Preparation method and application of special color master batch for nylon 66 stock solution coloring fiber

Abstract

The invention provides a preparation method and application of a special color master batch for nylon 66 stock solution colored fibers. The special color master batch for the nylon 66 stock solution colored fiber is prepared from the following raw materials: an organic / inorganic pigment, a powder wetting dispersant, a coupling agent and nylon 66 powder. The organic / inorganic pigment is firstly pretreated to prepare an organic / inorganic pre-dispersed pigment, and then the organic / inorganic pre-dispersed pigment is mixed with the nylon 66 powder, the powder wetting dispersant and the coupling agent to prepare the color master batch. The nylon 66 stock solution coloring fiber prepared from the color master batch is excellent in mechanical property and good in color fastness.

Description

Technical Field

[0001] This invention belongs to the textile field, specifically relating to a method for preparing a special masterbatch for nylon 66 solution-dyed fibers and its application. Background Technology

[0002] The technological bottleneck of relying on imported adiponitrile, the upstream raw material for nylon 66, has been overcome in China, leading to explosive growth in its production and ample supply. However, downstream high-performance, differentiated, and solution-dyed nylon 66 fiber products still require further development. Nylon 66 fiber, with its high strength, excellent abrasion resistance, high melting point, good elasticity, and fatigue resistance, occupies an irreplaceable position in industrial, functional textile, and engineering plastics reinforcement fields. Its superior overall performance makes it a preferred high-performance synthetic fiber, especially in applications requiring stringent abrasion resistance, high strength, and low-temperature resistance. Its relatively good moisture absorption and lightweight softness also give it a place in the high-end apparel sector.

[0003] Compared to traditional dyeing techniques for coloring nylon 66 fiber fabrics, solution-dyed nylon 66 fibers offer several advantages: uniform coloring, excellent colorfastness, high dye uptake, short production cycle, and low cost. Furthermore, processing textiles from solution-dyed fibers eliminates the need for dyeing processes, significantly reducing wastewater and carbon dioxide emissions, resulting in energy conservation, reduced consumption, and environmental friendliness. This effectively addresses the high energy consumption, high water consumption, and high COD emissions prevalent in the traditional dyeing industry. In the context of a green, low-carbon, and environmentally friendly era, nylon 66 solution-dyed fibers, with these advantages, are expected to find applications in the following fields: apparel (knitwear, casual wear, sportswear, etc.); automotive textiles (car interior carpets, car seat covers, etc.); home textiles (curtains, fabrics, carpets, etc.); portable equipment (tents, carrying cases, etc.); industrial textiles (tarpaulins, filter cloths, etc.); and military textiles (training uniforms, combat uniforms, clothing, etc.).

[0004] After years of development in solution dyeing technology, the domestic chemical fiber industry has achieved certain results in polyester and nylon 6 solution dyeing technologies. Currently, polyester and nylon 6 solution-dyed fibers have reached large-scale production, while nylon 66 solution-dyed fibers have not yet reached large-scale mass production technology. The main reasons are as follows: Although nylon 66 has a similar melting point to polyester, unlike the weakly acidic properties of polyester melt, nylon 66 possesses weakly alkaline and reducing properties. Therefore, the colorant or masterbatch system used in polyester solution dyeing cannot be easily transferred to the nylon 66 solution dyeing system. Furthermore, while nylon 66 and nylon 6 have similar acidity, alkalinity, and reducing properties, their physical properties differ due to differences in hydrogen bond arrangement. Nylon 6 exhibits two hydrogen bond arrangements, with approximately 50% of these arrangements consisting of longer and weaker tilted hydrogen bonds. Nylon 66, on the other hand, has only one hydrogen bond arrangement, with its hydrogen bonds arranged in a straight line, forming a strong and dense polymer structure. The atomic arrangement of nylon 66 is more regular than that of nylon 6. The tighter the hydrogen bond arrangement, the higher the crystallinity. Consequently, nylon 66 has a higher melting point (approximately 40°C higher than nylon 6) and slower permeability. Therefore, some dopant coloring systems suitable for nylon 6 are difficult to apply to nylon 66 coloring systems due to insufficient temperature resistance or differences in wetting properties.

