CN114293278A - 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 PDFInfo
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- CN114293278A CN114293278A CN202011000012.6A CN202011000012A CN114293278A CN 114293278 A CN114293278 A CN 114293278A CN 202011000012 A CN202011000012 A CN 202011000012A CN 114293278 A CN114293278 A CN 114293278A
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- 229920006141 Polyamide 5X Polymers 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000004744 fabric Substances 0.000 claims abstract description 36
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- 238000004043 dyeing Methods 0.000 claims abstract description 19
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 238000004804 winding Methods 0.000 claims description 85
- 238000009987 spinning Methods 0.000 claims description 63
- 238000001816 cooling Methods 0.000 claims description 51
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 39
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- 239000011347 resin Substances 0.000 claims description 38
- 238000009998 heat setting Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 23
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 22
- 238000007664 blowing Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 17
- 239000001361 adipic acid Substances 0.000 claims description 11
- 235000011037 adipic acid Nutrition 0.000 claims description 11
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- 230000000996 additive effect Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
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- QCNWZROVPSVEJA-UHFFFAOYSA-N Heptadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCC(O)=O QCNWZROVPSVEJA-UHFFFAOYSA-N 0.000 claims description 4
- BTZVDPWKGXMQFW-UHFFFAOYSA-N Pentadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCC(O)=O BTZVDPWKGXMQFW-UHFFFAOYSA-N 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- QQHJDPROMQRDLA-UHFFFAOYSA-N hexadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCC(O)=O QQHJDPROMQRDLA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 4
- BNJOQKFENDDGSC-UHFFFAOYSA-N octadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCC(O)=O BNJOQKFENDDGSC-UHFFFAOYSA-N 0.000 claims description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 4
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 4
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 claims description 4
- LWBHHRRTOZQPDM-UHFFFAOYSA-N undecanedioic acid Chemical compound OC(=O)CCCCCCCCCC(O)=O LWBHHRRTOZQPDM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002759 woven fabric Substances 0.000 claims description 4
- 238000005098 hot rolling Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 2
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006096 absorbing agent Substances 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 239000002216 antistatic agent Substances 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 claims description 2
- 239000006081 fluorescent whitening agent Substances 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 239000002667 nucleating agent Substances 0.000 claims description 2
- SBLKVIQSIHEQOF-UHFFFAOYSA-N octadec-9-enedioic acid Chemical compound OC(=O)CCCCCCCC=CCCCCCCCC(O)=O SBLKVIQSIHEQOF-UHFFFAOYSA-N 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 claims description 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 2
- 238000009940 knitting Methods 0.000 abstract description 3
- 238000009965 tatting Methods 0.000 abstract description 2
- 239000004952 Polyamide Substances 0.000 description 123
- 229920002647 polyamide Polymers 0.000 description 123
- 239000000835 fiber Substances 0.000 description 20
- 238000005507 spraying Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
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- 239000000155 melt Substances 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005562 fading Methods 0.000 description 2
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- XYWIPYBIIRTJMM-IBGZPJMESA-N 4-[[(2S)-2-[4-[5-chloro-2-[4-(trifluoromethyl)triazol-1-yl]phenyl]-5-methoxy-2-oxopyridin-1-yl]butanoyl]amino]-2-fluorobenzamide Chemical compound CC[C@H](N1C=C(OC)C(=CC1=O)C1=C(C=CC(Cl)=C1)N1C=C(N=N1)C(F)(F)F)C(=O)NC1=CC(F)=C(C=C1)C(N)=O XYWIPYBIIRTJMM-IBGZPJMESA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 239000001307 helium Substances 0.000 description 1
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention provides a polyamide 5X fully drawn yarn and 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 performance, so that the polyamide 5X fully drawn yarn can be widely applied to the field of knitting and tatting fabrics.
Description
Technical Field
The invention relates to polyamide 5X, in particular to polyamide 5X fully drawn yarn and a preparation method and application thereof.
Background
Polyamide fiber is one of synthetic fibers which are put into industrial production at the earliest time in the world, and plays a very important role in the field of synthetic fibers. The polyamide fibers are various, and currently, polyamide 6 and polyamide 66 are mainly used for industrial production and most widely applied. The main applications relate to: socks, lace underwear, corset, sports underwear, wedding dress, casual jacket, sports wear, wind-rain coat, outdoor tent, sleeping bag, climbing bag and the like; and industrial yarn is widely used in such fields as cord, transmission belt, hose, rope, fishing net, tire, parachute, etc.
The raw material for producing the polyamide 56 fiber is made by a biological method, is a green material, does not depend on petroleum resources and does not cause serious pollution to the environment, and can reduce the emission of carbon dioxide and the generation of greenhouse effect. The polyamide 56 fiber has the advantages of high strength, low-temperature dyeing property, hygroscopicity, flexibility, wear resistance, high elasticity and the like, and has wide development prospect in the fields of civil yarns and industrial yarns.
