CN110820079A - Preparation method of nano-doped polyamide parallel elastic composite fiber - Google Patents
Preparation method of nano-doped polyamide parallel elastic composite fiber Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/061—Load-responsive characteristics elastic
Abstract
The invention discloses a preparation method of nano-doped polyamide parallel elastic composite fibers. The preparation method comprises the steps of melting dry slices, accurately metering and extruding the melted dry slices through respective metering pumps, conveying the two extruded melts into the same spinning box body and a composite component through respective pipelines, converging the melts in a spinneret plate or at the outlet of the spinneret plate, bonding two melt trickle flows together, and cooling, forming and post-treating the melt by cross air blowing to obtain the parallel composite fiber. The intermolecular interaction of one component of the composite fiber is regulated and controlled by melt blending or in-situ polymerization doping one or more of nano layered silicate, metal compound and rare earth compound into polyamide, and the polyamide self-crimping parallel composite fiber is prepared by using the difference of the shrinkage rates of the modified component and the unmodified component through a double-component melt compounding spinning and drawing integrated device, so that the defects of low strength, poor hygroscopicity, no high temperature resistance, high machine washing cost and the like of the conventional elastic fiber are overcome.
Description
Technical Field
The invention relates to a preparation method of a two-component parallel composite fiber, belongs to the technical field of functional fibers and spinning, and particularly relates to a preparation method of a nano composite material and a polyamide parallel composite fiber.
Background
At present, the differentiated products in the chemical fiber market in China account for over 80 percent, but the homogenization is serious, and the elastic fiber draws wide attention along with the large-scale promotion of Lycra (Lycra) products. The polyurethane elastic fiber has the advantages of high elongation, high strength, aging resistance and the like which are superior to those of rubber silk, but the production equipment and the process of the polyurethane elastic fiber are complex, the raw material and processing cost is high, the dyeing is not easy, and the pollution problem is serious, thereby limiting the application of the polyurethane elastic fiber. In order to reduce the cost and facilitate the processing so as to meet the further requirements of the market, the parallel elastic composite fibers have acquired a great development space.
The parallel composite fiber is a bi-component composite filament formed by two high polymers with different shrinkage properties through composite spinning equipment according to a certain proportion. The two components arranged in parallel within the fiber will experience a difference in shrinkage during heat treatment due to the nature of the polymer molecular motion, with the fast shrinking component producing a shrinking pressure on the slow shrinking component and the fast shrinking component being subjected to a counter stretching force generated by the slow shrinking component. When the two acting forces reach equilibrium after being deformed to a certain degree along with contraction, the whole fiber is spontaneously twisted to form a three-dimensional spiral winding structure like a spring. The crimp elasticity of such bicomponent elastic fibers is very similar to that of natural wool, and the fibers and their fabrics are soft, bulky, and resilient.
With the increasing requirements of people on the comfort and health of fabrics, as high-grade textiles with excellent comprehensive performance, polyamide has the characteristics of good elasticity and wear resistance, good hygroscopicity, easiness in washing and drying, easiness in dyeing, skin friendliness, light weight and the like.
In addition, polyamide structures are diverse, and supramolecular structures with ordered hydrogen bonds can be formed between molecules, so that the intermolecular hydrogen bonds are regulated or shielded to some extent. If the polyamide is complexed with a small amount of metal ions, the performance of the polyamide can be obviously influenced. The composite fiber is used as a component of the bi-component composite fiber, the designability of the material is strong, and the parallel composite fiber prepared by using the modified polyamide as the raw material has richer performance and application range compared with the existing fiber products.
Therefore, the knitted elastic fabric is expected to have wider application prospect in the fields of high-grade underwear, sportswear, automobile decoration and medical use.
Disclosure of Invention
The invention aims to utilize nano layered silicate, metal compound, rare earth compound and polyamide to carry out nano compounding, regulate and control the crimping rate and the mechanical property of the polyamide bi-component nano composite fiber through the content or the variety of nano adulterants, and solve the defects of low strength, poor hygroscopicity, no high temperature resistance, high manufacturing cost and the like of the conventional elastic fiber.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. According to the preparation method of the nano-doped polyamide parallel elastic composite fiber provided by the invention, the nano-doped polyamide parallel elastic composite fiber is prepared by adopting a parallel composite spinning process.