[0005] In summary, due to the high processing temperature and chemical properties of nylon 66, existing solution dyeing systems and techniques are not suitable for the production of nylon 66 solution-dyed fibers. Therefore, developing a dedicated masterbatch for nylon 66 solution-dyed fibers is an urgent problem to be solved. Summary of the Invention

[0006] The purpose of this invention is to provide a special masterbatch for nylon 66 solution-dyed fibers and its preparation method, which fills the industry gap for special masterbatches for nylon 66 solution-dyed fibers and solves the problems of poor spinnability and poor mechanical properties in the spinning production of nylon 66 solution-dyed fibers.

[0007] The nylon 66 solution-dyed fiber masterbatch provided by this invention is made from raw materials comprising the following components: organic / inorganic pigments, powder wetting and dispersing agents, coupling agents, and nylon 66 powder.

[0008] By weight percentage: organic / inorganic pigments 5.0–35.0%; powder wetting and dispersing agent 1.0–3.0%; coupling agent 0.1–2.0%; nylon 66 powder balance.

[0009] Specifically, by weight percentage, the nylon 66 solution-dyed fiber masterbatch is made from raw materials comprising the following components: 10.0-20.0% organic / inorganic pigments; 1.0-2.0% powder wetting and dispersing agent; 1.0% coupling agent; and the remainder being nylon 66 powder. More specifically, by weight percentage, the nylon 66 solution-dyed fiber masterbatch is made from raw materials comprising the following components: 10.0% organic / inorganic pigments; 1.0% powder wetting and dispersing agent; 1.0% coupling agent; and the balance being nylon 66 powder. Alternatively, organic / inorganic pigments 20.0%; powder wetting and dispersing agent 2.0%; coupling agent 1.0%; nylon 66 powder balance.

[0010] The present invention relates to a special color masterbatch for solution-dyed nylon 66 fibers, which is a homogeneous nylon 66 special color masterbatch. Organic / inorganic pigments are used as coloring pigments, and powder wetting and dispersing agents can improve the wetting and dispersing effect of pigments; coupling agents are used to stabilize the coloring pigments inside the fiber or in the spinning melt, thereby improving the color fastness of solution-dyed fibers.

[0011] The organic / inorganic pigments are selected from at least one of the following: carbon black, phthalocyanine blue, phthalocyanine green, and perylene red. The powder particle size of the organic / inorganic pigment is ≤0.1μm; The powder wetting and dispersing agent is selected from at least one of polyester, polyether, amide dispersants and ionic polymers, specifically dispersant DP310 and dispersant 18700; The coupling agent is selected from at least one of the following: silane coupling agents, titanate coupling agents, and polymer coupling agents, specifically coupling agent 8104FA; The original particle size of the nylon 66 powder is ≤200.0 μm.

[0012] The present invention also provides a method for preparing the above-mentioned masterbatch for solution-dyed nylon 66 fibers.

[0013] The method for preparing a special masterbatch for nylon 66 solution-dyed fibers provided by the present invention includes the following steps: (1) Pretreatment of organic / inorganic pigments Weigh a mixture of deionized water and ethanol, add a liquid wetting and dispersing agent and stir at low speed, then add the organic / inorganic pigment, increase the stirring speed to 500-1500 rpm, and stir for 20-40 minutes (specifically 30 minutes); let it stand and wet for 12-24 hours to obtain an organic / inorganic pigment pre-dispersion, grind it again to refine the dispersion until the pigment particle size is ≤0.1μm; filter, dry and crush the ground pre-dispersion to obtain the organic / inorganic pre-dispersion pigment; (2) Material mixing Weigh out the above-mentioned organic / inorganic pre-dispersed pigments and nylon 66 powder, powder wetting and dispersing agent and coupling agent, mix them initially, and then mix them at high speed to obtain a uniformly dispersed mixture. (3) Preparation of color masterbatch The above mixture is added to a twin-screw extruder, and the material is conveyed, sheared, melted, and extruded at the set screw speed and screw temperature. The extruded strands are solidified and shaped, and then pelletized to obtain color masterbatch.

