CN115704117A - Polyamide fiber and preparation method thereof - Google Patents
Polyamide fiber and preparation method thereof Download PDFInfo
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- CN115704117A CN115704117A CN202110921212.3A CN202110921212A CN115704117A CN 115704117 A CN115704117 A CN 115704117A CN 202110921212 A CN202110921212 A CN 202110921212A CN 115704117 A CN115704117 A CN 115704117A
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 136
- 229920002647 polyamide Polymers 0.000 title claims abstract description 136
- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920006141 Polyamide 5X Polymers 0.000 claims abstract description 58
- 238000009987 spinning Methods 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 46
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 42
- 239000011347 resin Substances 0.000 claims abstract description 41
- 229920005989 resin Polymers 0.000 claims abstract description 41
- 239000000178 monomer Substances 0.000 claims abstract description 33
- 238000010583 slow cooling Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000155 melt Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000004804 winding Methods 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 55
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 19
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 8
- 239000001361 adipic acid Substances 0.000 claims description 6
- 235000011037 adipic acid Nutrition 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 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
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000007599 discharging Methods 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
- 230000002401 inhibitory effect Effects 0.000 claims description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 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
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-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
- 238000005507 spraying Methods 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
- 239000011261 inert gas Substances 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
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 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
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000000126 substance Substances 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
- 239000012620 biological material Substances 0.000 claims 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 238000004043 dyeing Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
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- 208000012886 Vertigo Diseases 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229920006122 polyamide resin Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 239000012632 extractable Substances 0.000 description 3
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- 238000005259 measurement Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 2
- 241001589086 Bellapiscis medius Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
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- 230000008018 melting Effects 0.000 description 2
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- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 description 2
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- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Polyamides (AREA)
Abstract
The invention relates to the technical field of high polymer materials, and discloses a polyamide fiber and a preparation method thereof, wherein the method comprises the following steps: (a) Directly feeding the polyamide 5X melt into a spinning manifold through a melt booster pump, or heating polyamide 5X resin to a molten state to form a polyamide 5X melt, and feeding the polyamide 5X melt into the spinning manifold; (b) The polyamide 5X melt is accurately metered by a metering pump, is sprayed out by a spinneret plate to form melt trickle, simultaneously, oligomer is removed by adopting saturated superheated steam, slow cooling and a monomer suction device, and then, the polyamide fiber is obtained through cooling, oiling and winding. According to the invention, by adding the saturated superheated steam device, the slow cooling device and the monomer suction device, the oligomer is less, the length of a shovel plate of the component is long, the yarn breaking frequency is less, the obtained polyamide fiber has less broken yarn, the yarn evenness of the fiber is low, the dyeing dark lines are less, the dyeing effect is good, and the polyamide fiber has excellent elongation at break, breaking strength and lower boiling water shrinkage.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyamide fiber and a preparation method thereof.
Background
Polyamides have been widely used as clothing, industrial materials, fibers, or general engineering plastics, and other many applications due to their excellent characteristics and ease of melt molding, and thus have received much attention. In the process of polyamide polymerization, because of cyclization reaction, a polymer macromolecular chain is broken into two sections when the chain lactam group exchange reaction occurs, or linear low molecular weight substances are directly subjected to dehydration reaction, so that a low molecular weight polymer, short for oligomer, is generated. Generally, oligomers are low molecular weight polymers ranging from mono-to decamers, including linear oligomers and cyclic oligomers.
Usually, the oligomer cannot be processed and shaped independently, and if a large amount of oligomer enters a spinning section along with chips, not only serious consequences are caused to the spinning process, but also great waste of raw materials is caused. The oligomer is mainly cyclic, and if the content of the dimer and the trimer after extraction is higher, the viscosity, the number average molecular weight and the molecular weight distribution of the slices are influenced, so that a series of negative effects such as strength reduction of the protofilament and increase of the waste silk rate are caused. The high content of low molecular extractables in the polymer not only vaporizes from the melt into gas and deteriorates the spinning environment, but also the residual low molecular extractables form "weak spots" in the fiber, which are easily broken by external force (such as drawing) and cause difficulty in spinning during melt spinning. In addition, low-molecular extractables are also easily precipitated on the surface of the filaments, thereby increasing the number of broken filaments and filaments during drawing and decreasing the strength of the finished filaments.
The polyamide 5X is a linear long-chain macromolecule synthesized by bio-based pentanediamine and dibasic acid, and amido bonds are easy to form hydrogen bonds, so that the polyamide 5X fiber has high strength and good hygroscopicity, and the moisture regain of the fiber can reach 2.0-5.5%. However, volatilization of oligomers in polyamide 5X increases bubbles in the melt of polyamide 5X and reduces the blade cycle of the spinning pack, thereby causing undesirable phenomena such as filament floating, filament breakage and low yield during melt spinning. Therefore, how to improve the unfavorable phenomena of filament floating, filament breakage, low yield and the like of polyamide 5X in the spinning process is an urgent problem to be solved in the prior art.
Disclosure of Invention
The invention provides a polyamide fiber and a preparation method thereof, aiming at solving the defects of the prior art and products, namely solving the problems of short period of a shovel plate of a spinning component, more floating filaments and broken filaments and low support rate caused by more oligomer precipitation in the polyamide 5X spinning process.