The civil polyamide filament has slightly lower mechanical property, the breaking strength is generally less than 4.0cN/dtex, the processing requirement of a high-speed warp knitting machine cannot be met more and more, the filament breakage condition in the weaving process can be caused, the tensile mechanical property 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, the shrinkage is serious in the dyeing process, the phenomenon of color fading is easily caused, particularly, the shrinkage is large in the cheese dyeing process, and the yarns close to the bobbin are difficult to permeate and dye due to large tension of the yarns because of different tension inside and outside the yarns, so that the phenomenon of color difference of the inner layer and the outer layer in dyeing is easily caused. In addition, the tension of the cone yarn after shrinkage is different in the unwinding process, the unwinding is difficult, yarn breakage is easily caused, the processing difficulty is increased, and the production cost investment is large. And the shrinkage in boiling water is large, the fabric is easy to cause large width shrinkage in the dyeing process, the width is difficult to control, and particularly, after the subsequent fabric is made into clothes, if the shrinkage is large after the subsequent fabric is washed by hot water, the shape retention of the clothes is poor.
Disclosure of Invention
One embodiment of the invention provides a polyamide 5X fully drawn yarn, wherein the dpf of a monofilament is less than or equal to 4, further less than or equal to 3, further less than or equal to 2, and further 0.5-2.
The titer of the fiber is less than or equal to 300dtex, further more than or equal to 200dtex, further more than or equal to 150dtex, further more than or equal to 100dtex, further more than or equal to 11dtex, 22dtex, 33dtex, 40dtex, 44dtex, 55dtex or 78 dtex.
The embodiment of the invention also provides a preparation method of the polyamide 5X fully drawn yarn, which comprises the steps of stretching the primary yarn formed by the polyamide 5X melt to obtain the polyamide 5X fully drawn yarn;
the stretching treatment comprises two-stage drafting by using three pairs of hot rollers, wherein the speeds of the three pairs of hot rollers are 300-5500 m/min respectively. 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 the speeds of the three pairs of hot rollers are respectively 2800-4900 m/min.
The invention further provides application of the polyamide 5X fully drawn yarn in knitted or woven fabrics.
The polyamide 5X fully drawn yarn provided by the embodiment of the invention has the characteristics of fine denier, high strength and low shrinkage rate.
Detailed Description
Exemplary embodiments that embody features and advantages of the invention are described in detail below in the specification. It is to be understood that the invention is capable of modification in various embodiments without departing from the scope of the invention, and that the description is intended to be illustrative in nature and not to limit the invention.
In one embodiment, the polyamide 5X is prepared by polymerizing 1, 5-pentanediamine and dicarboxylic acid, wherein X in 5X represents the number of carbon atoms of the dicarboxylic acid, and X is 4-18.
In one embodiment, the 1, 5-pentanediamine may be prepared from bio-based materials 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, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid, and Δ 9-1, 18-octadecenedioic acid.
One embodiment of the invention provides polyamide 5X fully drawn yarn, the fineness of which is less than or equal to 300 dtex.
In one embodiment, the fineness of the polyamide 5X fully drawn yarn may be 200dtex or less, more preferably 150dtex or less, still more preferably 100dtex, such as 20dtex, 22dtex, 44dtex, 45dtex, 55dtex, 60dtex, 70dtex, 75dtex, 78dtex, 80dtex, 90dtex, 120dtex, 150dtex, etc. Further, 11dtex, 22dtex, 33dtex, 40dtex, 44dtex, 55dtex or 78dtex may be used.
In one embodiment, the fineness of the polyamide 5X fully drawn yarn may be 22 to 78 dtex.
In one embodiment, the monofilament dpf of the polyamide 5X fully drawn yarn may be 4 or less, further 3 or less, further 2 or less, further 1 or less, for example, 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 monofilament fineness (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 breaking strength of the polyamide 5X fully drawn yarn is 5.5 to 8.5cN/dtex, further 5.8 to 8.3cN/dtex, further 6.0 to 7.8cN/dtex, further 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, 8.0 cN/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, and still more preferably 6% or less, for example, 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, and still more preferably 35% or less, for example, 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 initial modulus of the polyamide 5X fully drawn yarn is 15-40 cN/dtex, further 18-35 cN/dtex, further 20-30 cN/dtex, further 23-28 cN/dtex, such as 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, 23cN/dtex, 23.2cN/dtex, 23.5cN/dtex, 24cN/dtex, 25cN/dtex, 25.8cN/dtex, 26 cN/dtex.
In one embodiment, the dyeing uniformity (gray card) of the polyamide 5X fully drawn yarn may be not less than 3.5, further not less than 4.0, further not less than 4.5, and further not less than 5.0.
In one embodiment, the polyamide 5X fully drawn yarn may have a 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 not less than 92%, more preferably not less than 94%, still more preferably not less than 96%, and still more preferably not less than 98%, for example, 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 production rate of the polyamide 5X fully drawn yarn may be not less than 94%, more preferably not less than 95%, still more preferably not less than 96%, and still more preferably not less than 98%, for example, 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 production rate of the polyamide 5X fully drawn yarn may be 98.5 to 99.5%, where the production rate is (mass of finished fiber prepared/mass of total resin charged) × 100%.
In one embodiment, the polyamide 5X fully drawn yarn comprises an additive.
In one embodiment, the amount of the additive is 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 based on the total mass of the raw material for producing the polyamide 5X fully drawn yarn.
In one embodiment, the additive includes any one or more of a delustrant, 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 provided by the embodiment of the invention has the characteristics of high strength, low shrinkage and good dyeing property.
The polyamide 5X fully drawn yarn provided by the embodiment of the invention has good softness and dyeing performance, so that the polyamide 5X fully drawn yarn can be widely applied to the field of knitted and woven fabrics.