[0014] The combination of organic / inorganic pigment pre-dispersion, material uniform mixing, and twin-screw shear dispersion in the above method can effectively achieve uniform dispersion of coloring pigments, avoid a large amount of agglomeration, and thus improve the spinnability of nylon 66 solution-dyed fibers.

[0015] In step (1) of the above method, the mass ratio of deionized water to ethanol in the mixture can be 3-5:1, specifically 3:1 or 5:1; The liquid wetting and dispersing agent can be selected from at least one of cationic surfactants, anionic surfactants, nonionic surfactants, and superdispersants; specifically, it can be at least one of BYK190, BYK191, BYK163, and BYK110. Based on the organic / inorganic pigments comprising 100% by weight, the addition range of the liquid wetting and dispersing agent is 2-15%. The low-speed stirring is achieved by a glass rod stirring. The mass ratio of the organic / inorganic pigment to the mixture can be 1:1-10; The time for allowing the plant to stand and moisten can be 12-24 hours, specifically 24 hours. The grinding time can be 1 to 3 hours.

[0016] In step (2) of the above method, the speed of high-speed stirring can be 100-500 rpm, and the time can be 15-60 min, specifically 30 min.

[0017] In step (3) of the above method, the mixture is added to the 25# twin-screw extruder at a feed rate of 2.0-10.0 kg / h (specifically 5.0 kg / h); The screw speed is set to 200-350 rpm, and the screw temperature range is 220-280℃ for the T1-T8 zone.

[0018] The application of the above-mentioned masterbatch in the preparation of solution-dyed nylon 66 fibers also falls within the scope of protection of this invention.

[0019] The present invention also provides a method for preparing nylon 66 solution-dyed fibers using the above-mentioned masterbatch.

[0020] The method for preparing nylon 66 solution-dyed fibers provided by the present invention includes the following steps: Both the masterbatch and nylon 66 chips are vacuum dried. The dried masterbatch and nylon 66 chips are mixed and added to a single-screw spinning machine to melt. The spinning melt is metered by a metering pump and then extruded into filaments through the spinneret. The fibers are cooled by side air, oiled, and finally drawn and wound to obtain nylon 66 solution-dyed fibers.

[0021] In the above method, after vacuum drying, the moisture content of the masterbatch and nylon 66 chips is controlled at 100-400 ppm. The mass ratio of color masterbatch to nylon 66 chips can be 3-5:100; The screw process temperature is 270–300℃, and the metering pump speed is 12–18 rpm.

[0022] The masterbatch of this invention can be applied to the spinning production of nylon 66 solution-dyed fibers. It not only possesses good spinnability but also exhibits excellent compatibility with nylon 66 chips, enabling the successful preparation of high-performance nylon 66 solution-dyed fibers. The nylon 66 solution-dyed fibers obtained by this invention exhibit excellent mechanical properties and good color fastness. Detailed Implementation

[0023] The present invention will now be described in further detail with reference to specific embodiments. The given embodiments are merely illustrative of the invention and not intended to limit its scope. The embodiments provided below can serve as a guide for further improvements by those skilled in the art and do not constitute a limitation on the invention in any way.

[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0025] Example 1: Preparation of black masterbatch for Nylon 66 solution-dyed fibers (1) Pigment pretreatment: Weigh a mixture of 750g deionized water and 250g ethanol into a mixing tank, add 10wt% (based on the mass of carbon black pigment being 100%) of liquid wetting and dispersing agent (BYK-190), and stir evenly with a glass rod. Then, slowly add 350g of carbon black pigment under low-speed stirring with a top stirrer, and then increase the stirring speed to 1500rpm for about 30 minutes. Finally, let it stand for 24 hours to wet. The carbon black predispersed liquid obtained above is further refined and dispersed using a sand mill for 2.5 hours. The grinding is completed when the particle size of the pigment particles is ≤0.1μm. After filtration, drying, and crushing, the predispersed carbon black pigment can be successfully obtained and finally vacuum packaged.

[0026] (2) Material mixing: Weigh 300g of the above predispersed carbon black pigment, 2640g of nylon 66 powder, 30g of dispersant (18700) and 30g of coupling agent 8104 FA and mix them initially. Then transfer them to a high-speed mixer and mix them at a stirring speed of 350rpm for 30 minutes to obtain a uniformly dispersed mixture.