The production equipment required by the preparation process mainly comprises a screw extruder A, a screw extruder B, a melt conveying pipeline, a metering pump, a composite spinning assembly, a side blowing device, an oil feeding nozzle, a first hot roller (GR1), a second hot roller (GR2), a networkable, a winding machine and the like.
The preparation process of the parallel elastic composite fiber by adopting the equipment comprises the following steps:
the dried two raw materials are respectively fed into an A, B screw extruder, and are conveyed into a spinning manifold through respective pipelines after melt extrusion, and after the two melts are accurately metered by a metering pump, the two melts are converged in a spinneret plate or converged and bonded into a whole at the outlet of the spinneret plate. And cooling the filament by side blowing, oiling, passing through a first roller and a second roller, and winding and forming by a winding machine to obtain the parallel composite POY pre-oriented yarn. The rotation speeds of the first hot roller GR1 and the second hot roller GR2 are adjusted to form a certain draw ratio, and the side-by-side composite FDY pre-oriented yarn can be obtained after sizing and network. And (3) stretching or texturing the POY pre-oriented yarn to obtain a DT stretched yarn or a DTY stretched textured yarn.
The amide group carbonyl oxygen and the amino nitrogen in the polyamide fiber both contain lone pair electrons and are therefore very polar. Both nitrogen and oxygen atoms are likely to combine with protons and metal ions to form hydrogen and coordination bonds, and a small amount of metal ions can have a significant effect on the performance of the polyamide. Through the interaction with the nano layered silicate, the metal compound and the rare earth compound, the hydrogen bond among polyamide molecules can be adjusted or shielded to a certain degree, and finally the purpose of improving the performance of the polyamide material is achieved.
The component A is thermoplastic polyamide resin, and the component B is a compound consisting of the thermoplastic polyamide resin and a nano additive.
The nano additive is one or more of nano layered silicate, metal compound and rare earth compound, is doped into polyamide through melt blending or in-situ polymerization, and at least one dimension of the polyamide exists in a nano size, and the adding proportion is 0.5-4 wt%.
The polyamide is a crystalline polymer, the crystallization speed of the polyamide is obviously increased by adding the phyllosilicate, the size of spherulites is reduced, and the number of the spherulites is increased. The integrity of the spherulites is reduced due to the mutual interference between the spherulites. The silicate sheet is dispersed in the polyamide matrix in a nanometer size, so that the contact area between the silicate sheet and the polyamide matrix is greatly increased, and the layered silicate plays a role of a reinforcing agent in the polyamide matrix.
The nano composite material prepared by co-extruding polyamide and organic modified phyllosilicate has obviously improved mechanical property when the content of phyllosilicate is 2-4%. The metal ions are complexed to the amide groups in a different manner, with most of the metal ions being complexed to the carbonyl oxygen atom.
The alkaline earth metal and the rare earth metal have good effect of improving the performance of the polyamide, and have the advantage that the melting point, the crystallization temperature, the crystallinity and the like of the polyamide can be obviously reduced by less addition (less than or equal to 5 percent). The fluidity of the blend is good, which is beneficial to the practical processing, and the amorphous polyamide prepared by the coordination of the blend and metal ions can obtain high-performance fiber through high-power drawing, decomplexing and heat treatment.
The nano layered silicate is one or more of montmorillonite, diatomite and attapulgite;
the metal compound is one or more of zinc oxide, zinc chloride, lithium chloride and calcium chloride;
the rare earth compound is one or more of lanthanum oxide, cerium oxide, yttrium chloride, gadolinium trichloride and lanthanum acetate.
The process flow of the parallel composite spinning comprises the following steps:
1) the two raw material slices after vacuum drying are respectively sent into a screw extruder A and a screw extruder B, two melts after melt extrusion are conveyed into a spinning manifold through respective pipelines, then flow through the same spinning manifold and a composite component and are converged in a spinneret plate or at the outlet of the spinneret plate, two melt thin flows are bonded together, and the two melt thin flows are cooled by cross air blowing and oiled to form the parallel composite fiber.
