CN103774271B - A kind of function nylon 6 fiber and preparation method thereof - Google Patents
A kind of function nylon 6 fiber and preparation method thereof Download PDFInfo
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- CN103774271B CN103774271B CN201410029723.4A CN201410029723A CN103774271B CN 103774271 B CN103774271 B CN 103774271B CN 201410029723 A CN201410029723 A CN 201410029723A CN 103774271 B CN103774271 B CN 103774271B
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Abstract
The present invention relates to a kind of function nylon 6 fiber and preparation method thereof, this fiber includes that side chain nylon 6 functional agglomerate and conventional nylon 6 are cut into slices, and wherein the mass percent of side chain nylon 6 functional agglomerate is 6～10%；Its preparation method includes: (1) uses situ aggregation method or blending method to prepare side chain nylon 6 functional agglomerate；(2) side chain nylon 6 functional agglomerate is cut into slices with conventional nylon 6 crystallization respectively, mix after drying, the most vacuum dried the blended slice；Finally blended slice is carried out melt spinning.The present invention can improve or keep functional on the premise of, suitably reduce the consumption of functional additive, both reduced production cost, and added again the spinnability of fiber.
Description
Technical field
The invention belongs to function nylon fiber field, particularly to a kind of function nylon 6 fiber and preparation method thereof.
Background technology
Nylon 6 fiber has a series of premium properties, but there is also shortcoming, resistance to heat differential as low in modulus, fast light, the most aging,
Antistatic behaviour difference etc..Along with growth in the living standard, people are the most not exclusively satisfied with the warming effect that traditional fibre is brought,
More pursue functionalization, become more meticulous, health, quality.
Compared with developed countries, the nylon fiber new product that current China has independent intellectual property right is considerably less, really uses
Then less in the kind of industrialization, secondly nylon fiber price relatively polyester fiber is high, and fiber series of products must be located at high-end
Level, the competitiveness of guarantee enterprise.Therefore, develop novel nylon 6 fiber and its products, improve nylon 6 fiber
Differentiation rate and the application in superior quality fiber cloth are the inexorable trends of nylon industry development.
To be blended or to introduce preparation function nylon 6 master batch and the fibres thereof such as anti ultraviolet agent, antistatic additive, antiseptic in the way of copolymerization
Dimension, can be effectively improved fiber applications and be worth.Blending method introduces functional particles can make function grain by adding coupling agent
Son is dispersed in fibre section, if but particle can being made to maximize and be dispersed in fiber surface, by the specific surface area of contact
Increase, not only can make to optimize, maximize the effect of function particle, and can suitably reduce particle addition,
There is good spinning technique processing.
Summary of the invention
The technical problem to be solved is to provide a kind of function nylon 6 fiber and preparation method thereof, and the method ensures merit
Can particle maximize, Stable distritation in fiber surface, and functional particles can be avoided to be gathered in fibrillar center in a large number as far as possible and not
Directly can contact with the external world's such as human body skin etc., maximized performance is antistatic, uvioresistant, antibacterial, deodorizing, fire-retardant, remote
Infrared function affect such as grade.
A kind of function nylon 6 fiber of the present invention, this fiber includes that side chain nylon 6 functional agglomerate and conventional nylon 6 are cut into slices,
Wherein the mass percent of side chain nylon 6 functional agglomerate is 6～10%；Described side chain nylon 6 functional agglomerate is the most poly-
Close side chain nylon 6 functional agglomerate or blended side chain nylon 6 functional agglomerate.
Described blended side chain nylon 6 functional agglomerate is by side chain nylon 6 slice and nano functional additive, dispersant and coupling
Agent combines melt blending, prepared by pelletizing；The mass percent of the most each component is:
Described side chain nylon 6 slice is by caprolactam, molecular weight regulator, deionized water and 1,3,5-Benzenetricarboxylic acid or equal benzene four
Formic acid polymerisation under nitrogen protection prepares, and on the basis of described caprolactam, remaining each constituent mass percentage is:
Molecular weight regulator 5～7 ‰；
Deionized water 4～5%；
1,3,5-Benzenetricarboxylic acid or Pyromellitic Acid 1～2%.