[0027] (3) Preparation process of black masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature T1-T8 zone is 220~280℃. The material is conveyed, sheared and melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain black masterbatch 1#.

[0028] Example 2: Preparation of Nylon 66 solution-dyed (black) fibers Both black masterbatch #1 and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The masterbatch and nylon 66 chips were mixed at an addition ratio of 3% (3g masterbatch to 97g nylon 66 chips) and added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed was 3710 m / min; the fibers were then networked using a networker and finally wound into shape. No filament drift, fuzz, or breakage occurred during the fiber spinning process with this black masterbatch, successfully producing solution-dyed (black) nylon 66 fibers, designated F1.

[0029] Example 3: Preparation of Red Masterbatch for Nylon 66 Solution-Dyed Fibers (1) Pigment pretreatment: Weigh a mixture of 750g deionized water and 250g ethanol into a mixing tank, add 10wt% (based on the mass of perylene red pigment being 100%) of liquid wetting and dispersing agent (BYK-190), and stir evenly with a glass rod. Then, slowly add 350g of perylene red pigment under low-speed stirring with a top stirrer, and then increase the stirring speed to 1000rpm for about 30 minutes. Finally, let it stand for 24 hours to wet. The pre-dispersed perylene red pigment obtained above is further refined and dispersed using a sand mill for 2 hours. The grinding is completed when the particle size of the pigment particles is ≤0.1μm. After filtration, drying, and crushing, the pre-dispersed perylene red pigment can be successfully obtained and finally vacuum packaged.

[0030] (2) Material mixing: Weigh 300g of the above-mentioned predispersed perylene red pigment, 2640g of nylon 66 powder, 30g of dispersant DP310 and 30g of coupling agent 8104 FA and mix them initially. Then transfer them to a high-speed mixer and mix them at a stirring speed of 350rpm for 30 minutes to obtain a uniformly dispersed mixture.

[0031] (3) Preparation process of red masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature is 220-280℃ in the T1-T8 zone. The material is conveyed, sheared and melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain red masterbatch.

[0032] Example 4: Preparation of Nylon 66 solution-dyed (red) fibers Both the red masterbatch and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The red masterbatch was mixed with nylon 66 chips at an addition ratio of 3%, and then added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60 mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed was 3710 m / min; the fiber was then networked using a networker and finally wound into shape. No filament drift, fuzz, or breakage occurred during the fiber spinning process with this red masterbatch, successfully producing solution-dyed (red) nylon 66 fiber, designated F2.

[0033] Example 5: Preparation of blue masterbatch for solution-dyed nylon 66 fibers (1) Pigment pretreatment: Weigh 750g of a mixture of deionized water and 250g of ethanol into a mixing tank, add 10% of liquid wetting and dispersing agent BYK-190 and stir evenly with a glass rod. Then, slowly add 350g of phthalocyanine blue pigment under low-speed stirring with a top stirrer, and then increase the stirring speed to 1000rpm for about 30 minutes. Finally, let it stand for 24 hours to wet. The phthalocyanine blue predispersed solution obtained above is further refined and dispersed using a sand mill for 2 hours. The grinding is completed when the particle size of the pigment particles is ≤0.1μm. After filtration, drying and crushing, the predispersed phthalocyanine blue pigment can be successfully obtained and finally vacuum packaged.

[0034] (2) Material mixing: Weigh 300g of the above pre-dispersed phthalocyanine blue pigment, 2640g of nylon 66 powder, 30g of dispersant DP310 and 30g of coupling agent 8104 FA and mix them initially. Then transfer them to a high-speed mixer and mix them at a stirring speed of 350rpm for 30 minutes to obtain a uniformly dispersed mixture.

[0035] (3) Preparation process of blue masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature T1-T8 zone is 220~280℃. The material is conveyed, sheared and melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain blue masterbatch.