2) And (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like.
Further, the extrusion temperature is 255-295 ℃; the cooling air temperature is 17-25 ℃, and the air speed is 0.2-0.55 m/s; the winding speed is 3000-5000 m/min;
further, in the drafting step, the temperature of a hot plate is 70-85 ℃, the temperature of a hot plate is 110-120 ℃, the draw ratio is 1.2-1.6, and the drafting speed is 220-235 m/min;
furthermore, the filament number of the parallel elastic composite fiber is 1-6dtex, the breaking strength is 2.0-4.5cN/dtex, the crimp shrinkage rate is 30-60%, the crimp stability is 20-80%, and the crimp modulus is 10-20%.
By means of the technical scheme, the invention has the following advantages and beneficial technical effects:
1) the invention provides a preparation method of nano-doped polyamide bi-component parallel elastic composite fiber and a method for regulating and controlling the crimping performance.
2) The invention utilizes the nano layered silicate, the metal compound and the rare earth compound to carry out nano compounding on the polyamide, regulates and controls the crimping rate and the mechanical property of the polyamide bi-component nano composite fiber through the content or the variety of the nano adulterant, and solves the defects of low strength, poor hygroscopicity, no high temperature resistance, high machine washing cost and the like of the prior elastic fiber.
Drawings
FIG. 1 is a flow chart of the structure of the production apparatus for nano-doped polyamide bicomponent side-by-side elastic composite fiber of the present invention.
FIG. 2 is a process flow diagram of the preparation method of the nano-doped polyamide bi-component side-by-side elastic composite fiber of the present invention.
Fig. 3 is a schematic diagram of the spinneret configuration of the side-by-side composite assembly employed in the present invention.
In fig. 1: 1-section A feed inlet; 2-screw extruder a; 3-a melt conveying pipe; 4-a feed port of a slice B and 5-a screw extruder B; 6-B melt conveying pipeline; 7-A melt metering pump; 8-B melt metering pump; 9-a double-channel plate-outside composite spinning assembly; 10-side blowing device, upper oil nozzle; 11-first thermo roll (GR 1); 12-second thermo roll (GR 2); 13-a winder; 14-a biphenyl boiler; 15-exhaust tank.
In FIG. 3, 21-pulp feed plate; 22-a filter screen; 23-a baffle; 24-a distribution plate; 25-an upper distributor plate; 26-a lower distributor plate; 27-a double-channel spinneret plate and a side-by-side spinneret plate.
Detailed Description
The present invention will be described in further detail below with reference to the accompanying drawings and preferred embodiments, but the present invention is not limited to the following embodiments.
The equipment required by the process mainly comprises a screw extruder A, a screw extruder B, a melt conveying pipeline, a metering pump, a double-channel plate-outside composite spinning assembly, a side blowing device, an oil feeding nozzle, a first hot roller (GR1), a second hot roller (GR2), a network device, a winding machine and the like. As shown in FIG. 1, FIG. 1 is a schematic structural diagram of a production apparatus for nano-doped polyamide bicomponent side-by-side elastic composite fiber according to the present invention. The production apparatus includes: the device comprises a slice A feeding port 1, an A screw extruder 2, an A melt conveying pipeline 3, a slice B feeding port 4, a B screw extruder 5, a B melt conveying pipeline 6, an A melt metering pump 7, a B melt metering pump 8, a double-channel plate external composite spinning assembly 9, a side blowing device, an upper oil nozzle 10, a first hot roller (GR1)11, a second hot roller (GR2)12, a winding machine 13, a biphenyl boiler 14 and an exhaust tank 15.
FIG. 2 is a process flow of the preparation method of the nano-doped polyamide bi-component side-by-side elastic composite fiber of the invention. As shown in FIG. 2, the preparation process of the nano-doped polyamide bi-component parallel elastic composite fiber comprises the following steps:
referring to fig. 3 in combination, fig. 3 is a schematic view of a spinneret plate structure in a side-by-side composite assembly used in the present invention. The structure of the spinneret plate in the parallel composite component mainly comprises: a pulp inlet plate 21, a filter screen 22, a guide plate 23, a distribution plate 24, an upper distribution plate 25, a lower distribution plate 26 and a double-channel spinneret plate outer composite parallel type spinneret plate 27.