Described in-situ polymerization side chain nylon 6 functional agglomerate is by caprolactam, molecular weight regulator, deionized water, nanometer merit
Can additive, coupling agent and 1,3,5-Benzenetricarboxylic acid or Pyromellitic Acid, polymerisation prepares under nitrogen protection, with described oneself
On the basis of lactams, the mass percent of remaining each component is:
Described molecular weight regulator is one or more in the organic acid such as adipic acid, acetic acid.
Described nano functional additive is that antistatic additive, anti ultraviolet agent, antiseptic, deodorant, fire retardant, far infrared add
Add one or more of agent etc..
Described coupling agent is one or more in silane coupler, titanate coupling agent；Described silane coupler is commercially available
One or more in KH550, KH560, KH570；Described titanate coupling agent is commercially available NDZ-105, NDZ-133,
One or more in NDZ-201, NDZ-311, NDZ-311W, NDZ-401.
A kind of preparation method of the function nylon 6 fiber of the present invention, including:
(1) the blended preparation of side chain nylon 6 functional agglomerate:
By coupling agent, nano functional additive and EtOH Sonicate vibration 2～3h, through air-stream spraying post-drying, obtain coupling agent
Nano functional additive after modification；Then the nano functional additive after being modified by coupling agent mixes with side chain nylon 6 slice
After being sufficiently stirred for, enter double screw extruder and melt extrude, then carry out pelletizing, i.e. obtain side chain nylon 6 function female
Grain；
Or prepared by in-situ polymerization:
Or by caprolactam, molecular weight regulator, deionized water, nano functional additive, coupling agent and 1,3,5-Benzenetricarboxylic acid or
Pyromellitic Acid carries out in-situ polymerization at 250～270 DEG C, then through pelletizing, the polymer melt obtained i.e. is obtained side chain nylon 6
Functional agglomerate；
(2) be blended and spinning
Side chain nylon 6 functional agglomerate is cut into slices with conventional nylon 6 crystallization respectively, mix after drying, the most vacuum dried
Blended slice；Finally blended slice is carried out melt spinning.
After pelletizing described in step (1), product is carried out pure water extraction at 100～120 DEG C, extractable matter is reduced to
Less than 0.5%, finally it is dried to constant weight at nitrogen 110～140 DEG C.
Side chain nylon 6 functional agglomerate described in step (2) and conventional nylon 6 cut into slices crystallize respectively, be dried in be dried
Time is 20～24 hours, and baking temperature is 100～120 DEG C；Described vacuum drying is that vacuum is done at 100～120 DEG C
Dry 1～2 hour.
In melt spinning described in step (2) screw rod district temperature be 250～270 DEG C, spinning speed be 4200～
4400m/min, GR1 drawing temperature be normal temperature, GR2 drawing temperature be 160～185 DEG C, drafting multiple be 1.1～2.0 times,
Wherein spinneret orifice draw ratio is 2.5～3:1, increases annealing device, and the barrel dliameter of heating muff is identical with spinneret plate footpath, its
Slow cooling district temperature 250～270 DEG C, heating mantle tube length 5～7cm.
The optimal selection of the present invention is in-situ polymerization mode, and side chain nylon 6 master batch of preparation is formed spherical, has high fluidity
And it is functional.Prepared branched chain type nylon 6 slice relative viscosity 2.0～2.3, fusing point 218～221 DEG C, branched chain type Buddhist nun
Dragon 6 viscosity are low, have high fluidity.
Present invention screw rod district temperature in melt spinning is 250～270 DEG C, and spinning speed is 4200～4400m/min, GR1
Drawing temperature normal temperature, GR2 drawing temperature is 160～185 DEG C, and drafting multiple is 1.1～2.0 times, wherein spinneret orifice draw ratio
Being 2.5～3:1, increase annealing device, the barrel dliameter of heating muff is identical with spinneret plate footpath, its slow cooling district temperature 250～270
DEG C, heating mantle tube length 5～7cm, it is ensured that the tow difference variation of filament mouth is little, thus realize tow slow cooling effect, prop up simultaneously
Chain nylon 6 functional agglomerate leaves spinneret orifice and utilizes in slow cooling district its high fluidity to be enriched with at fiber surface by aperture is expanded, system
Obtain a kind of function nylon 6 fiber.
