Anti-pilling polymer composite fiber and preparation and application thereof
By introducing silicone resin and hydroxylated boron nitride nanosheets into polymer composite fibers, anti-pilling polymer composite fibers were prepared, solving the pilling problem of melt-spun fiber fabrics and achieving excellent anti-pilling performance and application of white fibers.
Patent Information
- Application Number
- CN202511076809.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-01
- Publication Date
- 2025-11-14
AI Technical Summary
Existing melt-spun polymer fiber fabrics have poor anti-pilling and anti-fuzzing properties, which affects the appearance quality and service life of the products.
Silicone resin and hydroxylated boron nitride nanosheets were introduced into polymer composite fibers, and anti-pilling polymer composite fibers were prepared by melt extrusion and spinning processes to improve the self-lubricating properties and interfacial bonding strength of the fibers.
It significantly improves the anti-pilling performance of the fiber, with an anti-pilling grade of up to 4.5. At the same time, the fiber is white, which reduces the limitations of color on the use of fabric.
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Figure CN120945514A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of textiles, and specifically relates to an anti-pilling polymer composite fiber and its preparation and application. Background Technology
[0002] Melt-spun polymer fibers, such as polyester, nylon, and polypropylene, offer advantages such as simple production processes, highly controllable properties, good chemical stability and durability, and low cost, making them widely used in textiles, apparel, automotive interiors, medical and health products, and composite materials. However, fabrics made from melt-spun polymer fibers often exhibit poor anti-pilling properties, affecting the appearance quality and lifespan of these products over long-term use. Therefore, developing melt-spun polymer fibers with excellent anti-pilling properties is significant in both responding to market demands and promoting green and sustainable development. Summary of the Invention
[0003] The technical problem to be solved by the present invention is to provide an anti-pilling polymer composite fiber and its preparation and application.
[0004] This invention provides an anti-pilling polymer composite fiber, wherein the composite fiber comprises 5-20% anti-pilling material and 80-95% polymer by mass percentage; wherein the anti-pilling material comprises silicone resin, hydroxylated boron nitride nanosheets and polymer.
[0005] Preferably, by mass percentage, the composite fiber component comprises 10-20% anti-pilling material and 80-90% polymer.
[0006] The anti-pilling material is an anti-pilling masterbatch.
[0007] The polymers mentioned are all melt-spun polymers, and each polymer includes one or more of polyester, polyamide, polypropylene, and polyethylene.
[0008] The polyester includes one or more of polyethylene terephthalate (PET), polypropylene terephthalate (PTT), and polybutylene terephthalate (PBT).
[0009] The anti-pilling masterbatch has a length of 3~5 mm.
[0010] Preferably, the molecular weight of the silicone resin is 600,000 to 800,000, and more preferably, it is 600,000 to 700,000.
[0011] Preferably, the diameter of the hydroxylated boron nitride nanosheets is 1~10 µm.
[0012] The preparation method of the hydroxylated boron nitride nanosheets:
[0013] Boron nitride was dispersed in mixed solution A, sonicated for 0.5-5 hours, and then allowed to stand. The supernatant after standing was filtered and dried to obtain few-layer boron nitride nanosheets. The prepared few-layer boron nitride nanosheets were dispersed in mixed solution B, stirred at room temperature, diluted, washed, filtered, and dried to obtain hydroxylated boron nitride nanosheets. Mixed solution A was a mixture of isopropanol and deionized water; mixed solution B was a mixture of concentrated sulfuric acid and hydrogen peroxide.
[0014] Further, mixed solution A is isopropanol and deionized water in a volume ratio of 1:1; mixed solution B is concentrated sulfuric acid and hydrogen peroxide in a volume ratio of 3:2; wherein the standing time is 8-12 hours; and the stirring time is 2-5 hours.
[0015] Preferably, the mass ratio of silicone resin, hydroxylated boron nitride nanosheets, and polymer in the anti-pilling material is 1~5:1~5:90~98.