An embodiment of the present invention provides a method for preparing polyamide 5X fully drawn yarn, which can be used for preparing the above polyamide 5X fully drawn yarn.
The invention provides a preparation method of polyamide 5X fully drawn yarn, which comprises the step of drawing nascent yarn formed by polyamide 5X melt to obtain the polyamide 5X fully drawn yarn, wherein the drawing treatment comprises the step of carrying out 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 according to the embodiment of the invention comprises the following steps:
(1) providing a polyamide 5X melt;
(2) spraying a polyamide 5X melt through a spinneret plate of a spinning manifold to form primary yarns;
(3) and cooling, oiling, two-stage drawing, heat setting and winding forming treatment are carried out on the as-spun 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 a polyamide 5X salt solution, increasing the pressure in a reaction system to 0.3-2.5 MPa, exhausting, maintaining the pressure, reducing the pressure to 0-0.2 MPa, vacuumizing to the vacuum degree of-0.01-0.08 MPa, wherein the pressure is gauge pressure, and obtaining a 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 the 1, 5-pentanediamine and the dicarboxylic acid in step (1-1) is (1-1.08): 1.
In one embodiment, the temperature of the reaction system at the end of the pressure holding 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 pressure reduction in the step (1-2) is 240 to 280 ℃, for example, 245 ℃, 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃, 275 ℃ and 278 ℃.
In one embodiment, the temperature after the vacuum-pumping in step (1-2) is 260 to 285 ℃, for example, 270 ℃, 275 ℃, 280 ℃, 283 ℃.
In one embodiment, the polyamide 5X resin of step (1) has a relative viscosity of 96% sulfuric acid of 2.4 to 3.0, further 2.5 to 2.9, further 2.6 to 2.8, such as 2.45, 2.5, 2.6, 2.7, 2.8, 2.9, etc.; the polyamide 5X resin may have a water content of 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, 700 ppm.
In one embodiment, the heating of the polyamide 5X resin to a molten state in step (1) is performed in a screw extruder, the screw being heated in five zones, wherein the temperature in one zone may be 200 to 260 ℃, for example 220 ℃, 225 ℃, 240 ℃, 245 ℃, 250 ℃, 255 ℃, 260 ℃; the temperature of the second zone can be 230-280 deg.C, such as 235 deg.C, 240 deg.C, 245 deg.C, 250 deg.C, 255 deg.C, 260 deg.C, 265 deg.C, 270 deg.C; the temperature of the third zone can be 240-290 ℃, such as 245 ℃, 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃, 275 ℃ and 280 ℃; the temperature of the fourth zone may be 240-300 deg.C, such as 245 deg.C, 250 deg.C, 260 deg.C, 270 deg.C, 275 deg.C, 280 deg.C, 285 deg.C, 290 deg.C; the temperature of the five zones may be 250-290 ℃, such as 255 ℃, 260 ℃, 270 ℃, 280 ℃, 283 ℃, 285 ℃ and 290 ℃.
In one embodiment, the temperature of the spinning beam of step (2) may be 250 to 295 ℃, further 255 to 290 ℃, further 260 to 288 ℃, further 265 to 285 ℃, for example, 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, further 12 to 23MPa, further 14 to 20MPa, for example 13MPa, 15MPa, 16MPa, 17MPa, 19MPa, 20 MPa.
In one embodiment, the cooling in step (3) is air cooling by cross-blowing or circular-blowing, and the air speed of the cross-blowing or circular-blowing 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, 0.8 m/s; the air temperature of the cross air blow or the circular air blow can be 15-25 ℃, further 16-22 ℃, further 18-20 ℃, for example, 19 ℃, 20 ℃ and 21 ℃; the humidity of the cross-blown air or the circular-blown air may be 60 to 85%, and further 65 to 75%, for example 76%, 78%, 80%, 82%, 83%.
In one embodiment, the drawing in step (3) is: the oiled spun yarn is first fed through godets to a first pair of hot rolls, subjected to a primary draw between the first and second pair of hot rolls, then subjected to a secondary draw between the second and third pair of hot rolls and preferably subjected to tension heat setting.
In one embodiment, the first hot roller pair speed is 300-3500 m/min, the second hot roller pair speed is 1200-5000 m/min, and the third hot roller pair speed is 2000-5500 m/min.
In one embodiment, the speeds of the three pairs of hot rollers are 500-3500 m/min.
In one embodiment, the speeds of the three pairs of hot rollers are 2800-4900 m/min.
In one embodiment, the temperature of the first thermo roll may be 50 to 100 ℃, further 55 to 90 ℃, further 60 to 80 ℃, for example 65 ℃, 70 ℃, 75 ℃, 85 ℃, 95 ℃; the number of winding turns of the first heat roller may be 4 to 8, further 4 to 7, and further 4 to 6, for example 5.
In one embodiment, the temperature of the second thermo-roll pair can be 130 to 180 ℃, further 140 to 170 ℃, further 150 to 160 ℃, for example 135 ℃, 145 ℃, 155 ℃, 165 ℃; the number of winding turns of the second pair of hot rollers can be 5-10 turns, further 5-8 turns, and further 5-7 turns, for example 6 turns.
In one embodiment, the temperature of the third pair of hot rolls can be 150 to 220 ℃, further 160 to 190 ℃, further 170 to 180 ℃, for example 175 ℃ to 185 ℃; the number of winding turns of the third pair of hot rollers can be 4-10 turns, further 5-7 turns, and further 5-6 turns.