In order to solve the above problems, the present invention provides a polyamide fiber having a breaking strength of 3.5 to 9.5cN/dtex, further 3.6 to 9.0cN/dtex, further 3.7 to 8.5cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide fiber is 15 to 90 percent, further 18 to 80 percent, and further 22 to 60 percent; and/or the presence of a gas in the gas,
the boiling water shrinkage of the polyamide fiber is 3-12%, further 4-11%, further 5-10%; and/or the presence of a gas in the gas,
the evenness unevenness of the polyamide fiber is less than or equal to 1.5 percent, further less than or equal to 1.3 percent, and further less than or equal to 1.1 percent; and/or the presence of a gas in the gas,
the polyamide fiber comprises undrawn yarn, pre-oriented yarn, medium-oriented yarn, high-oriented yarn, textured yarn, fully drawn yarn, industrial yarn, continuous bulked continuous yarn, short fiber and monofilament fiber.
In a second aspect, the present invention provides a process for preparing a polyamide fibre according to the first aspect of the invention, which process comprises:
(a) Directly feeding the polyamide 5X melt into a spinning manifold through a melt booster pump, or heating the polyamide 5X resin to a molten state to form the polyamide 5X melt, and then feeding the polyamide 5X melt into the spinning manifold;
(b) The polyamide fiber is prepared by accurately metering a polyamide 5X melt by a metering pump, spraying the melt by a spinneret plate to form melt trickle, removing polyamide oligomer in the melt trickle by a saturated superheated steam device, a slow cooling device and a monomer suction device, and then cooling, oiling and winding the melt.
Compared with the prior art, the implementation of the invention has at least the following advantages:
1. the polyamide 5X resin synthesized by the method has proper oligomer, viscosity, water content and terminal amino group, does not need the procedures of polymerization deashing and extraction for removing the oligomer, can be directly spun, and reduces the production cost.
2. The polyamide 5X fiber is prepared by adding saturated superheated steam and modifying a slow cooling and monomer suction device. The spinning process has the advantages of less oligomer, long period of a component shovel plate and less yarn breaking times, the obtained polyamide 5X fiber has less broken yarn, low yarn evenness rate of the fiber, less dark dyeing lines and good dyeing effect, and the fiber has excellent elongation at break, breaking strength and lower boiling water shrinkage. The spinning and dyeing yield is high.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
As described above, the first aspect of the present invention provides a polyamide fiber, the polyamide fiber has a breaking strength of 3.5 to 9.5cN/dtex, further 3.6 to 9.0cN/dtex, further 3.7 to 8.5cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide fiber is 15 to 90 percent, further 18 to 80 percent, and further 22 to 60 percent; and/or the presence of a gas in the atmosphere,
the boiling water shrinkage of the polyamide fiber is 3-12%, further 4-11%, further 5-10%; and/or the presence of a gas in the gas,
the yarn evenness rate of the polyamide fiber is less than or equal to 1.5 percent, further less than or equal to 1.3 percent, and further less than or equal to 1.1 percent; and/or the presence of a gas in the gas,
the fiber comprises the polyamide fiber, wherein the polyamide fiber comprises undrawn yarn, pre-oriented yarn (POY), middle Oriented Yarn (MOY), high Oriented Yarn (HOY), textured yarn (DTY), fully Drawn Yarn (FDY), industrial yarn (IDY), continuous Bulked Continuous Filament (BCF), short fiber and monofilament fiber.
In some embodiments of the invention, the polyamide fibers have a yield of 93% or more, further 94% or more, and further 95% or more.
In some embodiments of the present invention, the number of filament breaks of the polyamide fiber is less than or equal to 2 (number/24 h), further less than or equal to 1 (number/24 h), and further less than or equal to 0 (number/24 h).
In some embodiments of the invention, the number of filaments of the polyamide fiber is 2 or less (per 9 kg package), further 1 or less (per 9 kg package), and still further 0 or less (per 9 kg package).
In some embodiments of the invention, the polyamide fibers have a dyeing M-ratio of 93% or more, further 94% or more, and further 95% or more.
In a second aspect, the present invention provides a process for preparing a polyamide fibre as hereinbefore described, which process comprises:
(a) Directly feeding the polyamide 5X melt into a spinning manifold through a melt booster pump, or heating polyamide 5X resin to a molten state to form a polyamide 5X melt, and then feeding the polyamide 5X melt into the spinning manifold;
(b) The polyamide fiber is prepared by accurately metering a polyamide 5X melt by a metering pump, spraying the melt by a spinneret plate to form melt trickle, removing polyamide oligomer in the melt trickle by a saturated superheated steam device, a slow cooling device and a monomer suction device, and then cooling, oiling and winding the melt.
According to a preferred embodiment of the present invention, the method for removing the polyamide oligomer by using the saturated superheated steam device, the slow cooling device and the monomer suction device comprises the following steps: the method is characterized in that a saturated superheated steam device is arranged in a spinning box body, the saturated superheated steam entering the spinning box body is reheated by the box body and then sprayed from the periphery below a spinneret plate, polyamide oligomer overflowing from spinneret orifices and fiber surfaces of the spinneret plate is dissolved in the saturated superheated steam, meanwhile, a slow cooling device is arranged below the spinneret plate and used for increasing slow cooling temperature and inhibiting crystallization of the polyamide oligomer, the oligomer is prevented from forming white flocculent crystals in the spinneret plate and below the spinneret plate, the spinneret plate and the below of the spinneret plate are kept clean, then the polyamide oligomer dissolved in the saturated superheated steam is taken away through monomer suction, a monomer suction cover in a monomer suction device has an automatic constant temperature heating function, the oligomer is ensured not to be crystallized at an inlet of the suction cover, the polyamide oligomer is effectively prevented from polluting the spinneret plate, the below the spinneret plate and the inlet of the monomer suction cover, the shovel plate period of a spinning assembly is prolonged, the phenomena of head spinning and filament breakage caused by the oligomer in the spinning process are reduced, and the spinning production stability and the production rate are improved.