[0016] This invention provides a method for preparing any of the described anti-pilling polymer composite fibers, comprising:
[0017] (1) Mix silicone resin, hydroxylated boron nitride nanosheets, polymer and dispersant to obtain a mixture, melt extrusion granulation to obtain anti-pilling polymer masterbatch;
[0018] (2) Mix the anti-pilling polymer masterbatch and polymer chips, and melt spin them to obtain anti-pilling polymer composite fiber.
[0019] In step (1), the dispersant is polyethylene grafted with maleic anhydride; the content of the dispersant in the mixture is 0.5~3wt%.
[0020] The melt extrusion granulation temperature in step (1) can be selected according to the actual situation.
[0021] The melt extrusion granulation temperature in step (1) is 180 ℃~280 ℃.
[0022] In step (2), the mass ratio of anti-pilling polymer masterbatch to polymer chips is 5~20:80~95.
[0023] In step (2), the anti-pilling polymer masterbatch is dried at a temperature of 80-140°C for 8-10 hours.
[0024] In step (2), the polymer chips are dried at a temperature of 80-170 °C for 6-8 hours.
[0025] The melt spinning temperature in step (2) can be selected according to the actual situation.
[0026] In step (2), the melt spinning temperature is 200 ℃~295 ℃ and the spinning assembly pressure is 8~10 MPa.
[0027] The anti-pilling polymer composite fiber has a specification of 150D / 48F.
[0028] The present invention provides a textile comprising any of the aforementioned anti-pilling polymer composite fibers.
[0029] This invention provides an application of any of the described anti-pilling polymer composite fibers or textiles in the fields of clothing, automotive interiors, and outdoor protective equipment.
[0030] This invention introduces silicone resin and hydroxylated boron nitride nanosheets into polymer composite fibers. The hydroxylated boron nitride nanosheets exhibit better compatibility with the polymer matrix, facilitating better dispersion and improving the interfacial bonding strength between them. The polymer composite fiber obtained by silicone resin synergistically combining hydroxylated boron nitride nanosheets possesses excellent self-lubricating and abrasion resistance, while reducing friction between the fiber and the contact surface, thereby effectively improving the anti-pilling performance of the polymer composite fiber. Furthermore, the anti-pilling polymer composite fiber is white, reducing the limitations imposed by the fiber's own color on subsequent fabric applications.
[0031] Beneficial effects
[0032] The anti-pilling fiber of this invention exhibits excellent anti-pilling properties, with an anti-pilling rating of up to 4.5. Furthermore, the anti-pilling polymer composite fiber is white, which reduces the limitations imposed by the fiber's own color on subsequent fabric applications. Attached Figure Description
[0033] Figure 1 The figures show the results of the anti-pilling test; (a) the anti-pilling test results of Example 1; (b) the anti-pilling test results of Example 2; (c) the anti-pilling test results of Example 3; (d) the anti-pilling test results of Example 4; (e) the anti-pilling test results of Example 5; (f) the anti-pilling test results of Example 6; (g) the anti-pilling test results of Comparative Example 1; (h) the anti-pilling test results of Comparative Example 2; (i) the anti-pilling test results of Comparative Example 3; and (j) the anti-pilling test results of Comparative Example 4. Detailed Implementation
[0034] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.
[0035] Test Method: Pilling resistance was tested according to GB / T 4802.2—2008 "Textiles - Determination of Pilling Properties - Part 2: Modified Martindale Method". The sample diameter was 140 mm, the abrasive was standard wool fabric, the load pressure was 12 kPa, and the number of abrasion cycles was 7000. Each sample was tested 3 times. Pilling Grade: Grade 5: No change; Grade 4: Slight pilling / light fuzzing; Grade 3: Moderate pilling / moderate fuzzing, with balls of different sizes and densities covering part of the sample surface; Grade 2: Significant pilling / fuzzing, with balls of different sizes and densities covering most of the sample surface; Grade 1: Severe pilling / fuzzing, with balls of different sizes and densities covering the entire sample surface.
[0036] The dispersant used in the examples and comparative examples was polyethylene grafted maleic anhydride, purchased from Shanghai Maclean Biochemical Technology Co., Ltd.
