CN108588871B - Preparation method for preparing special-shaped high-strength polyamide 6 fiber by near-infrared light induced drafting - Google Patents
Preparation method for preparing special-shaped high-strength polyamide 6 fiber by near-infrared light induced drafting Download PDFInfo
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- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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Abstract
The invention relates to a method for preparing a special-shaped high-strength polyamide 6 fiber by near-infrared light induced drafting, which comprises the following steps: polymerizing nano tungsten oxide or iron sulfide and caprolactam in situ or blending the nano tungsten oxide or iron sulfide and polyamide 6, carrying out melt spinning on a profiled cross section spinneret plate to obtain modified polyamide 6 fiber with a profiled cross section, carrying out secondary drafting or multistage drafting, setting the temperature of a first drafting roller and a second drafting roller to be room temperature, and carrying out continuous near-infrared light irradiation on the fiber between the first drafting roller and the second drafting roller to obtain the modified polyamide 6 fiber. The method is simple and easy to operate, and the effects of high strength and special shape of the fiber are achieved through melt special-shaped spinning and accurate temperature control of the fiber amorphous region; the prepared melt-spun high-strength polyamide 6 fiber is high in mechanical strength, the breaking strength is 8.5-11.5 cN/dtex, and the elongation at break is 13.0-18.0%.
Description
Technical Field
The invention belongs to the field of preparation of special-shaped high-strength fibers, and particularly relates to a preparation method for preparing special-shaped high-strength polyamide 6 fibers by near-infrared light induced drafting.
Background
The special high-strength polyamide 6(PA6) fiber not only has the excellent properties of PA6 fiber such as strength, wear resistance, elastic recovery rate and the like, but also has the excellent characteristics of moisture permeability and air permeability through a special section, so that the special high-strength polyamide 6(PA6) fiber has wide application prospects in special application fields such as military training clothes and naval vessel fabrics. Therefore, the special-shaped high-strength high-modulus polyamide 6 fiber becomes a hot product concerned by polyamide production enterprises and related units.
At present, the high-strength polyamide 6 fiber mainly utilizes the technologies of plasticizing melt spinning, solid-state co-extrusion, dry spinning, zone stretching heat treatment and the like, but the strength and the modulus of the polyamide 6 fiber are not greatly broken through. With the understanding of the effect of polymer chain entanglement and intermolecular hydrogen bond on the inhibition of fiber stretching, the research direction of people gradually turns to that the intermolecular hydrogen bond is eliminated by complexation and the like before gel spinning and stretching to improve the stretching multiple so as to improve the strength and modulus of the fiber. However, the gel spinning and the metal element hydrogen bond complexing method not only increase the number of processes and cause environmental pollution due to the special spinning method, but also directly increase the production cost of the high-strength polyamide 6 fiber.
Understanding the high strength and high modulus of the polyamide 6 fiber shows that if the high strength polyamide 6 fiber is obtained, the hydrogen bond function between the polyamide molecular chains is fully utilized, and the orientation ratio of the molecular chains is increased. At present, the theoretical strength of polyamide 6 is 327cN/dtex and the theoretical modulus is 2442cN/dtex, calculated theoretically; the commercial high-strength polyamide 6 fibers reach 8.0cN/dtex and 88.0cN/dtex respectively, and the breakage is mainly caused by defects and weak points on the supermolecular structure of the fibers. In the process of stretching the fiber, the microcrystals in the polyamide crystal region have enough energy to be stretched and oriented by external force, while the first amorphous part in the fiber crystal structure is stretched, and under the same heating environment, the entanglement molecular chains in the amorphous region of the fiber are broken due to the excessive heat and stretching external force, so that the fiber strength is reduced. Therefore, how to control the thermal relationship between the crystalline region and the amorphous region becomes an important issue for the fiber stretch orientation.