In one embodiment, the speed of the first hot roller pair is 550-1700 m/min, and further 600-1600 m/min, such as 600m/min, 700m/min, 800m/min, 900m/min, 1500 m/min; the speed of the second pair of hot rollers is 1500-2400 m/min, and further can be 1600-2300 m/min, such as 1700m/min, 1800m/min, 1900m/min and 2000 m/min; the third pair of hot rolls has a speed of 2300 to 3300m/min, and further 2400 to 3200m/min, such as 2500m/min, 2700m/min, 2800m/min, and 3000 m/min.
In one embodiment, the speed of the first hot roller pair is 2900-3400 m/min, and further may be 2950-3300 m/min; for example 3000m/min, 3150m/min, 3200 m/min; the speed of the second pair of hot rollers is 3600-4900 m/min, and further can be 4000-4850 m/min, such as 3700m/min, 3800m/min, 4000m/min, 4500m/min, 4700m/min, 4750m/min, 4800 m/min; the speed of the third pair of hot rolls is preferably 3750-4850 m/min, and further 3800-4800 m/min, such as 3800m/min, 4000m/min, 4500m/min, 4700m/min, 4750m/min, and 4800 m/min.
In one embodiment, when the speed of the third pair of hot rollers is not greater than 3300m/min, the winding speed of the winding is 2200 to 3200m/min, more preferably 2300 to 3000m/min, still more preferably 2350 to 2800m/min, such as 2300m/min, 2350m/min, 2480m/min, 2500m/min, 2650m/min, 2750m/min, 2780m/min, and 2800 m/min.
In one embodiment, when the speed of the third pair of hot rolls is not less than 3300m/min, the winding speed of the winding is 3600 to 4950m/min, further 3650 to 4900m/min, further 3700 to 4850m/min, for example 3700m/min, 4700m/min, 4720m/min, and 4730 m/min.
According to the method provided by the embodiment of the invention, high-power drafting and high-temperature heat setting are realized by adopting three pairs of hot roller two-stage drafting, so that the fine-denier, high-strength and low-shrinkage civil polyamide 5X filament can be prepared, and the problems of low strength and large shrinkage in boiling water of the fine-denier polyamide 5X fiber are solved.
In one embodiment of the present invention, the fiber yield is improved by optimizing the quality of the polyamide 5X resin (for example, adjusting the viscosity and the water content thereof), optimizing the spinning process, and the like.
An 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 160 mm; the width shrinkage rate of the fabric is less than 8 percent, and more preferably less than or equal to 4 percent; the color fastness of the fabric after washing is more than 3.5 grade, and preferably more than or equal to 4 grade; the color fastness to sunlight of the fabric is more than 3.0 grade, and preferably more than or equal to 4 grade.
In one embodiment, the polyamide 5X fully drawn yarns may be used in the field of underwear, shirts, suits, yoga suits, down jackets, outdoor tents, suits, sportswear, sleeping bags, hiking coats, socks, bags, curtains, shoe materials, embroidery threads, trademarks, sofa cloth, elastic bands, combat uniforms, wedding dresses, leisure jackets, sports dresses, and hiking dresses.
The polyamide 5X fully drawn yarn and the production thereof according to an embodiment of the present invention will be further described with reference to specific examples. The relevant tests involved are as follows:
1) fineness, monofilament dpf: the fineness was measured according to GB/T14343, dpf per filament being the total fineness per number of fibers in the multifilament.
2) Breaking strength, elongation, initial modulus: the determination of the breaking strength and the elongation can refer to the GB/T14344-2008 chemical fiber tensile property test method; applying a pretension of 0.05 +/-0.005 cN/dtex, a holding distance of 500mm and a stretching speed of 500 mm/min; modulus is the breaking strength corresponding to 1% elongation at break x 100.
3) Shrinkage in boiling water: the pretension was measured according to GB/6505 at 0.05. + -. 0.005 cN/dtex.
4) Dyeing evenness (grey card)/grade: the dyeing uniformity test method of FZ/T50008 nylon filament keeps the temperature at 98 ℃ for 30min, and judges the dyeing uniformity.
5) Water content: measured according to a Karl Fischer moisture titrator.
6) Relative viscosity of resin 96% sulfuric acid: concentrated sulfuric acid method by Ubbelohde viscometer: accurately weighing 0.25 +/-0.0002 g of dried polyamide resin slices, and adding 50mL of concentrated sulfuric acid (96 wt%) for dissolution; measuring and recording the flowing time t of concentrated sulfuric acid in a constant-temperature water bath at 25 DEG C0And the polyamide sample solution flowing time t. Viscosity number calculation formula: relative viscosity t/t0(ii) a t-solution flow time; t is t0-solvent flow time.
7) Dyeing double A rate: the dyed double a rate (dyed vicat uniformity ≥ 4.5 grade fiber weight)/total weight of all dyed fibers) x 100%.
8) The yield is as follows: the yield (mass of finished fiber prepared/mass of resin charged in total) × 100%.
9) Washing color fastness: reference is made to the standard ISO 105C 06A 1S. The light fastness is referred to standard ISO 105B 02.
10) Fabric breadth shrinkage: shrinkage is (fabric width before dyeing-fabric width after dyeing)/fabric width before dyeing.