[0037] The polyester used in the examples and comparative examples was polyethylene terephthalate (PET), which was purchased from Hengli Petrochemical Co., Ltd.
[0038] Boron nitride powder with a flake diameter of 1~3µm was purchased from Shanghai Titan Technology Co., Ltd.
[0039] Boron nitride powder with a particle size of 5-10µm was purchased from Shanghai Titan Technology Co., Ltd.
[0040] Example 1
[0041] (1) Preparation of inorganic lubricant hydroxylated boron nitride nanosheets.
[0042] Boron nitride powder with a diameter of 1-3 µm was dispersed in a mixed solution of isopropanol and deionized water at a volume ratio of 1:1. After sonication for 4 h, the solution was allowed to stand for 12 h. The supernatant after standing was filtered and dried to obtain few-layer boron nitride nanosheets. The prepared few-layer boron nitride nanosheets were dispersed in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:2. After stirring at room temperature for 4 h, the solution was diluted, washed, filtered, and dried to obtain hydroxylated boron nitride nanosheets with a diameter of approximately 1-3 µm.
[0043] (2) Preparation of anti-pilling polyester masterbatch.
[0044] Organic polymer lubricant silicone resin with a molecular weight of 600,000, inorganic lubricant hydroxylated boron nitride nanosheets with a sheet diameter of 1~3µm, and polyester powder were dried separately and then mixed evenly in a high-speed mixer at a mass ratio of 2.5:2.5:95. 1 wt% dispersant was added, and the mixture was melt-extruded and granulated by a twin-screw extruder to prepare anti-pilling polyester masterbatch. The granulation temperature range was 240~270℃.
[0045] (3) Preparation of anti-pilling polyester composite fiber
[0046] The anti-pilling polyester masterbatch prepared above was dried at 120 ℃ for 8 h, and the polyester chips were dried at 170 ℃ for 8 h. They were then mixed evenly at a mass ratio of 5:95 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10MPa to obtain anti-pilling polyester composite fiber.
[0047] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0048] Example 2
[0049] The preparation method is the same as in Example 1, except that the preparation of anti-pilling polyester composite fiber in step (3) is different.
[0050] The preparation of anti-pilling polyester composite fiber is as follows: anti-pilling polyester masterbatch is dried at 120 ℃ for 8 h, and polyester chips are dried at 170 ℃ for 8 h. They are then mixed evenly at a mass ratio of 10:90 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0051] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0052] Example 3
[0053] The preparation method is the same as in Example 1, except that the preparation of anti-pilling polyester composite fiber in step (3) is different.
[0054] The preparation of anti-pilling polyester composite fiber is as follows: anti-pilling polyester masterbatch is dried at 120 ℃ for 8 h, and polyester chips are dried at 170 ℃ for 8 h. They are then mixed evenly at a mass ratio of 15:85 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0055] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0056] Example 4
[0057] The preparation method is the same as in Example 1, except that the preparation of the anti-pilling polyester composite fiber in step (3) is different.
[0058] The preparation of anti-pilling polyester composite fiber is as follows: anti-pilling polyester masterbatch is dried at 120 ℃ for 8 h, and polyester chips are dried at 170 ℃ for 8 h. They are then mixed evenly at a mass ratio of 20:80 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0059] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0060] Example 5
[0061] (1) Preparation of inorganic lubricant hydroxylated boron nitride nanosheets.
[0062] Boron nitride powder with a sheet diameter of 5-10 µm was dispersed in a mixed solution of isopropanol and deionized water at a volume ratio of 1:1. After sonication for 4 h, the solution was allowed to stand for 12 h. The supernatant after standing was filtered and dried to obtain few-layer boron nitride nanosheets. The prepared few-layer boron nitride nanosheets were dispersed in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at a volume ratio of 3:2. After stirring at room temperature for 4 h, the solution was diluted, washed, filtered, and dried to obtain hydroxylated boron nitride nanosheets with a sheet diameter of approximately 5-10 µm.
[0063] (2) Preparation of anti-pilling polyester masterbatch.