In some embodiments of the invention, the saturated superheated steam prior to entering the spinning beam has a temperature of from 80 ℃ to 200 ℃, further from 90 ℃ to 180 ℃, further from 100 ℃ to 160 ℃.
In some embodiments of the invention, the pressure of the saturated superheated steam prior to entering the spinning beam is between 0.8 and 2.2bar, further between 1.0 and 2.0bar, and further between 1.2 and 1.8bar.
In some embodiments of the invention, the slow cooling temperature is 180 to 320 ℃, further 220 to 300 ℃, further 240 to 280 ℃.
In some embodiments of the invention, the slow cooling height is ≦ 5cm, further ≦ 4cm, and further ≦ 3cm.
In some embodiments of the invention, the monomer is pumped at a pressure of 0.6MPa or more, further 0.65MPa or more, and still further 0.7MPa or more.
In some embodiments of the invention, the monomer extraction hood has a temperature of 100 to 260 ℃, further 120 to 230 ℃, and further 140 to 200 ℃.
In some embodiments of the invention, the diameter of the spinneret is 88mm or less, more preferably 77mm or less, and still more preferably 66mm or less.
According to some embodiments of the present invention, the shovel cycle of the assembly during the preparation of the polyamide fiber is greater than or equal to 16h, further greater than or equal to 18h, and further greater than or equal to 20h.
The apparatus and operating conditions for cooling, oiling and winding in step (b) are not particularly limited in the present invention, and conventional operations in the art can be adopted, and those skilled in the art can select the cooling, oiling and winding according to actual conditions.
In some embodiments of the invention, the polyamide 5X resin comprises 1,5-pentamethylenediamine structural units and dibasic acid structural units, the polyamide 5X resin contains a polyamide oligomer having a number average molecular weight of 2000 or less, and the content of the polyamide oligomer is 1.0wt% or less.
According to some embodiments of the invention, the polyamide 5X resin has a number average molecular weight of 2000 or more. The number average molecular weight is calculated from the elution curve of each sample obtained under the measurement conditions of the examples described later, using gel permeation chromatography (hereinafter abbreviated as GPC), from the area of the region surrounded by the baseline and the elution curve and ranging from the number average molecular weight of 2000 or more to the molecular weight of not more than the molecular weight at which the detection of the main peak is completed, and is obtained by conversion to standard polymethyl methacrylate (standard PMMA).
The polyamide resin of the present invention contains a polyamide oligomer having a number average molecular weight of 2000 or less, which is determined by GPC measurement under the same conditions as described above.
According to some embodiments of the invention, the polyamide oligomer is present in an amount of 0.95wt% or less, further 0.9wt% or less.
In some preferred embodiments of the invention, the pentanediamine may be chemically or biologically derived, and further is biologically derived 1,5-pentanediamine.
In some preferred embodiments of the invention, greater than 90mol% of the diacid building blocks are from adipic acid.
According to some embodiments of the invention, the diacid structural units of the polyamide 5X resin further comprise one or more from the group consisting 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, and octadecanedioic acid, terephthalic acid, isophthalic acid, phthalic acid.
According to some embodiments of the invention, the polyamide oligomer is selected from at least one of the following structures:
wherein n1 and n2 are respectively selected from integers of 1-8; preferably, n1 and n2 are each selected from integers of 1 to 6; more preferably, n1 and n2 are each independently an integer of 1 to 5; further preferably, n1 is 2, 3 or 4; n2 is 2, 3, 4 or 5;
m1 and m2 are each an integer of 2 to 18; preferably, m1 and m2 are each independently an integer of 4 to 16; further preferably, m1 is 4, 8 or 10 and m2 is 4, 8 or 10.
According to some embodiments of the invention, the polyamide 5X resin comprises a first polyamide having a structure according to formula I:
the number average molecular weight of the first polyamide is 2000 or more, and the content of the first polyamide in the polyamide 5X resin is 85wt% or more, further 90wt% or more, and further 95wt% or more. For example, the polyamide 5X resin has a first polyamide content of 99 to 99.98wt%.
In some embodiments of the invention, the polyamide 5X resin has a relative viscosity of 2.3 to 3.6, preferably 2.4 to 3.5, and more preferably 2.5 to 3.4.
In some embodiments of the invention, the polyamide 5X resin has a water content of 300 to 900ppm, preferably 350 to 800ppm, and more preferably 400 to 700ppm.
In some embodiments of the invention, the polyamide 5X resin has a terminal amino group content of 40 to 70mol/ton, preferably 43 to 60mol/ton, more preferably 45 to 55mol/ton.
