gas in the gas,
the raw materials for producing the polyamide 5X medium-strength yarn also contain comonomers and/or additives.
9. The polyamide 5X medium strength yarn of claim 8, wherein the comonomers comprise: any one or more of aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic dicarboxylic acid, ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, epsilon-caprolactam and omega-laurolactam; and/or the presence of a gas in the atmosphere,
the additive comprises: any one or more of a delustering agent, a flame retardant, an antioxidant, an ultraviolet absorbent, an infrared absorbent, a crystallization nucleating agent, a fluorescent brightener and an antistatic agent;
the additive accounts for 0.001-10% of the total weight of the raw materials.
10. A process for the preparation of a polyamide 5X mesogen yarn according to any of claims 1 to 9, characterized in that: the preparation method comprises the following steps:
(1) Polymerizing 1, 5-pentanediamine and dicarboxylic acid to form a polyamide 5X melt; or,
heating polyamide 5X resin to a molten state to form a polyamide 5X melt;
(2) Spinning the polyamide 5X melt to form primary yarns;
(3) Treating the primary raw silk to obtain the polyamide 5X medium-strength silk;
in the step (3), the processing includes the steps of:
cooling, oiling, stretching, heat setting and winding the primary raw silk to obtain the polyamide 5X medium-strength silk;
the stretching process is two-stage stretching:
the stretching process comprises the following steps: feeding the oiled as-spun yarn into a first pair of hot rollers through a godet roller, performing primary drawing between the first pair of hot rollers and a second pair of hot rollers, and performing secondary drawing between the second pair of hot rollers and a third pair of hot rollers and performing heat setting;
wherein the stretching multiple of the primary stretching is 3.0-4.5, and the stretching temperature is 60-180 ℃;
the stretching multiple of the secondary stretching is 1.0-2.0, and the stretching temperature is 140-200 ℃;
the temperature of the heat setting is 180-240 ℃;
the number of winding turns of the polyamide 5X fiber of the second pair of hot rollers is 6-12;
the number of winding turns of the polyamide 5X fiber of the third pair of hot rollers is 5-10;
the winding speed is 2000-3500m/min.
11. The method of manufacturing according to claim 10, wherein: the speed of the godet roller is 200-800m/min; and/or the presence of a gas in the gas,
the speed of the first hot roller pair is 300-900m/min; and/or the presence of a gas in the gas,
the speed of the second hot pair of rollers is 1500-2200m/min; and/or the presence of a gas in the gas,
the speed of the third pair of hot rolls is 2200 to 3000m/min; and/or the presence of a gas in the atmosphere,
the number of turns of the polyamide 5X fiber of the first hot roller is 4-8.
12. The production method according to claim 10 or 11, characterized in that: in the step (1), the polymerization comprises the following steps:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, dicarboxylic acid and water to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.05): 1;
(1-2) heating the salt solution of the polyamide, increasing the pressure in the reaction system to 0.3-2.0MPa, exhausting, maintaining the pressure, reducing the pressure to 0-0.2MPa, vacuumizing to-0.08 to-0.01 MPa, wherein the pressure is gauge pressure, and obtaining a polyamide 5X melt;
wherein the temperature of the reaction system is 232-265 ℃ when the pressure maintaining is finished;
the temperature of the reaction system after the pressure reduction is finished is 245-280 ℃;
the temperature after vacuum pumping is 260-280 ℃.
13. The production method according to claim 10 or 11, characterized in that: in the step (1), the polyamide 5X resin is polyamide 5X slices; and/or the presence of a gas in the gas,
the relative viscosity of 96% sulfuric acid of the polyamide 5X resin is 2.5-3.0; and/or the presence of a gas in the atmosphere,
the polyamide 5X resin has a water content of 50-1500ppm; and/or the presence of a gas in the gas,
the heating in the step (1) is carried out in a screw extruder which is divided into five zones for heating;
wherein the temperature of the first zone is 200-300 ℃; and/or the presence of a gas in the atmosphere,
the temperature of the second zone is 230-320 ℃; and/or the presence of a gas in the gas,
the temperature of the three zones is 240-350 ℃; and/or the presence of a gas in the gas,
the temperature of the fourth zone is 270-360 ℃; and/or the presence of a gas in the atmosphere,
the temperature of the fifth area is 270-400 ℃; and/or the presence of a gas in the atmosphere,
the second zone temperature is greater than the first zone temperature;
the three zone temperature, the four zone temperature, or the five zone temperature is greater than the first zone temperature or the second zone temperature;
when the raw material for producing the filaments in the polyamide 5X further comprises a comonomer and/or an additive, the comonomer and/or the additive is added in step (1).