11) Wicking height: performed with reference to the standard AATCC-197.
The raw materials 1, 5-pentanediamine, polyamide 56 resin, polyamide 510 resin, and polyamide 512 resin used in the following examples were all available from Kaiser (Jinxiang) biomaterials Co., Ltd.
Example 1
(1) 1, 5-Pentanediamine and adipic acid were polymerized to form a melt of polyamide 56 having a relative viscosity of 2.7 at 96% sulfuric acid. The specific process is as follows:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; wherein the molar ratio of the 1, 5-pentanediamine to the adipic acid is 1.05: 1;
(1-2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 2.2MPa, exhausting, maintaining the pressure, reducing the pressure to 0MPa, and vacuumizing to-0.05 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system after the pressure maintaining is finished is 250 ℃, the temperature of the reaction system after the pressure reduction is finished is 275 ℃, and the temperature after the vacuum pumping is 280 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly is 16 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain fine denier high-strength low-shrinkage polyamide 56 fully-drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.5m/s, the air temperature is 19 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot rolling pair is 800m/min, the temperature is 65 ℃, and the winding number is 4 circles; the speed of the second pair of hot rollers is 1800m/min, the temperature is 150 ℃, and the winding number is 6 circles; the speed of the third pair of hot rollers is 2500m/min, the temperature is 180 ℃, and the number of winding turns is 5;
the winding speed was 2480 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
And (3) preparing polyamide 56 fiber spinning yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through a weaving 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 relative viscosity of 2.8 at 96% sulfuric acid. The specific process is as follows:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; wherein the molar ratio of 1, 5-pentanediamine to adipic acid is 1.08: 1;
(1-2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 2.4MPa, exhausting, maintaining the pressure, reducing the pressure to 0MPa, and vacuumizing to-0.04 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system after the pressure maintaining is finished is 255 ℃, the temperature of the reaction system after the pressure reduction is finished is 278 ℃, and the temperature after the vacuum pumping is 283 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning box body is 280 ℃, and the pressure of the spinning assembly is 13 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain fine denier high-strength low-shrinkage polyamide 56 fully-drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.52m/s, the air temperature is 20 ℃, and the humidity is 76%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3100m/min, the temperature is 65 ℃, and the winding number is 4 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 160 ℃, and the number of winding turns is 5; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the number of winding turns is 5 turns;
the winding speed was 4700 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
And (3) preparing polyamide 56 fiber spinning yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through a weaving process. The parameters of the prepared polyamide 56 fabric are shown in table 2.
Example 3
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.6 and a water content of 520 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 240 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 260 ℃, the temperature of the fourth zone is 270 ℃, and the temperature of the fifth zone is 280 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 282 ℃, and the pressure of the spinning assembly is 17 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.48m/s, the air temperature is 18 ℃, and the humidity is 82%;
the drawing process is drawing, and specifically comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 600m/min, the temperature is 70 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 1700m/min, the temperature is 145 ℃, and the winding number is 7 circles; the speed of the third pair of hot rollers is 2400m/min, the temperature is 190 ℃, and the number of winding turns is 6;
the winding speed was 2350 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
Example 4
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.7 and a water content of 600 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 285 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning manifold is 286 ℃, and the pressure of the spinning assembly is 14 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.47m/s, the air temperature is 19 ℃, and the humidity is 78%;
the drafting process is two-stage drafting, and specifically comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 900m/min, the temperature is 70 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 1800m/min, the temperature is 160 ℃, and the winding number is 7 circles; the speed of the third pair of hot rollers is 2800m/min, the temperature is 185 ℃, and the number of winding turns is 6;
the winding speed was 2750 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
Example 5
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.9 and a water content of 400 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, 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 290 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly is 17 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.52m/s, the air temperature is 21 ℃, and the humidity is 83%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 1500m/min, the temperature is 65 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 3500m/min, the temperature is 150 ℃, and the winding number is 6 circles; the speed of the third pair of hot rollers is 3800m/min, the temperature is 170 ℃, and the number of winding turns is 6;
the winding speed was 3700 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
Example 6
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.8 and a water content of 500 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 285 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 284 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.55m/s, the air temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3000m/min, the temperature is 70 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 150 ℃, and the number of winding turns is 7; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the number of winding turns is 7 turns;
the winding speed was 4730 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained 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 polyamide 510 resin 96% sulfuric acid has a relative viscosity of 2.45 and a water content of 400 ppm; the screw is heated in five zones, 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 polyamide 510 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 260 ℃, and the pressure of the spinning assembly is 15 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 510 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.5m/s, the air temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot rolling pair is 800m/min, the temperature is 55 ℃, and the winding number is 4 circles; the speed of the second pair of hot rollers is 1800m/min, the temperature is 140 ℃, and the winding number is 8 circles; the speed of the third pair of hot rollers is 2700m/min, the temperature is 160 ℃, and the number of winding turns is 5;
the winding speed was 2650 m/min.
The parameters of the polyamide 510 fully drawn yarn obtained 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 polyamide 510 resin 96% sulfuric acid has a relative viscosity of 2.6 and a water content of 300 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 225 ℃, the temperature of the second zone is 240 ℃, the temperature of the third zone is 255 ℃, the temperature of the fourth zone is 260 ℃, and the temperature of the fifth zone is 255 ℃.