The preparation method of the present invention a kind of function nylon 6 fiber, it uses side chain nylon 6, and viscosity is low, with conventional nylon 6
Compare, there is high fluidity.In spinning process, when polymer melt is extruded from spinneret aperture, owing to melt enters
Spinneret aperture, produces longitudinal velocity gradient at flow direction, and melt generation tensile elasticity deformation, the time of staying is relatively wherein
Short, have little time to relax, in place of outlet, the effect of strand is released by external force, and the macromolecular chain of stretching, extension is returned to roll up
State, on the other hand be polymer in flow process by shear stress, cause the diameter of extrudate substantially to become big,
There is extrusion swelling phenomenon.At spinning nozzle, side chain nylon 6 is along with extrusion swelling, owing to flowing velocity is fast, first toward two
Side is quickly distributed, and drives functional particles to be enriched in fiber surface, increases annealing device in addition, it is ensured that particle-stabilised under manifold
Being distributed in surface, the fiber after cooling can reach similar postfinishing process effect, but has persistence, and fibrous outer is for propping up
Chain function nylon 6, nexine is conventional nylon 6.
The branched chain type nylon 6 that the present invention uses is low with conventional nylon 6 phase specific viscosity, has high fluidity, sprays at spinning manifold
Silk mouth extrusion, in conjunction with retarded cooling process, high fluidity side chain nylon 6 drives functional particles to be enriched in fiber surface, cooling
After fiber can reach required requirement.
Beneficial effect:
(1) side chain nylon 6 is better than conventional nylon 6 fluidity of molten, and polymer melt is extruded from spinneret aperture, adjoint
Melt swell effect, high-fluidity nylon 6 drives functional particles to be enriched in fiber surface, in conjunction with retarded cooling process, it is ensured that
Functional particles maximizes, Stable distritation in fiber surface, and functional particles can be avoided to be gathered in fibrillar center in a large number as far as possible and
Directly can not contact with the external world's such as human body skin etc..The maximized performance of particle of appearance is antistatic, uvioresistant, antibacterial, remove
The function affects such as smelly, fire-retardant, far infrared.
(2) present invention can improve or keep functional on the premise of, suitably reduce the consumption of functional additive, both dropped
Low production cost, adds again the spinnability of fiber.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
A kind of function nylon 6 fiber, it is cut into slices by side chain nylon 6 functional agglomerate and conventional nylon 6 and forms, its percent mass
Than being:
Side chain nylon 6 functional agglomerate 6%
Conventional nylon 6 is cut into slices surplus
Optimal selection in-situ polymerization, described polymerization side chain nylon 6 functional agglomerate, by 1,3,5-Benzenetricarboxylic acid, caprolactam, divides
Son amount conditioning agent, deionized water, nano functional additive, coupling agent, polymerisation prepares under nitrogen protection, with described
Caprolactam on the basis of, its raw material components mass percent is:
Described molecular weight regulator is acetic acid；
Described nano functional additive is antistatic additive.
Coupling agent can be the commercially available NDZ-105 of titanate coupling agent.
Prepared branched chain type nylon 6 slice relative viscosity is 2.3, and fusing point 221 DEG C, branched chain type nylon 6 viscosity is low, has
High fluidity.