According to some embodiments of the invention, the method of preparing the polyamide 5X resin comprises:
(1) Uniformly mixing 1,5-pentamethylene diamine, dibasic acid and water in an inert gas atmosphere to prepare a salt solution of polyamide;
(2) Heating the salt solution of polyamide, raising the pressure in the reaction system to 0.5-2.4 MPa, exhausting and maintaining the pressure, reducing the pressure to 0-0.2 MPa when the pressure maintaining is finished, and vacuumizing to obtain polyamide 5X melt, wherein the temperature of the reaction system is 235-268 ℃ after the pressure maintaining is finished, and the temperature of the reaction system is 248-282 ℃ after the pressure reducing is finished;
(3) Discharging the melt obtained in the step (2), and carrying out bracing and dicing.
In some embodiments of the invention, in step (1), the molar ratio of 1,5-pentanediamine to diacid is (1 to 1.08): 1.
in some embodiments of the present invention, in the step (2), the vacuum is applied so that the relative vacuum degree in the reaction system is from-0.02 MPa to-0.08 MPa.
In some embodiments of the invention, the vacuum is maintained for 18 to 70min.
In some embodiments of the invention, the vacuum termination temperature is controlled to be 263 to 278 ℃.
In some embodiments of the invention, in step (3), the pelletizing is carried out in water at a temperature of 15 to 50 ℃.
The inert gas in the step (1) of the invention is selected from one or more of nitrogen, argon, helium and the like, and is preferably selected from one or more of high-purity nitrogen, high-purity argon and high-purity helium.
The types of the dibasic acids are as described above, and are not described in detail herein.
All pressures stated herein are expressed as gauge pressure unless otherwise specified.
The present invention will be described in detail below by way of examples. In the following examples, various raw materials used are commercially available without specific description.
1. Method for detecting relative viscosity eta r
Concentrated sulfuric acid method with Ubbelohde viscometer: the dried polyamide sample was accurately weighed at 0.5. + -. 0.0002g, dissolved by adding 50mL of concentrated sulfuric acid (96%), and the concentrated sulfuric acid flow time t0 and the polyamide solution flow time t were measured and recorded in a thermostatic water bath at 25 ℃.
Relative viscosity calculation formula:
relative viscosity η r = t/t0
Wherein: t: the time of solution flow; t0: the solvent was run through time.
2. Water content ratio
Taking 1g of resin sample, and measuring by using a Karl Fischer moisture tester, wherein the detection temperature is 200 ℃, and the detection time is 20min.
3. Determination of the content of terminal amino groups
After the sample is dissolved by using trifluoroethanol, titrating by using hydrochloric acid standard solution and sodium hydroxide standard solution respectively, and calculating.
4. The molecular weight detection method comprises the following steps:
from the elution curve (vertical axis: signal intensity by detector, horizontal axis: elution time) of each sample obtained by using Gel Permeation Chromatography (GPC), the number average molecular weight of the main peak (polymer peak) in the elution curve was calculated by calibration from a standard sample of polymethyl methacrylate (PMMA).
The measurement was performed under the following conditions.
A detector: RI detector
A chromatographic column: 2 × PSS 7 μ PFG Linear M column 300 × 8.0mm solvent: hexafluoroisopropanol containing sodium trifluoroacetate at a concentration of 0.05 mol/L.
Temperature: 40 deg.C
Flow rate: 1mL/min
Injection amount: 100 μ L
Concentration: 3 to 5g/L
Sample preparation: the polyamide resin or the polyamide resin composition obtained in each example and the like was weighed in hexafluoroisopropanol containing 0.01 mol/L of sodium trifluoroacetate so as to be 0.5mg/mL in terms of the polyamide resin, and dissolved by stirring at room temperature for 1 hour, and the resulting solution was filtered through a hydrophobic membrane filter (pore size: 0.22 μm) to prepare a sample.
PMMA standard: a STANDARD elution curve (calibration curve) was prepared using STANDARD81506-1EA (number average molecular weight range: 500 to 27000000) prepared by Fluka.
5. The detection method of the content of the polyamide oligomer comprises the following steps:
drying a polyamide sample in a forced air oven at 130 ℃ for 7 hours, then placing the polyamide sample into an aluminum-plastic bag, sealing the opening of the aluminum-plastic bag, then placing the aluminum-plastic bag into a dryer for cooling, then accurately weighing about 2g of the polyamide sample, placing the polyamide sample into a 250mL round-bottom flask, adding 100mL purified water, heating and refluxing for 24 hours by using a heating jacket, taking the polyamide sample, washing the polyamide sample with the purified water for three times, drying the polyamide sample in the forced air oven at 130 ℃ for 7 hours, then transferring the polyamide sample into a pre-weighed aluminum-plastic bag, sealing the opening of the aluminum-plastic bag, then placing the polyamide sample into the dryer for cooling, weighing the total weight of the aluminum-plastic bag and the polyamide sample, subtracting the weight of the aluminum-plastic bag from the weight of the aluminum-plastic bag to obtain the weight of the polyamide sample after water boiling, and calculating the oligomer content by comparing the weight difference before and after water boiling of the polyamide sample. Each sample was tested in duplicate. When detecting the content of the oligomer in the melt, the melt is guided into a closed container, and after cooling, sampling is carried out to detect according to the method.
6. Elongation at break
Measured according to GB/T14344.
7. Breaking strength
Measured according to GB/T14344.
8. Shrinkage in boiling water
Measured according to GB/T6505-2008.