Research shows that nano materials such as tungsten oxide or iron sulfide can generate heat under infrared light due to specific nano size effect (CN102921006B, CN107381644A, literature (J.Am.chem.Soc.2012,134, 3995-3998; doctor's paper: synthesis of organic/inorganic hybrid nano photothermal conversion material and application research thereof in tumor treatment, Menzhou Qi)) and is applied to thermotherapy and chemotherapy of cancer. Therefore, whether the inorganic material with the nanometer size is introduced into the fiber or not can be controlled, the energy conversion of the nanometer particles in the amorphous area is controlled under the action of near infrared light, the amorphous temperature of the fiber is accurately regulated and controlled, and the orientation of the fiber is promoted at room temperature.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing special-shaped high-strength polyamide 6 fibers by near infrared light induced drafting, which utilizes nano-powder such as nano tungsten oxide or iron sulfide and the like dispersed in an amorphous area of special-shaped fibers to preferentially induce the temperature of the amorphous area of the fibers to be increased under the action of near infrared light at room temperature so as to promote the hydrogen bond in the polyamide 6 to be dissociated, and further enables a micro-fiber structure in a crystal area to be oriented in the axial direction of the fibers and the binding molecular chain content of the amorphous area to be increased under the action of external force drafting, thereby improving the mechanical property of the fibers.
The invention relates to a method for preparing special-shaped high-strength polyamide 6 fibers by near-infrared light induced drafting, which comprises the following steps:
(1) polymerizing nano tungsten oxide or ferric sulfide and caprolactam in situ or blending the nano tungsten oxide or ferric sulfide and polyamide 6, and performing melt spinning on a profiled cross section spinneret plate to obtain the modified polyamide 6 fiber with the profiled cross section, wherein the nano material accounts for 0.05-1.0 wt% of the weight of the polyamide 6; the melt spinning temperature is 240-260 ℃;
(2) secondarily drafting the modified polyamide 6 fiber with the special-shaped cross section in the step (1), setting the temperature of a first drafting roller and the temperature of a second drafting roller to be room temperature, and simultaneously carrying out continuous near-infrared light irradiation on the fiber between the first drafting roller and the second drafting roller to obtain a high-strength special-shaped polyamide 6 fiber;
or (2) performing multistage drafting on the modified polyamide 6 fiber with the special-shaped cross section in the step (1), setting the temperature of the first drafting roller and the temperature of the second drafting roller to be room temperature, setting the temperature of the other rollers to be 70-120 ℃, and simultaneously performing continuous near-infrared light irradiation on the fiber between the first drafting roller and the second drafting roller to obtain the high-strength special-shaped polyamide 6 fiber.
The Tungsten Oxide in the step (1) is prepared by referring to patents CN102921006B and CN107381644A and literature (Tunable Localized Surface plasma resources in Tungsten Oxide Nanocrystals, J.Am.chem.Soc.2012,134,3995-3998). For example, 0.35g WCl is weighed6Putting the mixture into a lining of a high-pressure reaction kettle with 100mL of solvent, adding 24mL of absolute ethyl alcohol under the stirring condition, then adding 56mL of PEG400 under the stirring condition, and continuing stirring for half an hour; transferring the mixture into a high-pressure reaction kettle, and reacting for 24 hours at 180 ℃; after the reaction is finished, carrying out centrifugal separation to obtain WO2.72A nanowire.
The iron sulfide reference doctor in the step (1)Preparation of a paper (synthesis of organic/inorganic hybrid nano photothermal conversion material and application research thereof in tumor treatment, menzhouqi): dissolving 96g of sulfur powder in 5L of diphenyl ether, stirring and degassing at 70 ℃ for 1 hour, and marking as solution A; 100g FeCl2·4H2Dissolving O in 10Kg of octadecylamine, degassing at 120 ℃ for 1 hour, heating to 220 ℃ under the protection of nitrogen, adding the solution A, reacting for 3 hours, and cooling to 100 ℃; adding 9L of trichloromethane to prevent the reaction system from solidifying, centrifuging the solution at 4400rpm for 5 minutes to take out large-size particles, and washing the large-size particles by ethanol to obtain the flaky ferric sulfide nanoparticles.
In the step (1), the tungsten oxide is WOx, and x is 2.72-3.0; the iron sulfide is FeS2。
The tungsten oxide in the step (1) is in a nanowire shape; the shape of the iron sulfide is nano-sheet; the particle size of the tungsten oxide or the iron sulfide is about 1 to 200 nm.