[0064] Organic polymer lubricant silicone resin with a molecular weight of 600,000, inorganic lubricant hydroxylated boron nitride nanosheets with a sheet diameter of 5~10µm, and polyester powder were dried separately and then mixed evenly in a high-speed mixer at a mass ratio of 2.5:2.5:95. 1 wt% dispersant was added, and the mixture was melt-extruded and granulated by a twin-screw extruder to prepare anti-pilling polyester masterbatch. The granulation temperature range was 240~270℃.
[0065] (3) Preparation of anti-pilling polyester composite fiber
[0066] The anti-pilling polyester masterbatch prepared above was dried at 120 ℃ for 8 h, and the polyester chips were dried at 170 ℃ for 8 h. They were then mixed evenly at a mass ratio of 5:95 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0067] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0068] Example 6
[0069] The preparation method is the same as in Example 4, except that the preparation of the anti-pilling polyester masterbatch in step (2) is different.
[0070] The preparation of the anti-pilling polyester masterbatch: Organic polymer lubricant silicone resin with a molecular weight of 800,000, inorganic lubricant hydroxylated boron nitride nanosheets with a sheet diameter of 1~3µm, and polyester powder were dried separately, then mixed evenly in a high-speed mixer at a mass ratio of 2.5:2.5:95. 1wt% dispersant was added, and the mixture was melt-extruded and granulated using a twin-screw extruder to obtain the anti-pilling polyester masterbatch. The granulation temperature range was 240~270 ℃.
[0071] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0072] Comparative Example 1
[0073] (1) Preparation of inorganic lubricant hydroxylated boron nitride nanosheets, same as in Example 1.
[0074] (2) Preparation of anti-pilling polyester masterbatch.
[0075] Inorganic lubricant hydroxylated boron nitride nanosheets with a diameter of 1~3µm and polyester powder were dried separately, then mixed evenly in a high-speed mixer at a mass ratio of 5:95. 1wt% of dispersant was added, and the mixture was melt-extruded and granulated in a twin-screw extruder to prepare anti-pilling polyester masterbatch. The granulation temperature range was 240~270 ℃.
[0076] (3) Preparation of anti-pilling composite polyester fiber
[0077] The anti-pilling polyester masterbatch prepared above was dried at 120 ℃ for 8 h, and the polyester chips were dried at 170 ℃ for 8 h. They were then mixed evenly at a mass ratio of 10:90 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0078] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0079] Comparative Example 2
[0080] (1) Preparation of anti-pilling polyester masterbatch.
[0081] Untreated boron nitride powder with a flake diameter of 1-3µm, silicone resin (organic polymer lubricant with a molecular weight of 600,000), and polyester powder were dried separately and then mixed evenly in a high-speed mixer at a mass ratio of 2.5:2.5:95. 1 wt% dispersant was added, and the mixture was melt-extruded and granulated using a twin-screw extruder to obtain anti-pilling polyester masterbatch at a granulation temperature of 240-270 ℃.
[0082] (2) Preparation of anti-pilling polyester composite fiber
[0083] The anti-pilling polyester masterbatch prepared above was dried at 120 ℃ for 8 h, and the polyester chips were dried at 170 ℃ for 8 h. They were then mixed evenly at a mass ratio of 10:90 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0084] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0085] Comparative Example 3
[0086] (1) Preparation of anti-pilling polyester masterbatch.
[0087] Organic polymer lubricant silicone resin with a molecular weight of 600,000 and polyester powder were dried separately and then mixed evenly in a high-speed mixer at a mass ratio of 5:95. 1 wt% dispersant was added, and the mixture was melt-extruded and granulated by a twin-screw extruder to obtain anti-pilling polyester masterbatch. The granulation temperature range was 240~270℃.
[0088] (2) Preparation of anti-pilling polyester composite fiber
[0089] The anti-pilling polyester masterbatch prepared above was dried at 120 ℃ for 8 h, and the polyester chips were dried at 170 ℃ for 8 h. They were then mixed evenly at a mass ratio of 10:90 and spun through a melt spinning system at a spinning temperature of 275 ℃~280 ℃, with a spinning specification of 150D / 48F and a spinning component pressure of 10 MPa to obtain anti-pilling polyester composite fiber.