(2) Spraying the polyamide 510 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 258 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 510 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.45m/s, the air temperature is 18 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3000m/min, the temperature is 50 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 145 ℃, and the number of winding turns is 6; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the number of winding turns is 7 turns;
the winding speed was 4720 m/min.
The parameters of the polyamide 510 fully drawn yarn obtained are shown in Table 1.
Example 9
(1) Heating polyamide 512 resin to a molten state in a screw extruder to form a polyamide 512 melt; wherein the polyamide 512 resin contains 96% sulfuric acid with relative viscosity of 2.6 and water content of 450 ppm; the screw is heated in five zones, 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 polyamide 512 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form a primary yarn; wherein the temperature of the spinning manifold is 250 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 512 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.48m/s, the air temperature is 22 ℃, and the humidity is 80%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 700m/min, the temperature is 50 ℃, and the winding number is 4 circles; the speed of the second pair of hot rollers is 1900m/min, the temperature is 135 ℃, and the winding number is 7 circles; the speed of the third pair of hot rollers is 2800m/min, the temperature is 180 ℃, and the number of winding turns is 5 turns;
the winding speed was 2780 m/min.
The parameters of the polyamide 512 fully drawn yarn obtained are shown in Table 1.
Example 10
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.8 and a water content of 500 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 285 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 284 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.55m/s, the air temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3000m/min, the temperature is 70 ℃, and the winding number is 3 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 150 ℃, and the number of winding turns is 4; the speed of the third pair of hot rollers is 4750m/min, the temperature is 180 ℃, and the number of winding turns is 3; the winding speed was 4730 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
Example 11
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.8 and a water content of 500 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 285 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 284 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.55m/s, the air temperature is 20 ℃, and the humidity is 75%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3000m/min, the temperature is 40 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 100 ℃, and the number of winding turns is 7; the speed of the third pair of hot rollers is 4750m/min, the temperature is 130 ℃, and the number of winding turns is 7 turns; the winding speed was 4730 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained 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 relative viscosity of 2.8 at 96% sulfuric acid. The specific process is as follows:
(1-1) under the condition of nitrogen, uniformly mixing 1, 5-pentanediamine, adipic acid and water to prepare a salt solution of polyamide; wherein the molar ratio of 1, 5-pentanediamine to adipic acid is 1.08: 1;
(1-2) heating the salt solution of polyamide, increasing the pressure in the reaction system to 2.4MPa, exhausting, maintaining the pressure, reducing the pressure to 0MPa, and vacuumizing to-0.04 MPa to obtain a polyamide 56 melt; wherein the pressures are gauge pressures; the temperature of the reaction system after the pressure maintaining is finished is 255 ℃, the temperature of the reaction system after the pressure reduction is finished is 278 ℃, and the temperature after the vacuum pumping is 283 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning box body is 280 ℃, and the pressure of the spinning assembly is 13 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.52m/s, the air temperature is 20 ℃, and the humidity is 76%;
the drafting is a first-level drafting, which comprises the following steps: feeding the oiled as-spun yarn into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 3100m/min, the temperature is 65 ℃, and the winding number is 4 circles; the speed of the second pair of hot rollers is 4800m/min, the temperature is 160 ℃, and the number of winding turns is 5;
the winding speed was 4700 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
And (3) preparing polyamide 56 fiber spinning yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through a weaving process. The parameters of the prepared polyamide 56 fabric are shown in table 2.
Comparative example 2
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.3 and a water content of 600 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 245 ℃, the temperature of the second zone is 265 ℃, the temperature of the third zone is 275 ℃, the temperature of the fourth zone is 285 ℃, and the temperature of the fifth zone is 285 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning manifold is 286 ℃, and the pressure of the spinning assembly is 14 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.47m/s, the air temperature is 19 ℃, and the humidity is 78%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 900m/min, the temperature is 70 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 1800m/min, the temperature is 160 ℃, and the winding number is 7 circles; the speed of the third pair of hot rollers is 2800m/min, the temperature is 185 ℃, and the number of winding turns is 6; the winding speed was 2750 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained are shown in Table 1.
And (3) preparing polyamide 56 fiber spinning yarns from the prepared polyamide 56 fully drawn yarns through a spinning process, and preparing the polyamide 56 fabric through a weaving process. The parameters of the prepared polyamide 56 fabric are shown in table 2.
Comparative example 3
(1) Heating polyamide 56 resin to a molten state in a screw extruder to form a polyamide 56 melt; wherein the polyamide 56 resin 96% sulfuric acid has a relative viscosity of 2.6 and a water content of 1300 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 240 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 260 ℃, the temperature of the fourth zone is 270 ℃, and the temperature of the fifth zone is 280 ℃.
(2) Spraying the polyamide 56 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 282 ℃, and the pressure of the spinning assembly is 17 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 56 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by cross air blow, the air speed of the cross air blow is 0.48m/s, the air temperature is 18 ℃, and the humidity is 82%;
the drafting is two-stage drafting, which comprises the following steps: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, performing secondary drafting between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 600m/min, the temperature is 70 ℃, and the winding number is 5 circles; the speed of the second pair of hot rollers is 1700m/min, the temperature is 145 ℃, and the winding number is 7 circles; the speed of the third pair of hot rollers is 2400m/min, the temperature is 190 ℃, and the number of winding turns is 6; the winding speed was 2350 m/min.