The dried two raw materials are respectively sent into a screw extruder A2 and a screw extruder B5, the raw materials are conveyed into a spinning box body through respective pipelines after being melted and extruded, and the two melts are converged in a spinneret plate or converged and bonded into a whole at the outlet of the spinneret plate after being accurately metered by a melt metering pump A7 and a melt metering pump B8 respectively.
And cooling the filament by a side blowing device, oiling, passing through a first roller and a second roller, and winding and forming by a winding machine to obtain the parallel composite POY pre-oriented yarn. The rotation speeds of the first hot roller GR1 and the second hot roller GR2 are adjusted to form a certain draw ratio, and the side-by-side composite FDY pre-oriented yarn can be obtained after sizing and network. And (3) stretching or texturing the POY pre-oriented yarn to obtain a DT stretched yarn or a DTY stretched textured yarn.
The invention relates to a method for preparing polyamide self-crimping parallel composite fiber, which comprises the steps of doping one or more of nano layered silicate, metal compound and rare earth compound into polyamide through melt blending or in-situ polymerization to regulate and control the intermolecular interaction of one component of the composite fiber, and preparing the polyamide self-crimping parallel composite fiber through a double-component melt compounding spinning and drawing integrated device by utilizing the difference of the shrinkage rates of the modified component and the unmodified component.
In addition, the process flow chart of the invention for preparing nano-doped polyamide parallel elastic composite fiber by adopting the parallel composite spinning process is shown in the combined figure 2. The technological process includes melting dry chips, metering and extruding with metering pumps, conveying the two extruded melts via pipes to spinning box and compounding assembly, merging in or at the outlet of spinneret plate, adhering two melt flows together, and side blowing to cool, form and post-treat to obtain parallel composite fiber.
Further, the process flow of the parallel composite spinning is specifically as follows:
1) and respectively feeding the two raw material slices (the component a is thermoplastic polyamide resin, and the component B is a compound formed by the thermoplastic polyamide resin and a nano additive) which are subjected to vacuum drying into a screw extruder A and a screw extruder B.
Wherein the nano additive is one or more of nano phyllosilicate, metal compound and rare earth compound. One or more of the nano layered silicate montmorillonite, the diatomite and the attapulgite are embedded with long-chain organic cations among the layers of the silicate through cation exchange reaction, the layered silicate is uniformly dispersed in a polyamide matrix, and then the nano composite material is prepared by blending through a double-screw extruder.
Wherein the extrusion temperature of the screw extruder A and the screw extruder B is 255-295 ℃; the cooling air temperature is 17-25 ℃, and the air speed is 0.2-0.55 m/s; the winding speed is 3000-5000 m/min.
The two melts after melt extrusion are conveyed into a spinning manifold through respective pipelines, then flow through the same spinning manifold and a composite component, and are converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and are cooled by cross air blow and oiled to form parallel composite fibers.
2) And (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like. In the drafting step, the temperature of a hot plate is 70-85 ℃, the temperature of a hot plate is 110-120 ℃, the draw ratio is 1.2-1.6, and the drafting speed is 220-235 m/min.
The filament number of the parallel elastic composite fibers is 1-6dtex, the breaking strength is 2.0-4.5cN/dtex, the crimp shrinkage rate is 30-60%, the crimp stability is 20-80%, and the crimp modulus is 10-20%.
In a word, the thermoplastic polyamide resin is used as a component a, a composite formed by the thermoplastic polyamide resin and the nano additive is used as a component b, and a double-component melting composite spinning and drawing integrated machine is adopted to prepare the double-component polyamide parallel composite fiber.
For the parallel composite fiber with larger difference of intrinsic viscosity of the two components, the problem that the spinnability of the two components is lost due to overlarge difference of the intrinsic viscosity is solved due to the special-shaped structure of the spinneret orifice.