14. The method for producing as claimed in claim 13, characterized in that: the relative viscosity of 96% sulfuric acid of the polyamide 5X resin is 2.6-2.9; and/or the presence of a gas in the atmosphere,
the polyamide 5X resin has a water content of 200-800ppm.
15. The method for producing as claimed in claim 14, wherein: the relative viscosity of 96% sulfuric acid of the polyamide 5X resin is 2.7-2.8; and/or the presence of a gas in the gas,
the polyamide 5X resin has a water content of 300-700ppm.
16. The method of claim 15, wherein: the polyamide 5X resin has a water content of 400-600ppm.
17. The method of manufacturing according to claim 10, wherein: in the step (2), the spinning comprises the following steps:
spraying the polyamide 5X melt through a spinneret plate of a spinning manifold to form the primary yarn;
the temperature of the spinning manifold is 200-350 ℃; and/or the presence of a gas in the atmosphere,
the pressure of a spinning assembly of the spinning manifold is 10-30MPa; and/or the presence of a gas in the atmosphere,
the number of holes of the spinneret plate is 48-576f; and/or the presence of a gas in the atmosphere,
the spinneret draw ratio of the spinneret plate is 50-300.
18. The method of claim 17, wherein: the temperature of the spinning manifold is 210-330 ℃; and/or the presence of a gas in the gas,
the pressure of a spinning assembly of the spinning manifold is 15-25MPa; and/or the presence of a gas in the atmosphere,
the number of holes of the spinneret plate is 64-480f; and/or the presence of a gas in the gas,
the spinneret has a spinneret draw ratio of 70 to 140.
19. The method for preparing a polycarbonate resin composition according to claim 18, wherein: the temperature of the spinning manifold is 220-310 ℃; and/or the presence of a gas in the gas,
the pressure of a spinning assembly of the spinning manifold is 17-24MPa; and/or the presence of a gas in the atmosphere,
the number of holes of the spinneret plate is 96-288f; and/or the presence of a gas in the atmosphere,
the spinneret draw ratio of the spinneret plate is 80-110.
20. The method of manufacturing according to claim 19, wherein: the temperature of the spinning manifold is 240-300 ℃; and/or the presence of a gas in the gas,
the number of holes of the spinneret plate is 96-192f; and/or the presence of a gas in the gas,
the spinneret draw ratio of the spinneret plate is 90-100.
21. The method for producing as claimed in claim 10, characterized in that: the cooling is carried out by cross air blowing; the wind speed of the cross air blow is 0.5-0.9m/s; the air temperature of the side blowing air is 15-32 ℃; the humidity of the cross air blower is 60-80%; and/or the presence of a gas in the atmosphere,
the winding tension during winding forming is 50-150cN.
22. The method of manufacturing according to claim 21, wherein: the wind speed of the cross air blow is 0.6-0.8m/s; the air temperature of the cross air blow is 20-28 ℃; the humidity of the cross air blow is 65-78%; and/or the presence of a gas in the gas,
the winding tension during winding forming is 70-120cN; and/or the presence of a gas in the atmosphere,
the winding speed is 2200 to 3000m/min.
23. The method of manufacturing according to claim 22, wherein: the air temperature of the cross air blow is 23-26 ℃; and/or the presence of a gas in the gas,
the winding tension during winding forming is 75-110cN; and/or the presence of a gas in the gas,
the winding speed is 2200-2800m/min.
24. The method of claim 23, wherein: the winding tension during winding forming is 80-100cN.
25. The method for producing as claimed in claim 10, characterized in that: in the stretching process, the total stretching multiple is 3.0-9.0.
26. The method of manufacturing according to claim 25, wherein: the total stretching multiple is 4.0-6.0; and/or the presence of a gas in the atmosphere,
the heat setting temperature is 200-230 ℃; and/or the presence of a gas in the gas,
the speed of the godet roller is 400-600m/min; and/or the presence of a gas in the gas,
the speed of the first thermo roll is 500-700m/min; and/or the presence of a gas in the gas,
the speed of the second pair of hot rollers is 1600-2000m/min; and/or the presence of a gas in the gas,
the speed of the third pair of hot rolls is 2200 to 2800m/min; and/or the presence of a gas in the atmosphere,
the number of winding turns of the polyamide 5X fibers of the first hot roller is 5-7; and/or the presence of a gas in the gas,
the number of winding turns of the polyamide 5X fiber of the second pair of hot rollers is 7-10; and/or the presence of a gas in the atmosphere,
the number of turns of the polyamide 5X fiber of the third pair of heated rolls is 6-8.
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