The parameters of the polyamide 56 fully drawn yarn obtained 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 polyamide 510 resin 96% sulfuric acid has a relative viscosity of 2.6 and a water content of 300 ppm; the screw is heated in five zones, wherein the temperature of the first zone is 225 ℃, the temperature of the second zone is 240 ℃, the temperature of the third zone is 255 ℃, the temperature of the fourth zone is 260 ℃, and the temperature of the fifth zone is 255 ℃.
(2) Spraying the polyamide 510 melt obtained in the step (1) through a spinneret plate of a spinning manifold to form primary yarns; wherein the temperature of the spinning beam is 258 ℃, and the pressure of the spinning assembly is 12 MPa.
(3) Cooling, oiling, drafting, heat setting and winding the primary yarn obtained in the step (2) to obtain polyamide 510 fully drawn yarn;
wherein the cooling in the step (3) is air cooling by side blowing, the air speed of the side blowing is 0.45m/s, the air temperature is 18 ℃, and the humidity is 75%;
the drafting is a first-level drafting, which comprises the following steps: feeding the oiled as-spun yarn into a first pair of hot rollers through a godet roller, performing primary drafting between the first pair of hot rollers and a second pair of hot rollers, and performing tension heat setting;
the speed of the first hot roller is 2800m/min, the temperature is 50 ℃, and the number of winding turns is 5; the speed of the second pair of hot rollers is 4200m/min, the temperature is 145 ℃, and the number of winding turns is 6 turns;
the winding speed was 4720 m/min.
The parameters of the polyamide 510 fully drawn yarn obtained are shown in Table 1.
TABLE 1 Polyamide 5X fully drawn yarn parameters prepared in examples and comparative examples
It can be seen from table 1 that the high-power drafting and high-temperature heat setting are realized by adopting two-stage drafting of three pairs of hot rollers and controlling the speed, temperature and other parameters of the hot rollers, the civil polyamide 5X filament with fine denier, high strength and low shrinkage is prepared, the problems of low strength and large shrinkage in boiling water of the fine denier polyamide 5X fiber are solved, and the fiber yield is improved by optimizing the spinning process.
Table 2 parameters of polyamide 5X facing prepared in examples and comparative examples
As can be seen from Table 2, the color fastness of the fabric of the present application in example 1 and example 2 is higher than that of the comparative example 1 and example 2, and the higher color fastness enables the fabric product to be less prone to falling off and fading of the pigment on the fabric when the fabric product is exposed to rain, sweat or light during wearing. The low width shrinkage rate of the fabric indicates that the shrinkage degree of the fabric after high-temperature dyeing is small, and the production cost is greatly reduced. The wicking height is higher in both the length direction and the width direction, so that the moisture absorption and sweat releasing functions of the fabric product are excellent, and the fabric is particularly suitable for application to underwear, shirts, suits, yoga coats, down coats, outdoor jackets, socks and the like.
Unless otherwise defined, all terms used herein have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of the present invention, and those skilled in the art may make various other substitutions, alterations, and modifications within the scope of the present invention, and thus, the present invention is not limited to the above-described embodiments but only by the claims.
Claims (10)
1. The monofilament dpf of the polyamide 5X fully drawn yarn is less than or equal to 4, further less than or equal to 3, further less than or equal to 2, and further 0.5-2;
preferably, the breaking strength is 5.5 to 8.5cN/dtex, further can be 5.8 to 8.3cN/dtex, further can be 6.0 to 7.8cN/dtex, further can be 6.3 to 7.5 cN/dtex;
preferably, the boiling water shrinkage is less than or equal to 10%, further more preferably less than or equal to 8%, further more preferably less than or equal to 7%, further more preferably less than or equal to 6%;
preferably, the elongation at break is less than or equal to 50%, further more preferably less than or equal to 45%, still further more preferably less than or equal to 40%, further more preferably less than or equal to 35%;
preferably, the initial modulus is 15-40 cN/dtex, further can be 18-35 cN/dtex, further can be 20-30 cN/dtex, further can be 23-28 cN/dtex;
preferably, the dyeing uniformity (gray card) is more than or equal to 3.5 grade, further more than or equal to 4.0 grade, further more than or equal to 4.5 grade, further more than or equal to 5.0 grade;
preferably, the dyeing double A rate is more than or equal to 94 percent, further more than or equal to 96 percent, further more than or equal to 98 percent, further more than or equal to 99 percent;
preferably, the yield is not less than 94%, more preferably not less than 95%, still more preferably not less than 96%, and still more preferably not less than 98%.
2. The polyamide 5X fully drawn yarn according to claim 1, wherein the polyamide 5X is obtained by polymerizing 1, 5-pentanediamine and a dicarboxylic acid; the dicarboxylic acid is saturated or unsaturated straight-chain aliphatic dicarboxylic acid containing 4-18 carbon atoms;
preferably, 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.
3. The polyamide 5X fully drawn yarn according to claim 1, comprising an additive including any one or more of a delustrant, 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 presence of a gas in the gas,
the mass of the additive accounts for 0.001-5% of the total mass of the raw materials for producing the polyamide 5X fully drawn yarn.