By causing the low viscosity component to be extruded through the circular arc shaped slit and the high viscosity component to be extruded through the circular hole. Because the spinneret orifices are different in shape, the flow speed and the flow stress of the two components are influenced mutually in the flow process, so that the two components can be extruded out from the spinneret orifices at the same speed, the corner bending phenomenon is avoided, and the spinnability of the parallel composite fibers with the two components having larger difference of intrinsic viscosities is realized.
The following raw material products are as follows: polyamide 6, organically treated montmorillonite, attapulgite, nano zinc oxide and the like are all commercially available products.
Example 1
A preparation method of nano-doped polyamide parallel elastic composite fiber comprises the following process steps:
1) polyamide 6 and organically treated montmorillonite are mixed according to the mass ratio of 1: 99, and carrying out melt blending in a double screw to obtain the polyamide 6/montmorillonite nano composite with the montmorillonite content of 1.0 percent (weight percentage).
2) The polyamide 6 is used as the component A, the polyamide 6/montmorillonite nano composite is used as the component B, parallel melt composite spinning is carried out, the spinning is converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the side-blown cooling and oiling are carried out to form parallel composite fibers.
Wherein the weight ratio of the component A to the component B is 5: 5, the spinning temperature is 260 ℃ and 275 ℃, the spinning speed is 4100m/min, the cooling air temperature is 20 ℃, and the air speed is 0.25 m/s.
3) And (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like. Wherein the drawing multiple is 1.25 times, and the FDY fully drawn yarn is spun.
The fiber had a single fiber fineness of 2.25dtex, a breaking strength of 3.8cN/dtex, a crimp shrinkage of 51%, a crimp stability of 39% and a crimp modulus of 16%.
Example 2
A preparation method of nano-doped polyamide parallel elastic composite fiber comprises the following process steps:
1) adding attapulgite into polyamide 6 during polymerization according to a mass ratio of 1.5: 98.5 to obtain the polyamide 6/attapulgite nano composite with the attapulgite content of 1.5 percent (weight percentage).
2) The polyamide 6 is used as the component A, the polyamide 6/attapulgite nano composite is used as the component B, parallel melt composite spinning is carried out, the spinning is converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the side-blown cooling and oiling are carried out to form parallel composite fibers.
Wherein, the proportion of the component A/B is 6: 4, the spinning temperature is 260 ℃ and 275 ℃, the spinning speed is 4200m/min, the cooling air temperature is 20 ℃, and the air speed is 0.25 m/s.
3) And (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like. Wherein the drawing multiple is 1.25 times, and the FDY fully drawn yarn is spun.
The fiber filament number was 3.75dtex, the breaking strength was 3.6cN/dtex, the crimp shrinkage was 47%, the crimp stability was 52%, and the crimp modulus was 14%.
Example 3
A preparation method of nano-doped polyamide parallel elastic composite fiber comprises the following process steps:
1) carrying out melt blending on polyamide 6 and nano zinc oxide in a double screw according to a mass ratio of 2.5: 97.5 to obtain the polyamide 6/zinc oxide nano composite with the zinc oxide content of 2.5 percent (weight percentage).
2) The polyamide 6 is used as an A component, the polyamide 6/zinc oxide nano compound is used as a B component to carry out parallel melt composite spinning, the spinning is converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the spinning is cooled by cross air blowing and oiled to form parallel composite fibers.
Wherein, the proportion of the component A/B is 6: 4, spinning at the spinning temperature of 260-275 ℃, the spinning speed of 3800m/min, the cooling air temperature of 20 ℃ and the air speed of 0.25m/s to prepare the POY pre-oriented yarn.
3) And (3) elasticizing the POY pre-oriented yarn to obtain a DTY drawn textured yarn with the drawing multiple of 1.2. The fiber had a single fiber fineness of 3.05dtex, a breaking strength of 3.4cN/dtex, a crimp shrinkage of 55%, a crimp stability of 63% and a crimp modulus of 11%.