[0036] Example 6: Preparation of Nylon 66 solution-dyed (blue) fibers Both the blue masterbatch and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The blue masterbatch was mixed with nylon 66 chips at an addition ratio of 3%, and then added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60 mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed was 3710 m / min; the fibers were then networked using a networker and finally wound into shape. No filament drift, fuzz, or breakage occurred during the fiber spinning process with this blue masterbatch, successfully producing solution-dyed (blue) nylon 66 fibers, designated F3.

[0037] Example 7: Preparation of Green Masterbatch for Nylon 66 Solution-Dyed Fibers (1) Pigment pretreatment: Weigh 750g of a mixture of deionized water and 250g of ethanol into a mixing tank, add 10% of liquid wetting and dispersing agent BYK-190 and stir evenly with a glass rod. Then, slowly add 350g of phthalocyanine green pigment under low-speed stirring with a top stirrer, and then increase the stirring speed to 1000rpm for about 30 minutes. Finally, let it stand for 24 hours to wet. The phthalocyanine green predispersed solution obtained above is further refined and dispersed using a sand mill for 2 hours. The grinding is completed when the particle size of the pigment particles is ≤0.1μm. After filtration, drying and crushing, the predispersed phthalocyanine green pigment can be successfully obtained and finally vacuum packaged.

[0038] (2) Material mixing: Weigh 300g of the above pre-dispersed phthalocyanine green pigment, 2640g of nylon 66 powder, 30g of dispersant 18700 and 30g of coupling agent 8104 FA and mix them initially. Then transfer them to a high-speed mixer and mix them at a stirring speed of 350rpm for 30 minutes to obtain a uniformly dispersed mixture.

[0039] (3) Preparation process of green masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature is 220-280℃ in the T1-T8 zone. The material is conveyed, sheared and melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain green masterbatch.

[0040] Example 8: Preparation of Nylon 66 solution-dyed (green) fibers Both the green masterbatch and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The green masterbatch was mixed with nylon 66 chips at an addition ratio of 3%, and then added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60 mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed was 3710 m / min; the fiber was then networked using a networker and finally wound into shape. No filament drift, fuzz, or breakage occurred during the fiber spinning process with this green masterbatch, successfully producing solution-dyed (green) nylon 66 fiber, designated F4.

[0041] Example 9: Preparation of black masterbatch for Nylon 66 solution-dyed fibers (1) Pigment pretreatment: Weigh a mixture of 2.5 kg of deionized water and 0.5 kg of ethanol into a mixing tank, add 25% (based on the mass of carbon black pigment being 100%) of liquid wetting and dispersing agent (BYK-190), and stir evenly with a glass rod. Then, slowly add 1.5 kg of carbon black pigment under low-speed stirring with a top stirrer, and then increase the stirring speed to 1500 rpm for about 30 minutes. Finally, let it stand for 24 hours to wet. The carbon black predispersed liquid obtained above is finely dispersed in batches using a sand mill and ground for 2.5 hours. The grinding is stopped when the particle size of the pigment particles is ≤0.1 μm. After filtration, drying, and crushing, the predispersed carbon black pigment can be successfully obtained and finally vacuum packaged.

[0042] (2) Material mixing: Weigh 1.2 kg of the above pre-dispersed carbon black pigment, 4.62 kg of nylon 66 powder, 0.12 kg of dispersant (18700) and 0.06 kg of coupling agent 8104 FA and mix them initially. Then transfer them to a high-speed mixer and mix them at a stirring speed of 350 rpm for 30 minutes to obtain a uniformly dispersed mixture.

[0043] (3) Preparation process of black masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature is 220-280℃ in the T1-T8 zone. The material is conveyed, sheared, melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain black masterbatch.

[0044] Example 10: Preparation of Nylon 66 solution-dyed (black) fibers Both the black masterbatch and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The masterbatch was mixed with nylon 66 chips at an addition ratio of 3.5% (referring to 3.5g of masterbatch and 96.5g of nylon 66), and then added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed was 3710 m / min; the fibers were then networked using a networker and finally wound into shape. No filament drift, fuzz, or breakage occurred during the fiber spinning process with this black masterbatch, successfully producing solution-dyed (black) nylon 66 fibers, designated F5.