4. A preparation method of polyamide 5X fully drawn yarn comprises the steps of carrying out drawing 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 rollers, wherein the speeds of the three pairs of hot rollers are 300-5500 m/min respectively;
preferably, the stretching treatment comprises cooling, oiling, two-stage drafting, heat setting and winding forming which are sequentially carried out;
preferably, the three pairs of heat rolls include a first pair of heat rolls, a second pair of heat rolls, and a third pair of heat rolls; the speed of the first pair of hot rollers is 300-3500 m/min, the speed of the second pair of hot rollers is 1200-5000 m/min, and the speed of the third pair of hot rollers is 2000-5500 m/min.
5. The method of claim 4, comprising polymerizing 1, 5-pentanediamine and a dicarboxylic acid to form the polyamide 5X melt; alternatively, the first and second electrodes may be,
heating a polyamide 5X resin to a molten state to form the polyamide 5X melt;
preferably, the polyamide 5X resin has a relative viscosity of 96% sulfuric acid of 2.4 to 3.0, more preferably 2.5 to 2.9, still more preferably 2.6 to 2.8; the water content is 200-1000 ppm, further 300-900 ppm, further 400-800 ppm, further preferably 500-600 ppm; and/or the presence of a gas in the gas,
heating the polyamide 5X resin in a screw extruder to a molten state, wherein the screw extruder is divided into five zones for heating, the temperature of the first zone is 200-260 ℃, the temperature of the second zone is 230-280 ℃, the temperature of the third zone is 240-290 ℃, the temperature of the fourth zone is 240-300 ℃, and the temperature of the fifth zone is 250-290 ℃;
preferably, the polyamide 5X melt is sprayed out through a spinneret plate of a spinning manifold to form the raw silk; the temperature of the spinning manifold is 250-295 ℃, further can be 255-290 ℃, further can be 260-288 ℃, further can be 265-285 ℃; the pressure of a spinning assembly of the spinning manifold is 10-25 MPa, further can be 12-23 MPa, and further can be 14-20 MPa.
6. The method of claim 4, comprising: mixing 1, 5-pentanediamine, dicarboxylic acid and water to prepare a polyamide 5X salt solution; and
heating the polyamide 5X salt solution, raising the pressure in the system to 0.3-2.5 MPa, exhausting, maintaining the pressure, reducing the pressure to 0-0.2 MPa, and vacuumizing to the vacuum degree of-0.01-0.08 MPa to obtain the polyamide 5X melt; the pressures are gage pressures;
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 pressure reduction is finished is 240-280 ℃;
the temperature of the system after vacuumizing is 260-285 ℃.
7. The process of claim 4, wherein the two stage drawing comprises feeding the as-spun filament first through a godet roll to the first pair of hot rolls, performing a one stage drawing between the first pair of hot rolls and the second pair of hot rolls, and then performing a two stage drawing between the second pair of hot rolls and the third pair of hot rolls.
8. A process as claimed in claim 7, wherein the first pair of hot rolls has a speed of 550 to 1700m/min, further 600 to 1600m/min, the second pair of hot rolls has a speed of 1500 to 2400m/min, further 1600 to 2300m/min, and the third pair of hot rolls has a speed of 2300 to 3300m/min, further 2400 to 3200 m/min;
or the speed of the first pair of hot rollers is 2900-3400 m/min, further 2950-3300 m/min, the speed of the second pair of hot rollers is 3600-4900 m/min, further 4000-4850 m/min, and the speed of the third pair of hot rollers is preferably 3750-4850 m/min, further 3800-4800 m/min;
the temperature of the first hot rolling pair is 50-100 ℃, further 55-90 ℃, further 60-80 ℃; the number of winding turns of the first hot roller is 4-8, further 4-7, further 4-6;
the temperature of the second pair of hot rollers is 130-180 ℃, further 140-170 ℃, further 150-160 ℃; the number of winding turns of the second pair of hot rollers is 5-10, further 5-8 and further 5-7;
the temperature of the third pair of hot rollers is 150-220 ℃, further 160-190 ℃, further 170-180 ℃; the number of winding turns of the third pair of hot rollers is 4-10, further 5-7, further 5-6.
9. The method according to claim 4, wherein the cooling is performed by air cooling with cross-blown air or circular-blown air, and the air speed of the cross-blown air or the circular-blown air is 0.4-0.9 m/s, and further 0.5-0.8 m/s; the air temperature of the cross air blow or the circular air blow is 15-25 ℃, further 16-22 ℃, further 18-20 ℃; the humidity of the cross air blowing or the circular air blowing is 60-85%, and further can be 65-75%.
10. Use of a polyamide 5X fully drawn yarn according to any one of claims 1 to 3 or of a polyamide 5X fully drawn yarn obtained by a process according to any one of claims 4 to 9 in knitted or woven fabrics;
preferably, the knitted fabric wicking height (30 min): the length direction is more than or equal to 150mm, and the width direction is more than 160 mm; the width shrinkage rate of the fabric is less than 8 percent, and more preferably less than or equal to 4 percent; the color fastness of the fabric after washing is more than 3.5 grade, and preferably more than or equal to 4 grade; the color fastness to sunlight of the fabric is more than 3.0 grade, and preferably more than or equal to 4 grade;
preferably, the knitted and woven fabric is used for underwear, shirts, suits, yoga suits, down jackets, outdoor jackets, socks, bags, curtains, shoe materials, embroidery threads, trademarks, sofa cloth, elastic bands, combat uniforms, wedding dresses, leisure jackets, outdoor tents, tools, sportswear, sleeping bags or mountain bikes.
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