9. Number of filament breakage
Number of filament breakage (number of times/24 h): and (5) manual statistics. A lower number of filament breaks is considered to mean better spinnability.
10. Uneven evenness of evenness
The determination was carried out according to the method of GB/T14346-93.
11. Rate of formation of fibers
Production yield = (weight of finished fiber produced/total weight of charged resin) × 100%.
12. M rate
The dyeing uniformity of the polyamide fiber prepared by the above preparation method was measured by a dyeing uniformity method (astm z 7667-1999), and the M-ratio was measured by a 5-grade color discrimination standard method.
M rate = (dyeing uniformity is equal to or more than 4.5 grade fiber quantity)/total quantity of all dyed fibers) × 100%.
13. Number of broken filaments
The number of the broken filaments is manually judged.
Preparation example 1
(1) Uniformly mixing 1,5-pentamethylene diamine, adipic acid and water under the condition of nitrogen, wherein the mole ratio of 1,5-pentamethylene diamine to adipic acid is 1.05, and preparing 65wt.% of nylon salt solution, wherein the percentages are the mass percentages of the nylon salt solution; the pH at a nylon salt solution concentration of 10wt.% was 7.83.
(2) Heating the solution, increasing the pressure in the reaction system to 2.2MPa, taking 1 hour and 30 minutes, exhausting, maintaining the pressure at 2.42MPa, keeping the temperature of the reaction system at 250 ℃ when the pressure maintaining is finished, taking 3 hours when the pressure maintaining is finished, reducing the pressure to reduce the pressure in the reaction system to 0.002MPa (gauge pressure), taking 1 hour when the temperature of the reaction system is 270 ℃ after the pressure reducing is finished, and taking 1 hour when the pressure reducing is finished. And vacuumizing to maintain the relative vacuum degree in the reaction system at-0.05 MPa, wherein the vacuumizing time is 28min, and the temperature after vacuumizing is 273 ℃, so as to obtain the polyamide melt.
(3) Melting and discharging the melt obtained in the step (2), and bracing and dicing to obtain polyamide 56 resin; the granulation is carried out in water, the water temperature is 19 ℃, the rotating speed of a roller is 500rpm, and the granulation time is 23min.
Preparation example 2
(1) Uniformly mixing 1,5-pentanediamine, sebacic acid and water under the condition of nitrogen, wherein the molar ratio of 1,5-pentanediamine to sebacic acid is 1.07, and preparing 60wt.% of a nylon salt solution, wherein the percentages are in percentage by mass of the nylon salt solution; the pH at 10wt.% nylon salt solution concentration was 7.8.
(2) Heating the solution, increasing the pressure in the reaction system to 2.2MPa, taking 1 hour and 30 minutes, exhausting, maintaining the pressure at 2.4MPa, keeping the temperature of the reaction system at 245 ℃ when the pressure maintaining is finished, taking 3 hours when the pressure maintaining is finished, reducing the pressure to reduce the pressure in the reaction system to 0.002MPa (gauge pressure), taking 260 ℃ when the pressure reducing is finished, and taking 1 hour when the pressure reducing is finished. Vacuumizing to maintain the relative vacuum degree in the reaction system at-0.05 MPa for 25min, and controlling the temperature after vacuumizing to 268 ℃ to obtain the polyamide melt.
(2) Melting and discharging the melt obtained in the step (2), and bracing and dicing to obtain polyamide 510 resin; the granulation is carried out in water, the water temperature is 18 ℃, the rotating speed of a roller is 510rpm, and the granulation time is 25min.
Example 1
The polyamide 56 resin prepared in preparation example 1 was fed into a spinning apparatus through a feeder, heated by a single screw and uniformly distributed into a spinning pack at a spinning box temperature of 282 ℃. The melt is sprayed out through a spinneret plate to form melt fine flow, the diameter of the spinneret plate is 0.22mm, the length of the spinneret plate is 0.605mm, and the number of holes is 48. The method is characterized in that a saturated superheated steam device is arranged in a spinning box body, the saturated superheated steam entering the spinning box body is reheated by the box body and then sprayed into the spinning plate from the periphery below the spinneret plate, polyamide oligomer overflowing from spinneret orifices and fiber surfaces of the spinneret orifices is dissolved in the saturated superheated steam, a slow cooling device is arranged below the spinneret plate and used for increasing slow cooling temperature and inhibiting crystallization and separation of the polyamide oligomer, then the polyamide oligomer dissolved in the saturated superheated steam is taken away through monomer suction, a monomer suction cover in a monomer suction device has an automatic constant-temperature heating function, the temperature of the saturated superheated steam before entering the spinning box body is 120 ℃, the pressure of the saturated superheated steam before entering the spinning box body is 1.6bar, the slow cooling temperature is 250 ℃, the slow cooling height is 3cm, the pressure of the monomer suction is 0.65MPa, the temperature of the monomer suction cover is 150 ℃, and the diameter of the spinneret plate is 77mm. Then cooling and forming by a side blowing device, wherein the air temperature of the side blowing device is 18 ℃, the air humidity is 85 percent, and the air speed is 0.42m/s. And (3) oiling the cooled and formed filament bundle, drawing the filament bundle to a first filament guiding disc and a second filament guiding disc after a spinning channel, and winding the filament bundle into a spinning cake on a winding machine, wherein the speed of the first filament guiding disc is 4490m/mi, the speed of the second filament guiding disc is 4510m/mi, and the winding speed is 4500m/min, so that the polyamide 56 pre-oriented yarn (POY) is obtained.