[0045] Table 1. Experimental formulation design of color masterbatches in Examples 1, 3, 5, 7, and 9. Weight percentage (wt%)

[0046] Comparative Example 1: Preparation of Black Masterbatch for Nylon 66 Solution-Dyed Fibers (1) Material mixing: Weigh 300g of untreated carbon black pigment and 2640g of nylon 66 powder, 30g of dispersant (18700) and 30g of coupling agent 8104 FA for initial mixing, then transfer to a high-speed mixer and mix for 30 minutes at a stirring speed of 350rpm to obtain a uniformly dispersed mixture.

[0047] (2) Preparation process of black masterbatch: The above mixture is fed into a 25# twin-screw extruder at a feed rate of 5.0 kg / h. The screw speed is set to 350 rpm and the screw temperature T1-T8 zone is 220~280℃. The material is conveyed, sheared and melted and extruded. The extruded strip is solidified in a water bath and then pelletized by a pelletizer to obtain black masterbatch 2#.

[0048] Comparative Example 2: Preparation of Nylon 66 solution-dyed (black) fibers Both black masterbatch #2 and nylon 66 chips were vacuum dried, with the moisture content controlled between 100 and 400 ppm. The masterbatch was mixed with nylon 66 chips at a 3% addition ratio and added to the hopper above the screw feed inlet. The melt spinning equipment used was an SJ-60×30 high-torque single-screw compounding extruder with a screw diameter of 60 mm, a screw length-to-diameter ratio of 30:1, and a total of 7 heating zones. After the temperature of each heating zone of the single screw reaches the set temperature (270-300℃), the spinning chips are fed into the screw through the feed port and conveyed and melted. The spun melt is filtered and metered by a metering pump, and then extruded into filaments by a spinneret (a total of 34 spinneret holes, each with a diameter of 0.23mm, an aspect ratio of 2.0, and concentrically distributed). The filaments are then cooled and shaped under the action of side blowing air (temperature 25℃, wind speed 0.45m / s), oiled through an oil nozzle, and then drawn and heat-set by heated rollers. The drawing speeds of the first, second, third, fourth, and fifth drawing rollers are 1360m / min, 2800m / min, 3600m / min, 3900m / min, 3850m / min, and 3900m / min, respectively. The winding speed is 3710 m / min; and the fibers are then networked using a networker and finally wound into shape. Occasionally, this black masterbatch exhibits filament drift, fuzz, or breakage during fiber spinning, resulting in solution-dyed (black) Nylon 66 fibers, designated F6.

[0049] Test results of relevant properties of F1~F6 Nylon 66 solution-dyed fibers: The nylon 66 solution-dyed fiber products prepared above all have a specification of 40D / 34F. The mechanical properties of the fibers were tested according to the standard GB / T14344-2022, "Test Method for Tensile Properties of Chemical Fiber Filaments". The color fastness to washing of the fibers or fabrics was tested according to the standard GB / T 5713-2013, "Textiles - Tests for Color Fastness - Water Fastness". The color fastness to sunlight of the fibers or fabrics was tested according to the standard GB / T 8427-2019, "Textiles - Tests for Color Fastness - Artificial Light Fastness: Xenon Arc - Controlled". The color fastness to rubbing of the fibers or fabrics was tested according to the standard GB / T 3920-2008, "Textiles - Tests for Color Fastness - Rubbing Fastness". All test results are average values, and are listed below.

[0050] Table 2. Results of fiber mechanical strength and color fastness tests

[0051] As shown in Table 2, if pigments are not pretreated, they may agglomerate during the preparation of masterbatches due to insufficient wetting and dispersion of pigment particles. This results in larger pigment particle sizes, which can lead to stress concentration points during fiber spinning and stretching. Consequently, fibers are prone to fuzzing, breakage, or sparse strands, thus affecting the mechanical strength and color fastness of the fibers.

[0052] The present invention has been described in detail above. Those skilled in the art will recognize that the invention can be practiced in a wide range of ways with equivalent parameters, concentrations, and conditions without departing from its spirit and scope, and without requiring unnecessary experiments. While specific embodiments have been provided, it should be understood that further modifications can be made to the invention. In summary, according to the principles of the invention, this application is intended to include any changes, uses, or improvements to the invention, including changes made using conventional techniques known in the art that depart from the scope disclosed herein.