The melt spinning process parameters in the step (1) are as follows: the spinning speed is 1000-4000 m/min, the hot roller temperature is 80-90 ℃, and the draw ratio is 1-2.
The special-shaped section in the step (1) is triangular, trefoil, hollow, cross, flat or Y-shaped.
The irradiation power of the near infrared light in the step (2) is 25.0-200.0W/cm2The irradiation distance of the near infrared light is 2-30 cm.
In the step (2), the draft ratio of the first draft roller is 1.05-1.10, the draft ratio of the second draft roller is 1.50-1.70, and the draft ratios of the other rollers are 1.01-2.
The breaking strength of the high-strength profiled polyamide 6 fiber in the step (2) is 8.5-11.5 cN/dtex, and the elongation at break is 13.0-18.0%.
The invention prepares nano materials with a certain size range according to the preparation technology of nano tungsten oxide and iron sulfide in patents CN102921006B and CN107381644A, documents (J.Am.chem.Soc.2012,134,3995-3998) and doctor's papers (synthesis of organic/inorganic hybrid nano photothermal conversion materials and application research thereof in tumor treatment). Then the special-shaped high-strength polyamide 6 fiber is added into polyamide master batches, and a method for preparing the special-shaped high-strength polyamide 6 fiber through temperature-controlled drafting orientation in an amorphous area of the special-shaped fiber is explored through melt special-shaped spinning, so that the idea is improved for the high-strength processing of the general polymer special-shaped fiber.
The invention breaks through the traditional drafting process of the conventional polyamide 6 fiber, utilizes near infrared light to accurately control the temperature of the amorphous area of the fiber crystal structure, realizes the high-order drafting of the fiber and obviously improves the tensile breaking strength of the polyamide 6 fiber.
Advantageous effects
(1) The method is simple and easy to operate, and achieves the effects of high strength and special shape of the fiber through melt special-shaped spinning and accurate temperature control of the fiber amorphous area.
(2) The melt-spun high-strength polyamide 6 fiber prepared by the invention has high mechanical strength, the breaking strength is 8.5-11.5 cN/dtex, and the elongation at break is 13.0-18.0%.
Drawings
FIG. 1 is a scanning electron microscope image of a high-strength cross-section polyamide 6 fiber in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Tungsten oxide WO is prepared with reference to patent CN102921006B2.72A nanowire.
(2) Mixing caprolactam, water and tungsten oxide WO with the size of about 200nm2.72Uniformly mixing the nanowires, wherein the mass ratio of water to caprolactam is 1:1, and tungsten oxide WO2.721 wt% of caprolactam, heating to 255 deg.C, and polymerizing for 18 hours to obtain modified polyamide 6. Drying at 120 deg.C under vacuum drum drying environment for 24 hr, spinning at 3000m/min with cross spinneret (d is 0.3mm) at 240 deg.C, and shaping to obtain the final productA cross-section shaped polyamide 6 fiber having a hot roll temperature of 85 ℃ and a draw ratio of 2.
(3) Drawing the modified cross-section profiled polyamide 6 fiber in the step (2) on a four-stage drawing device, wherein the temperature of a first drawing roller and a second drawing roller is set to be 20 ℃, the temperature of a third drawing roller is set to be 70 ℃, and the temperature of a fourth setting roller is set to be 110 ℃. 200W/cm is adopted for the first drawing roller and the second drawing roller2The near-infrared light source continuously irradiates the fiber, the irradiation distance is controlled to be 2cm, and the nano powder generates instantaneous heat to enable the heat of a local micro-area to reach 80-95 ℃. The first drawing roller has a drawing ratio of 1.10, the second drawing roller has a drawing ratio of 1.50, the third drawing roller has a drawing ratio of 2.0, the heat setting roller has a drawing ratio of 1.01, and after the fiber is drawn in multiple stages, the tensile breaking strength of the cross-section profiled PA6 fiber reaches 10.6cN/dtex (CV value 3.2%), the breaking elongation reaches 17.3% (CV value 6.8%), and the breaking work reaches 23.94 Nx cm. The test data were taken as the average of 20 groups of fiber filament test data, as specified in table 1.
Figure 1 illustrates that the fiber retains a good profile cross section after drawing.