Example 2
A polyamide 56 pre-oriented yarn (POY) was produced according to the same process as in example 1, except that the temperature of saturated superheated steam before entering the spinning beam was adjusted to 130 ℃.
Example 3
A polyamide 56 pre-oriented yarn (POY) was prepared according to the same process as in example 1, except that the slow cooling temperature was adjusted to 280 ℃.
Example 4
A polyamide 56 pre-oriented yarn (POY) was produced according to the same process as in example 1, except that the slow cooling height was adjusted to 2cm.
Example 5
Polyamide 56 pre-oriented yarn (POY) was produced by the same process as in example 1 except that the pressure under which the monomer was sucked was adjusted to 0.75MPa.
Example 6
A polyamide 510 pre-oriented yarn (POY) was produced by the same procedure as in example 1, except that the polyamide 510 resin produced in preparation example 2 was used in place of the polyamide 56 resin.
Comparative example 1
A polyamide 56 pre-oriented yarn (POY) was prepared according to the same process as in example 1, except that there was no saturated superheated steam device and slow cooling device.
Comparative example 2
A polyamide 56 pre-oriented yarn (POY) was prepared according to the same process as in example 1, except that there was no saturated superheated steam unit.
Comparative example 3
A polyamide 56 pre-oriented yarn (POY) was prepared according to the same process as in example 1, except that no slow cooling device was provided.
Comparative example 4
A polyamide 56 pre-oriented yarn (POY) was produced according to the same process as in example 1, except that the temperature of saturated superheated steam before entering the spinning beam was adjusted to 70 ℃.
Comparative example 5
A polyamide 56 pre-oriented yarn (POY) was prepared according to the same process as in example 1, except that the slow cooling temperature was adjusted to 150 ℃.
Comparative example 6
Polyamide 56 pre-oriented yarn (POY) was produced by the same procedure as in example 1, except that the slow cooling height was adjusted to 6cm.
Comparative example 7
Polyamide 56 pre-oriented yarn (POY) was produced by the same process as in example 1 except that the pressure under which the monomer was sucked was adjusted to 0.5MPa.
Comparative example 8
A polyamide 56 pre-oriented yarn (POY) was produced by the same process as in example 1, except that the diameter of the spinneret was adjusted to 95mm.
Comparative example 9
A polyamide 510 pre-oriented yarn (POY) was produced by the same procedure as in example 1, except that there were no saturated superheated steam device and slow cooling device, and that the polyamide 510 resin produced in preparation example 2 was used in place of the polyamide 56 resin.
Examples 7 to 12
Respectively passing the polyamide 56 pre-oriented yarn or the polyamide 510 pre-oriented yarn prepared in examples 1 to 6 through a yarn guide and a yarn cutter to a 1 st roller, carrying out hot drawing in a hot box, then carrying out cooling setting by adopting a cooling plate, obtaining a certain twist degree by a false twister, passing through a tension on-line detector, a 2 nd roller, then adding a network through a network nozzle, then oiling through a 3 rd roller, a yarn breaking sensor and a tanker, and finally winding to obtain the polyamide 56 textured yarn (DTY) or the polyamide 510 textured yarn (DTY). The processing speed was 600m/min, the draw ratio was 1.28, the D/Y ratio was 1.65 and the hot box temperature was 185 ℃.
Comparative examples 10 to 18
The polyamide 56 pre-oriented yarn or the polyamide 510 pre-oriented yarn prepared in comparative examples 1 to 9 was passed through a yarn guide, a yarn cutter to the 1 st roller, hot-drawn in a hot box, then cooled and set using a cooling plate, obtained a certain twist by a false twister, passed through a tension on-line detector, the 2 nd roller, then networked by a network nozzle, then oiled by a 3 rd roller, a yarn breakage sensor, an oil tanker, and finally wound to obtain polyamide 56 textured yarn (DTY) or polyamide 510 textured yarn (DTY). The processing speed was 600m/min, the draw ratio was 1.28, the D/Y ratio was 1.65 and the hot box temperature was 185 ℃.
Example 13
The polyamide 56 resin obtained in example 1 was fed into a spinning apparatus through a feeder and uniformly distributed into a spinning pack by single screw heating, the temperature of the spinning pack being 280 ℃. The melt is sprayed out through a spinneret plate to form melt fine flow, the diameter of the spinneret plate is 0.22mm, the length of the spinneret plate is 0.605mm, and the number of holes is 48. The method comprises the steps of arranging a saturated superheated steam device in a spinning box body, reheating the saturated superheated steam entering the spinning box body, spraying the reheated saturated superheated steam into the spinning plate from the periphery below a spinneret plate, dissolving polyamide oligomer overflowing from spinneret orifices and fiber surfaces of the spinneret orifices in the saturated superheated steam, arranging a slow cooling device below the spinneret plate for increasing slow cooling temperature and inhibiting crystallization of the polyamide oligomer, sucking and taking away the polyamide oligomer dissolved in the saturated superheated steam through a monomer, enabling a monomer suction cover in a monomer suction device to have an automatic constant-temperature heating function, enabling the temperature of the saturated superheated steam before entering the spinning box body to be 130 ℃, enabling the pressure of the saturated superheated steam before entering the spinning box body to be 1.5bar, enabling the slow cooling temperature to be 260 ℃, enabling the slow cooling height to be 3cm, enabling the pressure of monomer suction to be 0.6MPa, enabling the temperature of the monomer suction cover to be 120 ℃ and enabling the diameter of the spinneret plate to be 77mm. Then cooling and forming by a side blowing device, wherein the air temperature of the side blowing device is 20 ℃, the air humidity is 90 percent, and the air speed is 0.40m/s. After oiling and spinning the cooled and formed filament bundle, drawing the filament bundle to a first pair of cold rollers and a second pair of hot rollers, wherein the speed of the first pair of cold rollers is 2840m/min, the speed of the second pair of cold rollers is 4830m/min, the winding speed is 4800m/min, the drawing multiple is 1.7, and the setting temperature is 165 ℃, so that the polyamide 56 fully drawn Filament (FDY) is obtained.