Its preparation method is:
(1) preparation of side chain nylon 6 functional agglomerate
Caprolactam metering after, with by metering 1,3,5-Benzenetricarboxylic acid molecular weight regulator, deionized water, functional additive,
Silane coupler by static mixer, adds polymerization tower together, and through polymerization open loop, polymerization temperature is at 250 DEG C.Poly-
Conjunction melt, through pelletizing, extracts at 100 DEG C of pure water, extractable matter is reduced to less than 0.5%.Section after extraction is passed through nitrogen
110 DEG C of gas is dried to constant weight.
(2) be blended and spinning
Being cut into slices with conventional nylon 6 by side chain nylon 6 functional agglomerate and crystallize respectively, be dried 20 hours, baking temperature is 100
DEG C, mixing the most in proportion, be dried 1 hour in vacuum drum baking oven, baking temperature is 100 DEG C, prepares blended slice；
By blended slice, carrying out co-blended spinning through apparatus for melt spinning, process route is: screw extruder → prefilter →
Measuring pump → filament spinning component → spinneret → cross air blasting oils → drawing-off → winding, and screw rod district temperature is 250～270 DEG C, spinning speed
Degree is 160 DEG C for 4200m/min, GR2 drawing temperature, and drafting multiple is 1.1 times, and wherein spinneret orifice draw ratio is 2.5:
1, increase annealing device, the barrel dliameter of heating muff is identical with spinneret plate footpath, its slow cooling district temperature 250 DEG C, heating muff
Long 7cm, it is ensured that the tow difference variation of filament mouth is little, thus realize tow slow cooling effect, side chain nylon 6 function is female simultaneously
Grain leaves spinneret orifice and utilizes in slow cooling district its high fluidity to be enriched with at fiber surface by aperture is expanded, prepares a kind of function nylon
6 fibers.
Embodiment 2
A kind of function nylon 6 fiber, it is cut into slices by side chain nylon 6 functional agglomerate and conventional nylon 6 and forms, its percent mass
Than being:
Side chain nylon 6 functional agglomerate 8%
Conventional nylon 6 is cut into slices surplus
Optimal selection in-situ polymerization, described polymerization side chain nylon 6 functional agglomerate, by Pyromellitic Acid, caprolactam, divides
Son amount conditioning agent, deionized water, nano functional additive, coupling agent, polymerisation prepares under nitrogen protection, with described
Caprolactam on the basis of, its raw material components mass percent is:
Described molecular weight regulator is acetic acid；
Described nano functional additive is antiseptic and far infrared additive.
Coupling agent can be silane coupler KH560 and titanate coupling agent NDZ-311 W.
Prepared branched chain type nylon 6 slice relative viscosity is 2.2, and fusing point 220 DEG C, branched chain type nylon 6 viscosity is low, has
High fluidity.
Its preparation method is:
(1) preparation of side chain nylon 6 functional agglomerate
Caprolactam metering after, with by metering Pyromellitic Acid molecular weight regulator, deionized water, functional additive,
Silane coupler by static mixer, adds polymerization tower together, and through polymerization open loop, polymerization temperature is at 260 DEG C.Poly-
Conjunction melt, through pelletizing, extracts at 110 DEG C of pure water, extractable matter is reduced to less than 0.5%.Section after extraction is passed through nitrogen
120 DEG C of gas is dried to constant weight.
(2) be blended and spinning
Being cut into slices with conventional nylon 6 by side chain nylon 6 functional agglomerate and crystallize respectively, be dried 22 hours, baking temperature is 110 DEG C,
Mixing the most in proportion, be dried 1.5 hours in vacuum drum baking oven, baking temperature is 110 DEG C, prepares blended slice；
By blended slice, carrying out co-blended spinning through apparatus for melt spinning, process route is: screw extruder → prefilter →
Measuring pump → filament spinning component → spinneret → cross air blasting oils → drawing-off → winding, and screw rod district temperature is 250～270 DEG C, spinning speed
Degree is 4300m/min, GR1 drawing temperature normal temperature, and GR2 drawing temperature is 170 DEG C, and drafting multiple is 1.3 times, prepares
Function nylon 6 fiber.Wherein spinneret orifice draw ratio is 2.75:1, increases annealing device, the barrel dliameter of heating muff and spinneret
Plate plate footpath is identical, its slow cooling district temperature 260 DEG C, heating mantle tube length 6cm, it is ensured that the tow difference variation of filament mouth is little, from
And realizing tow slow cooling effect, side chain nylon 6 functional agglomerate leaves spinneret orifice and utilizes its high fluidity to pass through in slow cooling district simultaneously
Aperture is expanded to be enriched with at fiber surface, prepares a kind of function nylon 6 fiber.