TABLE 1
Example 2
(1) Reference (Tunable Localized Surface plasma reactions in Tungsten oxides Nanocrystals, J.Am. chem. Soc.2012,134,3995-3998) Tungsten Oxide WO was prepared2.80A nanowire.
(2) Mixing PA6 and tungsten oxide WO about 50nm long2.80Nanowire (tungsten oxide WO)2.800.1 wt% of PA6), heating to 250 ℃, and blending by a double screw to obtain the modified polyamide 6. Drying at 120 deg.C under vacuum drum drying environment for 24 hr, spinning at 260 deg.C with triangular spinneret (d ═ 0.3mm) at 1000m/min to obtainModified triangular profiled polyamide 6 fiber, wherein the hot roll temperature is 90 ℃ and the draw ratio is 1.2.
(3) Drawing the modified triangular profiled polyamide 6 fiber in the step (2) on a four-stage drawing device, wherein the temperature of a first drawing roller and a second drawing roller is set to be 20 ℃, the temperature of a third drawing roller is set to be 75 ℃, and the temperature of a fourth setting roller is set to be 120 ℃. The first drawing roller and the second drawing roller adopt 25W/cm2The near-infrared light source continuously irradiates the fiber, the irradiation distance is controlled to be 2cm, and the nano powder generates instantaneous heat to enable the heat of a local micro-area to reach 65-75 ℃. The first drawing roller has a drawing ratio of 1.05, the second drawing roller has a drawing ratio of 1.50, the third drawing roller has a drawing ratio of 2.0, the heat setting roller has a drawing ratio of 1.02, and after the fiber is drawn in multiple stages, the tensile breaking strength of the fiber with the triangular section and the special shape PA6 reaches 9.2cN/dtex, and the breaking elongation of the fiber reaches 17%.
Example 3
(1) The tungsten oxide WO is prepared by referring to the patent CN107381644A3A nanowire.
(2) Mixing caprolactam, water and tungsten oxide WO with the length of about 150nm3.0Uniformly mixing nanowires, wherein water accounts for 2 wt% of the mass of caprolactam, and tungsten oxide WO3.00.6 wt% of caprolactam, heated to 255 ℃ and polymerized for 18 hours to obtain modified polyamide 6. Drying at 120 deg.C under drum vacuum drying environment for 24 hr, and spinning at 240 deg.C with flat or Y-shaped spinneret (d 0.3mm) at 2000m/min to obtain modified flat or Y-shaped section profiled polyamide 6 fiber with hot roll temperature of 85 deg.C and draw ratio of 2.
(3) Drawing the modified flat or Y-shaped section special-shaped polyamide 6 fiber in the step (2) on a four-stage drawing device, wherein the temperature of a first drawing roller and a second drawing roller is set to be 20 ℃, the temperature of a third drawing roller is set to be 70 ℃, and the temperature of a fourth setting roller is set to be 110 ℃. The first drawing roller and the second drawing roller adopt 100W/cm2The near-infrared light source continuously irradiates the fiber, the irradiation distance is controlled to be 30cm, and the nano powder generates instantaneous heat to enable the heat of a local micro-area to reach 65-75 ℃. Wherein the draft ratio of the first drafting roller is 1.05, the draft ratio of the second roller is 1.50, the draft ratio of the third roller is 2.0, the draft ratio of the heat setting roller is 1.01, and the fiber passes through a plurality of rollersAfter the secondary drafting, the tensile breaking strength of the flat or Y-shaped cross section special-shaped PA6 fiber reaches 9.2cN/dtex, and the breaking elongation reaches 14%.
Example 4
(1) The nanometer sheet-shaped iron sulfide FeS is prepared by referring to a doctor paper (synthesis of organic/inorganic hybrid nanometer photothermal conversion material and application research thereof in tumor treatment, Menzhou Qi)2。
(2) Mixing PA6 and FeS flake iron sulfide with the size of about 100nm2(iron sulfide FeS)21 wt% of PA6, heating to 250 ℃, and blending by a double screw to obtain the modified polyamide 6. Drying at 120 deg.C under rotary drum vacuum drying environment for 24 hr, spinning at 260 deg.C with trilobal or hollow section spinneret (d ═ 0.3mm) at 2000m/min to obtain modified trilobal or hollow section polyamide 6 fiber, wherein the temperature of hot roll is 85 deg.C, and the draw ratio is 1.6.