Example 14
Polyamide 510 Fully Drawn Yarn (FDY) was produced by the same procedure as in example 13, except that the polyamide 510 resin obtained in production example 2 was used in place of the polyamide 56 resin obtained in production example 1.
Comparative example 19
Polyamide 56 Fully Drawn Yarn (FDY) was produced by the same process as in example 13, except that there was no saturated superheated steam unit and no slow cooling unit.
Comparative example 20
Polyamide 56 Fully Drawn Yarn (FDY) was prepared by the same procedure as in example 13, except that there was no saturated superheated steam unit.
Comparative example 21
Polyamide 510 Fully Drawn Yarn (FDY) was produced by the same procedure as in example 13, except that there was no saturated superheated steam device and that the polyamide 510 resin produced in production example 2 was used in place of the polyamide 56 resin.
TABLE 1 Polyamide 5X resin Performance test results Table
TABLE 2 Polyamide 5X POY fiber Performance test results Table
TABLE 3 Polyamide 5X DTY fiber test results Table
TABLE 4 Polyamide 5X FDY fiber test results Table
Tables 1 to 4 show that: according to the invention, by adding the saturated superheated steam, slow cooling and monomer suction devices, the polyamide 5X oligomer pollution spinneret plate, the spinneret plate lower part and the monomer suction hood inlet of the spinneret plate are effectively reduced in the spinning process, the shovel plate period of the spinning component is prolonged, the phenomena of head spinning and filament breakage caused by the oligomer in the spinning process are reduced, and the spinning production stability and the production rate are improved, so that the obtained polyamide 5X fiber has less broken filaments, low evenness of the fiber, less dark dyeing lines, good dyeing effect, excellent elongation at break, breaking strength, lower boiling water shrinkage and higher spinning and dyeing yield. The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. A polyamide fiber, characterized in that the breaking strength of the polyamide fiber is 3.5 to 9.5cN/dtex, further 3.6 to 9.0cN/dtex, further 3.7 to 8.5cN/dtex; and/or the presence of a gas in the gas,
the elongation at break of the polyamide fiber is 15 to 90 percent, further 18 to 80 percent, and further 22 to 60 percent; and/or the presence of a gas in the gas,
the boiling water shrinkage of the polyamide fiber is 3-12%, further 4-11%, further 5-10%; and/or the presence of a gas in the gas,
the yarn evenness rate of the polyamide fiber is less than or equal to 1.5 percent, further less than or equal to 1.3 percent, and further less than or equal to 1.1 percent; and/or the presence of a gas in the gas,
the polyamide fiber comprises undrawn yarn, pre-oriented yarn, medium-oriented yarn, high-oriented yarn, textured yarn, fully drawn yarn, industrial yarn, continuous bulked continuous yarn, short fiber and monofilament fiber.
2. A process for preparing a polyamide fiber according to claim 1, characterized in that it comprises:
(a) Directly feeding the polyamide 5X melt into a spinning manifold through a melt booster pump, or heating polyamide 5X resin to a molten state to form a polyamide 5X melt, and then feeding the polyamide 5X melt into the spinning manifold;
(b) The polyamide fiber is prepared by accurately metering a polyamide 5X melt by a metering pump, spraying the melt by a spinneret plate to form melt trickle, removing polyamide oligomer in the melt trickle by a saturated superheated steam device, a slow cooling device and a monomer suction device, and then cooling, oiling and winding the melt.
3. The method according to claim 2, wherein the method for removing the polyamide oligomer by using the saturated superheated steam device, the slow cooling device and the monomer suction device comprises the following steps: the method is characterized in that a saturated superheated steam device is arranged in a spinning box body, the saturated superheated steam entering the spinning box body is reheated by the box body and then sprayed into the spinning plate from the periphery below the spinneret plate, polyamide oligomer overflowing from spinneret orifices and fiber surfaces of the spinneret orifices is dissolved in the saturated superheated steam, a slow cooling device is arranged below the spinneret plate and used for increasing slow cooling temperature and inhibiting crystallization and separation of the polyamide oligomer, then the polyamide oligomer dissolved in the saturated superheated steam is taken away through monomer suction, and a monomer suction cover in a monomer suction device has an automatic constant-temperature heating function.