Example 4
A preparation method of nano-doped polyamide parallel elastic composite fiber comprises the following process steps:
1) carrying out melt blending on polyamide 66 and nano lanthanum oxide in a double screw according to a mass ratio of 1.5: 98.5 to obtain the polyamide 66/lanthanum oxide nano composite with the lanthanum oxide content of 1.5 percent (weight percentage).
2) The polyamide 66 is used as an A component, the polyamide 66/lanthanum oxide nano composite is used as a B component, parallel melt composite spinning is carried out, the spinning is converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the side-blown cooling and oiling are carried out to form parallel composite fibers.
Wherein, the proportion of the component A/B is 7: 3, the spinning temperature is 260 ℃ and 285 ℃, the spinning speed is 3300m/min, the cooling air temperature is 18 ℃, and the air speed is 0.40 m/s.
3) And (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like.
The fiber filament number was 3.45dtex, the breaking strength was 3.2cN/dtex, the crimp shrinkage was 52%, the crimp stability was 27%, and the crimp modulus was 17%.
Example 5
A preparation method of nano-doped polyamide parallel elastic composite fiber comprises the following process steps:
1) carrying out melt blending on polyamide 66 and nano cerium oxide in a double screw according to a mass ratio of 3: 97 to obtain a polyamide 66/cerium oxide nanocomposite having a lanthanum oxide content of 3.0% by weight.
2) The polyamide 6 is used as the component A, the polyamide 66/lanthanum oxide nano compound is used as the component B, parallel melt composite spinning is carried out, the spinning is converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the side-blown cooling and oiling are carried out to form parallel composite fibers.
Wherein, the proportion of the component A/B is 4: 6, the spinning temperature is 260-285 ℃, the spinning speed is 3000m/min, the cooling air temperature is 18 ℃, and the air speed is 0.3 m/s;
3) and (3) immediately entering a guiding stretching and shaping stage after cooling and shaping, stretching the fiber by using a speed difference between GR1 and GR2, carrying out heat shaping on the fiber by using a high-temperature hot box of GR2, and obtaining fiber protofilaments by processes of networking, winding and the like. Wherein the drawing multiple is 1.2 times, and the FDY fully drawn yarn is spun.
The fiber filament number was 4.5dtex, the breaking strength was 2.8cN/dtex, the crimp shrinkage was 38%, the crimp stability was 73%, and the crimp modulus was 12%.
The following are contents of the effect test examples.
Effect test example 1
The post-treatment mode of the parallel composite fibers is dry heat treatment. Taking the same package of filament, winding 20 circles of filament, each circle of filament is about 50cm in length, knotting two ends into hank silk, and balancing for 30min at normal temperature and normal pressure.
To investigate the influence of the heat treatment temperature, the composite fiber was placed in an oven and dry-heat treated in a relaxed state at 40 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃ and 160 ℃ for 10 min.
To study the effect of heat treatment time, the composite fibers were heat treated at 120 ℃ for 2.5min, 5min, 7.5min, 10min, 12.5min, and 15min for relaxation.
To examine the effect of the heat treatment tension, the composite fiber was subjected to dry heat treatment at 120 ℃ for 10min while applying tensions of 0.4gf, 0.8gf, 1.2gf and 1.6gf, respectively. After the samples subjected to dry heat treatment are taken out, the samples are balanced for 30min at normal temperature and normal pressure for subsequent tests.
Effect test example 2
Before the tensile test, the linear density of the fiber needs to be determined, the YG086 type yarn length measuring instrument is firstly used for winding 100 circles of the filament, the skein is knotted, the mass (g) is weighed by an electronic balance, and the linear density (dtex) is 100 times of the weight of the skein.
The tensile test of the filament was carried out using an XL-II type yarn tensile tester, the clamping distance of the clamps was 250mm, the pre-tension was 5cN, and the drawing speed was 500 mm/min. Before the test, the head yarn of 50m or more of the surface layer of the package was removed, the test was conducted 20 times for each package, and 15 times with small dispersion were taken to calculate the average values of the breaking strength (cN/dtex) and the elongation at break (%).