Embodiment 3
A kind of function nylon 6 fiber, it is cut into slices by side chain nylon 6 functional agglomerate and conventional nylon 6 and forms, its percent mass
Than being:
Side chain nylon 6 functional agglomerate 10%
Conventional nylon 6 is cut into slices surplus
Optimal selection in-situ polymerization, described polymerization side chain nylon 6 functional agglomerate, by 1,3,5-Benzenetricarboxylic acid, caprolactam, divides
Son amount conditioning agent, deionized water, nano functional additive, coupling agent, polymerisation prepares under nitrogen protection, with described
Caprolactam on the basis of, its raw material components mass percent is:
Described molecular weight regulator is adipic acid, acetic acid；
Described nano functional additive deodorant and far infrared additive.
Coupling agent can be titanate coupling agent NDZ-133, NDZ-201.
Prepared branched chain type nylon 6 slice relative viscosity is 2.1, and fusing point 219 DEG C, branched chain type nylon 6 viscosity is low, has
High fluidity.
Its preparation method is:
(1) preparation of side chain nylon 6 functional agglomerate
Caprolactam metering after, with by metering 1,3,5-Benzenetricarboxylic acid molecular weight regulator, deionized water, functional additive,
Silane coupler by static mixer, adds polymerization tower together, and through polymerization open loop, polymerization temperature is at 270 DEG C.Poly-
Conjunction melt, through pelletizing, extracts at 120 DEG C of pure water, extractable matter is reduced to less than 0.5%.Section after extraction is passed through nitrogen
140 DEG C of gas is dried to constant weight.
(2) be blended and spinning
Being cut into slices with conventional nylon 6 by side chain nylon 6 functional agglomerate and crystallize respectively, be dried 24 hours, baking temperature is 120
DEG C, mixing the most in proportion, be dried 2 hours in vacuum drum baking oven, baking temperature is 120 DEG C, prepares blended slice；
By blended slice, carrying out co-blended spinning through apparatus for melt spinning, process route is: screw extruder → prefilter →
Measuring pump → filament spinning component → spinneret → cross air blasting oils → drawing-off → winding, and screw rod district temperature is 250～270 DEG C, spinning speed
Degree is 4400m/min, GR1 drawing temperature normal temperature, and GR2 drawing temperature is 185 DEG C, and drafting multiple is 1.5 times, wherein
Spinneret orifice draw ratio is 3:1, increases annealing device, and the barrel dliameter of heating muff is identical with spinneret plate footpath, its slow cooling district temperature
270 DEG C, heating mantle tube length 5cm, it is ensured that the tow difference variation of filament mouth is little, gradually to normal temperature, thus realize tow and delay
Cold-working use, prepares a kind of function nylon 6 fiber.
Embodiment 4
A kind of function nylon 6 fiber, it is cut into slices by side chain nylon 6 functional agglomerate and conventional nylon 6 and forms, its percent mass
Than being:
Side chain nylon 6 functional agglomerate 9%
Conventional nylon 6 is cut into slices surplus；
Described blended side chain nylon 6 functional agglomerate is by side chain nylon 6 slice and nano functional additive, dispersant and coupling
Agent combines melt blending, prepared by pelletizing；The mass percent of the most each component is:
Described side chain nylon 6 slice is by caprolactam, molecular weight regulator, deionized water and 1,3,5-Benzenetricarboxylic acid or equal benzene four
Formic acid polymerisation under nitrogen protection prepares, and on the basis of described caprolactam, remaining each constituent mass percentage is:
Molecular weight regulator 6 ‰；
Deionized water 5%；
1,3,5-Benzenetricarboxylic acid or Pyromellitic Acid 2%.