4. A method according to claim 3, characterized in that the temperature of the saturated superheated steam before entering the spinning beam is 80-200 ℃, further 90-180 ℃, further 100-160 ℃; and/or the presence of a gas in the gas,
the pressure of the saturated superheated steam before entering the spinning manifold is 0.8-2.2bar, further 1.0-2.0bar, further 1.2-1.8bar; and/or the presence of a gas in the gas,
the slow cooling temperature is 180-320 ℃, further 220-300 ℃, and further 240-280 ℃; and/or the presence of a gas in the gas,
the slow cooling height is less than or equal to 5cm, further less than or equal to 4cm, and further less than or equal to 3cm; and/or
The pressure of monomer suction is more than or equal to 0.6MPa, further more than or equal to 0.65MPa, and further more than or equal to 0.7MPa; and/or the presence of a gas in the gas,
the temperature of the monomer suction hood is 100-260 ℃, further 120-230 ℃, and further 140-200 ℃; and/or the presence of a gas in the gas,
the diameter of the spinneret plate is less than or equal to 88mm, further less than or equal to 77mm, and further less than or equal to 66mm; and/or the presence of a gas in the gas,
the period of a shovel plate of the assembly in the preparation process of the polyamide fiber is more than or equal to 16h, further more than or equal to 18h, and further more than or equal to 20h.
5. The method according to any one of claims 2 to 4, wherein the polyamide 5X resin comprises 1,5-pentanediamine structural units and dibasic acid structural units, the polyamide 5X resin contains a polyamide oligomer having a number average molecular weight of 2000 or less, and the content of the polyamide oligomer is 1.0wt% or less.
6. The method according to claim 5, wherein the polyamide 5X resin has a number average molecular weight of 2000 or more; and/or the presence of a gas in the gas,
the polyamide oligomer content is 0.95wt% or less, and further 0.9wt% or less; and/or the presence of a gas in the gas,
1,5-pentanediamine is 1,5-pentanediamine from a chemical source or a biological material source, and further is 1,5-pentanediamine from a biological material source; and/or the presence of a gas in the gas,
more than 90mol% of the dibasic acid structural units are derived from adipic acid; and/or the presence of a gas in the gas,
the dibasic acid structural unit of the polyamide 5X resin further 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 and octadecanedioic acid, terephthalic acid, isophthalic acid and phthalic acid.
7. Process according to claim 5 or 6, characterized in that the polyamide oligomer is selected from at least one of the following structures:
wherein n1 and n2 are respectively selected from integers of 1-8; preferably, n1 and n2 are each selected from integers of 1 to 6; more preferably, n1 and n2 are each independently an integer of 1 to 5; further preferably, n1 is 2, 3 or 4; n2 is 2, 3, 4 or 5;
m1 and m2 are each an integer of 2 to 18; preferably, m1 and m2 are each independently an integer of 4 to 16; further preferably, m1 is 4, 8 or 10 and m2 is 4, 8 or 10.
8. The method of any of claims 5-7, wherein the polyamide 5X resin comprises a first polyamide having a structure according to formula I:
the number average molecular weight of the first polyamide is 2000 or more, and the content of the first polyamide in the polyamide 5X resin is 85wt% or more, further 90wt% or more, and further 95wt% or more.
9. The process according to any one of claims 5 to 8, characterized in that the polyamide 5X resin has a relative viscosity of 2.3 to 3.6, preferably 2.4 to 3.5, more preferably 2.5 to 3.4; and/or the presence of a gas in the gas,
the polyamide 5X resin has a water content of 300 to 900ppm, preferably 350 to 800ppm, and more preferably 400 to 700ppm; and/or the presence of a gas in the gas,
the polyamide 5X resin has an amino group-terminated content of 40 to 70mol/ton, preferably 43 to 60mol/ton, and more preferably 45 to 55mol/ton.
10. The method according to any one of claims 5 to 9, wherein the method for preparing the polyamide 5X resin comprises:
(1) Uniformly mixing 1,5-pentamethylene diamine, dibasic acid and water in an inert gas atmosphere to prepare a salt solution of polyamide;
(2) Heating the salt solution of polyamide, raising the pressure in the reaction system to 0.5-2.4 MPa, exhausting and maintaining the pressure, reducing the pressure to 0-0.2 MPa when the pressure maintaining is finished, and vacuumizing to obtain polyamide 5X melt, wherein the temperature of the reaction system is 235-268 ℃ after the pressure maintaining is finished, and the temperature of the reaction system is 248-282 ℃ after the pressure reducing is finished;
(3) Discharging the melt obtained in the step (2), and carrying out bracing and dicing.
11. The method of claim 10, wherein in step (1), the molar ratio of 1,5-pentanediamine to the dibasic acid is (1-1.08): 1; and/or the presence of a gas in the gas,
in the step (2), the vacuum pumping is performed to ensure that the relative vacuum degree in the reaction system is-0.02 MPa to-0.08 MPa; and/or the presence of a gas in the gas,
in the step (2), the vacuum time is maintained for 18-70 min; and/or the presence of a gas in the gas,
in the step (2), the vacuum ending temperature is controlled to be 263-278 ℃; and/or the presence of a gas in the atmosphere,
in the step (3), the granulation is carried out in water, and the water temperature is 15-50 ℃.
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| CN112410916A (en) * | 2019-08-22 | 2021-02-26 | 上海凯赛生物技术股份有限公司 | Polyamide 56 fiber with low boiling water shrinkage rate and preparation method and application thereof |
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