The crimping rate and the crimping recovery rate of the composite fiber are tested by adopting a GB/T6506-2001 synthetic fiber textured yarn crimping performance test method. The end filament of about 50m of the surface layer of the package was removed, the filament was wound for 20 turns of about 50cm, and both ends were knotted to form a skein (total linear density about 1600 dtex). The upper end of the skein is hung on a hook on a sample table and is balanced for 30min under the environment of normal temperature and normal pressure.
Hanging a heavy weight with a hook at the lower end of the skein to curl and straighten the skein, wherein the skein is stressed by 0.2cN/dtex (320gf) for 10s, and measuring the length L of the skein by using a graduated scaleg(to the nearest 0.01 cm).
Removing the heavy weight, replacing with the light weight, allowing the crimp to reappear, applying force to the skein of 0.001cN/dtex (1.6gf) for 10min, and measuring the skein length Lz。
The formula for calculating the crimping rate is as follows: CC ═ Lg-Lz)/LgThe test was performed 20 times per package, and 15 times with smaller dispersion were taken and averaged.
The composite fiber products prepared by taking two existing processes as comparison examples are compared with the product prepared by the preparation method of the nano-doped polyamide parallel elastic composite fiber, and the obvious effect of the process is remarkable.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, so that any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (6)
1. A preparation method of nano-doped polyamide side-by-side elastic composite fiber is characterized by comprising the following steps:
the parallel elastic composite fiber is formed by spinning a component A and a component B in a parallel mode; the component A is thermoplastic polyamide resin, and the component B is a compound consisting of the thermoplastic polyamide resin and a nano additive;
the nano additive is one or more of nano layered silicate, metal compound and rare earth compound, is doped into polyamide through melt blending or in-situ polymerization, and at least one dimension of the nano additive exists in the polyamide in a nano size, and the adding proportion is 0.5-4 wt%.
2. The method of preparing nano-doped polyamide side-by-side elastic composite fiber according to claim 1, wherein: the nano layered silicate is one or more of montmorillonite, diatomite and attapulgite;
the metal compound is one or more of zinc oxide, zinc chloride, lithium chloride and calcium chloride;
the rare earth compound is one or more of lanthanum oxide, cerium oxide, yttrium chloride, gadolinium trichloride and lanthanum acetate.
3. The method for preparing nano-doped polyamide side-by-side elastic composite fiber according to claim 1, comprising the following steps:
1) the two raw material slices after vacuum drying are respectively sent into an A, B screw extruder, the two melts after melt extrusion are conveyed into a spinning manifold through respective pipelines, then flow through the same spinning manifold and a composite component and are converged in a spinneret plate or at the outlet of the spinneret plate, two melt trickle flows are bonded together, and the two melt trickle flows are cooled by cross air blowing and oiled to form parallel composite fibers;
2) and (3) immediately feeding the cooled and formed fiber into a guiding, stretching and shaping stage, wherein the speed difference between a first hot roller GR1 and a second hot roller GR2 forms the stretching of the fiber, the high-temperature hot box of the second hot roller GR2 carries out heat shaping on the fiber, and the fiber protofilament is obtained through a networking and winding process.
4. The method of preparing nano-doped polyamide side-by-side elastic composite fiber according to claim 1, wherein: the parallel composite spinning is carried out at the temperature of 250-295 ℃, the spinning speed is 3000-5000 m/min, the cooling air temperature is 17-25 ℃, the air speed is 0.20-0.55m/s, and the proportion range of the A/B components is 3: 7-7: 3.
5. the method of preparing nano-doped polyamide side-by-side elastic composite fiber according to claim 4, wherein: the parallel composite spinning can be spun into POY pre-oriented yarns and FDY fully drawn yarns, and the POY pre-oriented yarns can be drawn or elasticated to obtain DT drawn yarns or DTY drawn textured yarns.
6. The method of preparing nano-doped polyamide side-by-side elastic composite fiber according to claim 1, wherein: the filament number of the parallel elastic composite fibers is 1-6dtex, the breaking strength is 2.0-4.5cN/dtex, the crimp shrinkage rate is 30-60%, the crimp stability is 20-80%, and the crimp modulus is 10-20%.
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