Claims

1. A color masterbatch made from raw materials comprising: organic / inorganic pigments, powder wetting and dispersing agents, coupling agents and nylon 66 powder.

2. The masterbatch according to claim 1, characterized in that, By weight percentage: organic / inorganic pigments 5.0–35.0%; powder wetting and dispersing agent 1.0–3.0%; coupling agent 0.1–2.0%; nylon 66 powder balance.

3. The masterbatch according to claim 1, characterized in that, The organic / inorganic pigments are selected from at least one of the following: carbon black, phthalocyanine blue, phthalocyanine green, and perylene red. The powder particle size of the organic / inorganic pigment is ≤0.1μm.

4. The masterbatch according to claim 1, characterized in that, The powder wetting and dispersing agent is selected from at least one of polyester, polyether, amide dispersants and ionic polymers; The coupling agent is selected from at least one of the following: silane coupling agents, titanate coupling agents, and polymer coupling agents; The original particle size of the nylon 66 powder is ≤200.0 μm.

5. A method for preparing the color masterbatch according to any one of claims 1-4, comprising the following steps: (1) Pretreatment of organic / inorganic pigments Weigh a mixture of deionized water and ethanol, add a liquid wetting and dispersing agent and stir at low speed, add the organic / inorganic pigment, increase the stirring speed to 500-1500 rpm, and stir for 20-40 min; let it stand and wet for 12-24 hours to obtain an organic / inorganic pigment pre-dispersion, grind it again to refine the dispersion until the pigment particle size is ≤0.1μm; filter, dry and crush the ground pre-dispersion to obtain the organic / inorganic pre-dispersion pigment; (2) Material mixing Weigh out the above-mentioned organic / inorganic pre-dispersed pigments and nylon 66 powder, powder wetting and dispersing agent and coupling agent, mix them initially, and then mix them at high speed to obtain a uniformly dispersed mixture. (3) Preparation of color masterbatch The above mixture is added to a twin-screw extruder, and the material is conveyed, sheared, melted, and extruded at the set screw speed and screw temperature. The extruded strands are solidified and shaped, and then pelletized to obtain color masterbatch.

6. The method according to claim 5, characterized in that, In step (1), the mass ratio of deionized water to ethanol in the mixture is 3-5:1; The liquid wetting and dispersing agent is selected from at least one of cationic surfactants, anionic surfactants, nonionic surfactants, and hyperdispersants; Based on the organic / inorganic pigments comprising 100% by weight, the wetting and dispersing agent is added in the range of 2-15%. The mass ratio of the organic / inorganic pigment to the mixture is 1:1-10; The time for allowing the mixture to stand and moisten is 12-24 hours. The grinding time is 1 to 3 hours.

7. The method according to claim 5, characterized in that, In step (2), the high-speed stirring speed is 100-500 rpm and the time is 15-60 min; In step (3) of the above method, the mixture is added to the 25# twin-screw extruder at a feed rate of 2.0-10.0 kg / h; The screw speed is set to 200-350 rpm, and the screw temperature range is 220-280℃ for the T1-T8 zone.

8. The application of the masterbatch according to any one of claims 1-4 in the preparation of nylon 66 solution-dyed fibers.

9. A method for preparing nylon 66 solution-dyed fibers, comprising the following steps: The masterbatch and nylon 66 chips as described in any one of claims 1-4 are subjected to vacuum drying. The dried masterbatch and nylon 66 chips are mixed and added to a single-screw spinning machine to melt. The spinning melt is metered by a metering pump and then extruded into filaments through the spinneret. The filaments are cooled by side air, oiled, and finally drawn and wound to obtain nylon 66 solution-dyed fibers.

10. The method according to claim 9, characterized in that, After vacuum drying, the moisture content of the masterbatch and nylon 66 chips is controlled at 100-400 ppm. The mass ratio of color masterbatch to nylon 66 chips is 3-5:100; The screw process temperature is 270–300℃, and the metering pump speed is 12–18 rpm.

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