Described molecular weight regulator is adipic acid；
Described nano functional additive is anti ultraviolet agent, antiseptic.
Coupling agent can be Silane coupling agent KH550.
Prepared branched chain type nylon 6 slice relative viscosity is 2.0, and fusing point 218 DEG C, branched chain type nylon 6 viscosity is low, has
High fluidity.
Its preparation method is:
(1) the blended preparation of side chain nylon 6 functional agglomerate
By coupling agent, nano functional additive and EtOH Sonicate vibration 2～3h, through air-stream spraying post-drying, obtain coupling agent
Nano functional additive after modification；Then the nano functional additive after being modified by coupling agent mixes with side chain nylon 6 slice
After being sufficiently stirred for, enter double screw extruder and melt extrude, then carry out pelletizing, i.e. obtain side chain nylon 6 function female
Grain；
(2) be blended and spinning
Being cut into slices with conventional nylon 6 by side chain nylon 6 functional agglomerate and crystallize respectively, be dried 22 hours, baking temperature is 110 DEG C,
Mixing the most in proportion, be dried 1.5 hours in vacuum drum baking oven, baking temperature is 110 DEG C, prepares blended slice；
By blended slice, carrying out co-blended spinning through apparatus for melt spinning, process route is: screw extruder → prefilter →
Measuring pump → filament spinning component → spinneret → cross air blasting oils → drawing-off → winding, and screw rod district temperature is 250～270 DEG C, spinning speed
Degree is 4300m/min, GR1 drawing temperature normal temperature, and GR2 drawing temperature is 170 DEG C, and drafting multiple is 2.0 times, prepares
Function nylon 6 fiber.Wherein spinneret orifice draw ratio is 2.75:1, increases annealing device, the barrel dliameter of heating muff and spinneret
Plate plate footpath is identical, its slow cooling district temperature 260 DEG C, heating mantle tube length 6cm, it is ensured that the tow difference variation of filament mouth is little, from
And realizing tow slow cooling effect, side chain nylon 6 functional agglomerate leaves spinneret orifice and utilizes its high fluidity to pass through in slow cooling district simultaneously
Aperture is expanded to be enriched with at fiber surface, prepares a kind of function nylon 6 fiber.
Claims (2)
1. a preparation method for function nylon 6 fiber, including:
(1) by caprolactam, molecular weight regulator, deionized water, nano functional additive, coupling agent and Pyromellitic Acid 250～
270 DEG C carry out in-situ polymerization, then through pelletizing, the polymer melt obtained i.e. are obtained side chain nylon 6 functional agglomerate；Wherein, with institute
On the basis of the caprolactam stated, the mass percent of remaining each component is:
(2) side chain nylon 6 functional agglomerate is cut into slices with conventional nylon 6 crystallization respectively, mix after drying, the most vacuum dried must be total to
Mixed section；Finally blended slice is carried out melt spinning；Wherein the mass percent of side chain nylon 6 functional agglomerate be 6～
10%, in described melt spinning, screw rod district temperature is 250～270 DEG C, spinning speed is 4200～4400m/min, GR1 lead
Stretch temperature be normal temperature, GR2 drawing temperature be 160～185 DEG C, drafting multiple be 1.1～2.0 times, wherein spinneret orifice draw ratio is
2.5～3:1, increase annealing device, the barrel dliameter of heating muff is identical with spinneret plate footpath, its slow cooling district temperature 250～270 DEG C,
Heating mantle tube length 5～7cm.
The preparation method of function nylon 6 fiber the most according to claim 1, it is characterised in that: described in step (1)
Pelletizing after, product is carried out pure water extraction at 100～120 DEG C, extractable matter is reduced to less than 0.5%, finally at nitrogen
It is dried to constant weight at 110～140 DEG C.
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Effective date of registration: 20181207 Address after: 215144 Shiqiao Village, Beiqiao Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Suzhou Baoli Di material Polytron Technologies Inc Address before: 201620 No. 2999 North Renmin Road, Songjiang new town, Songjiang District, Shanghai. Patentee before: Donghua University |