(3) Drawing the modified trilobal or hollow section polyamide 6 fiber in the step (2) on a four-stage drawing device, wherein the temperature of a first drawing roller and a second drawing roller is set to be 20 ℃, the temperature of a third drawing roller is set to be 75 ℃, and the temperature of a fourth setting roller is set to be 120 ℃. The first drawing roller and the second drawing roller adopt 100W/cm2The near-infrared light source continuously irradiates the fiber, the irradiation distance is controlled to be 5cm, and the nano powder generates instantaneous heat to enable the heat of a local micro-area to reach 75-80 ℃. The first drawing roller has a drawing ratio of 1.10, the second drawing roller has a drawing ratio of 1.50, the third drawing roller has a drawing ratio of 2.0, the heat setting roller has a drawing ratio of 1.01, and after the fiber is drawn in multiple stages, the tensile breaking strength of the trilobal or hollow section special-shaped PA6 fiber reaches 10.2cN/dtex, and the breaking elongation of the fiber reaches 18%.
Claims (7)
1. A method for preparing a profiled high-strength polyamide 6 fiber by near-infrared light induced drafting comprises the following steps:
(1) polymerizing nano tungsten oxide or ferric sulfide and caprolactam in situ or blending the nano tungsten oxide or ferric sulfide and polyamide 6, and performing melt spinning on a profiled cross section spinneret plate to obtain the modified polyamide 6 fiber with the profiled cross section, wherein the nano material accounts for 0.05-1.0 wt% of the mass of the caprolactam or the polyamide 6; the melt spinning temperature is 240-260 ℃;
(2) performing secondary drafting on the modified polyamide 6 fiber with the special-shaped cross section in the step (1), setting the temperature of a first drafting roller and the temperature of a second drafting roller to be room temperature, and simultaneously performing continuous near-infrared light irradiation on the fiber between the first drafting roller and the second drafting roller to obtain a high-strength special-shaped polyamide 6 fiber;
or (2) performing multistage drafting on the modified polyamide 6 fiber with the special-shaped cross section in the step (1), setting the temperature of the first drafting roller and the temperature of the second drafting roller to be room temperature, setting the temperature of the other rollers to be 70-120 ℃, and simultaneously performing continuous near-infrared light irradiation on the fiber between the first drafting roller and the second drafting roller to obtain the high-strength special-shaped polyamide 6 fiber.
2. The method for preparing the profiled high-strength polyamide 6 fiber by near infrared light induced drafting according to claim 1, wherein in the step (1), the tungsten oxide is WOx, and x is 2.72 to 3.0; the iron sulfide is FeS2。
3. The method for preparing profiled high-strength polyamide 6 fiber by near infrared light-induced drawing according to claim 1, wherein the tungsten oxide of step (1) is in a shape of a nanowire; the shape of the iron sulfide is nano-sheet; the particle size of the tungsten oxide or the iron sulfide is 1-200 nm.
4. The method for preparing the profiled high-strength polyamide 6 fiber by near infrared light induced drafting according to claim 1, wherein the process parameters of the melt spinning in the step (1) are as follows: the spinning speed is 1000-4000 m/min, the hot roller temperature is 80-90 ℃, and the draw ratio is 1-2.
5. The method for preparing the profiled high-strength polyamide 6 fiber by near-infrared light-induced drawing according to claim 1, wherein the profiled cross section in the step (1) is triangular, trilobal, hollow, cross-shaped, flat or Y-shaped.
6. The method for preparing the profiled high-strength polyamide 6 fiber by near infrared light induced drafting according to claim 1, wherein the irradiation power of the near infrared light in the step (2) is 25.0 to 200.0W/cm2The irradiation distance of the near infrared light is 2-30 cm.
7. The method for preparing the profiled high-strength polyamide 6 fiber by near infrared light induced drafting according to claim 1, wherein the drafting ratio of the first drafting roller in the drafting process in the step (2) is 1.05 to 1.10, the drafting ratio of the second drafting roller is 1.50 to 1.70, and the drafting ratio of the other rollers is 1.01 to 2.
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