[0090] The anti-pilling polyester composite fiber prepared above was knitted into a knitted fabric using a knitting machine, and then its anti-pilling performance was tested.
[0091] Comparative Example 4
[0092] Preparation of conventional polyester fibers
[0093] Polyester chips were dried at 170 °C for 8 hours and then spun using a melt spinning system at a temperature of 275 °C to 280 °C. The spinning specifications were 150D / 48F, and the pressure of the spinning assembly was 10 MPa, thus obtaining conventional polyester fibers.
[0094] The conventional polyester fibers were knitted into fabrics using a knitting machine, and then their anti-pilling properties were tested.
[0095] Table 1. Pilling and fuzzing test results of the examples and comparative examples
[0096] As can be seen from Table 1, Examples 2-6 are all superior to Comparative Examples 1-4.
[0097] The test results images show that Comparative Example 4 exhibits the most severe pilling, with fuzz balls of varying sizes covering almost the entire surface of the sample. Comparative Examples 2 and 3 show similar results, with fuzz balls covering only a portion of the sample surface. Comparative Example 1 shows a slightly better fuzz ball coverage rate than Comparative Examples 2 and 3. Example 1 shows a significant improvement over Comparative Examples 2-4, approaching the level of Comparative Example 1. Examples 2, 3, 5, and 6 are similar, showing no obvious pilling, only some fuzzing. Example 4 exhibits only slight fuzzing, with a surface finish superior to Examples 2, 3, 5, and 6.
Claims
1. An anti-pilling polymer composite fiber, characterized in that, By weight percentage, the composite fiber component comprises 5-20% anti-pilling material and 80-95% polymer; The anti-pilling material consists of silicone resin, hydroxylated boron nitride nanosheets, and polymers.
2. The anti-pilling polymer composite fiber according to claim 1, characterized in that, The anti-pilling material is an anti-pilling resin masterbatch; the polymers include one or more of polyester, polyamide, polypropylene, and polyethylene; The polyester includes one or more of polyethylene terephthalate (PET), polypropylene terephthalate (PTT), and polybutylene terephthalate (PBT).
3. The anti-pilling polymer composite fiber according to claim 1, characterized in that, The silicone resin has a molecular weight of 600,000 to 800,000; the hydroxylated boron nitride nanosheets have a diameter of 1 to 10 µm.
4. The anti-pilling polymer composite fiber according to claim 1, characterized in that, The mass ratio of silicone resin, hydroxylated boron nitride nanosheets, and polymer in the anti-pilling material is 1~5:1~5:90~98.
5. A method for preparing the anti-pilling polymer composite fiber according to any one of claims 1-4, comprising: (1) Mix silicone resin, hydroxylated boron nitride nanosheets, polymer and dispersant to obtain a mixture, melt extrusion granulation to obtain anti-pilling polymer masterbatch; (2) Mix the anti-pilling polymer masterbatch and polymer chips, and melt spin them to obtain anti-pilling polymer composite fiber.
6. The preparation method according to claim 5, characterized in that, The dispersant in step (1) is polyethylene grafted maleic anhydride; the content of the dispersant in the mixture is 0.5~3wt%; The melt extrusion granulation temperature in step (1) is 180 ℃~280 ℃.
7. The preparation method according to claim 5, characterized in that, In step (2), the mass ratio of anti-pilling polymer masterbatch to polymer chips is 5~20:80~95.
8. The preparation method according to claim 5, characterized in that, In step (2), the anti-pilling polymer masterbatch is dried at a temperature of 80-140°C for 8-10 hours. In step (2), the polymer chips are dried at a temperature of 80-170°C for 6-8 hours. The melt spinning temperature in step (2) is 200 ℃~295 ℃.
9. A textile product, characterized in that, The textile comprises the anti-pilling polymer composite fiber as described in any one of claims 1-4.
10. The application of the anti-pilling polymer composite fiber according to any one of claims 1-4, or the textile according to claim 9, in the fields of clothing, automotive interiors, and outdoor protective equipment.