Flame-retardant antistatic polyester fiber and its preparation method
Patent Information
- Application Number
- CN202611092512.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-22
- Publication Date
- 2026-08-21
AI Technical Summary
然而,该技术本质上仍属于采用粉体助剂与聚酯切片熔融共混,各组分之间相容性差,且难以分散,助剂添加量高达20%,对纤维的物理性能影响较大,难以工业化生产
二乙基次膦酸铝(ADP)在未改性状态下,与疏水性的含磷的咪唑类离子液体(YL-404)间界面张力大,且颗粒间存在极强的范德华力、氢键及毛细作用,而表面缺乏足够的静电排斥或空间位阻,易絮沉,难以均匀分散。本发明以1-[3-(三乙氧基硅烷基)丙基]-3-甲基咪唑氯化物(Si-ImCl)对二乙基次膦酸铝(ADP)进行表面改性。Si-ImCl的-Si(OEt)3端在超声条件下水解,与ADP表面少量的Al-OH发生缩合反应,形成稳定的Si-O-Al共价键,将咪唑鎓阳离子链段牢固锚定于ADP颗粒表面。改性后,向外伸展的咪唑鎓阳离子降低了ADP的表面能,使其由亲水转为疏水/有机亲和,解决了在离子液体YL-404的润湿问题;并且,向外伸展的咪唑鎓阳离子与柔性碳链构成了“静电+空间位阻”双重防线,依靠同种电荷相互排斥,再借助外层长碳链隔开颗粒间距,削弱ADP颗粒间的范德华引力,改善了ADP在含磷咪唑类离子液体中的分散稳定性,解决了传统阻燃剂在离子液体中易絮凝、难以均匀分散的问题。
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Figure CN122610236A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of polyester fiber technology, and particularly relates to a flame-retardant and antistatic polyester fiber and its preparation method. Background Technology
[0002] Polyester fiber fabrics, as the world's largest-produced synthetic fabric, occupy an important position in fields such as industrial protective clothing, home furnishings, military equipment, and medical and health care due to their excellent elastic modulus, abrasion resistance, and mechanical strength. However, polyester fiber itself has shortcomings such as being prone to static electricity and having poor flame retardant properties, making it difficult to meet the high-quality requirements of diverse scenarios.
[0003] Extensive research has been conducted on the functional modification of polyester fibers. In terms of antistatic modification, Ma Qian et al. (Engineering Plastics Application, 2024, 52(8):46-51,80) used stearic acid-modified nano-antimony doped tin dioxide coated titanium dioxide as a light-colored conductive filler, and prepared PA6 antistatic masterbatch by melt blending, and then obtained light-colored antistatic fibers by composite spinning. However, this system relies on a high filler addition amount (volume fraction ≥50%), which can easily reduce melt fluidity and narrow the spinning process window. Moreover, the cost of nanocomposite fillers is relatively high, which is not conducive to industrial production. In terms of flame retardant modification, Ren Jiawei et al. (Journal of Textile Research, 2023, 44(2):1-10) used diethylphosphinate as the main flame retardant and macromolecular organosilicon as a synergist to prepare phosphorus-silicon flame retardant polyester fibers by melt spinning. However, 17.5% masterbatch needs to be added to meet the flame retardant requirements, and the breaking strength drops to 1.25-1.63 cN / dtex, which cannot meet the strength and toughness requirements of high-end textiles. Yangzhou Guangtai Chemical Fiber Co., Ltd. (CN202411513790.3) prepared flame retardant polymers with phosphorus-containing, tricyclic, and triazole multi-structure monomers, and compounded them with nano-boron fibers to prepare reinforced flame retardant recycled polyester fibers. However, the monomer and radiation process are costly and the equipment requirements are stringent. The nanofillers are prone to agglomeration, making industrialization difficult.
[0004] Therefore, industrial flame-retardant and antistatic modified polyester currently relies mainly on powder flame retardant blending and spinning, primarily involving two main processes: direct blending and spinning of powder additives and spinning of functional masterbatches. However, powder blending and spinning generally suffers from problems such as easy agglomeration and uneven dispersion of powder fillers, as well as low flame retardant efficiency requiring extremely high addition amounts to achieve the desired effect. Compared to powder functional additives, liquid functional additives possess superior fluidity and dispersibility, theoretically solving problems such as agglomeration and uneven dispersion. However, liquid additives are prone to volatilization and decomposition at high temperatures, and traditional liquid loading technologies have low loading capacities, making it difficult to meet flame retardant requirements. Furthermore, the melt spinning temperature of polyester is as high as 260~290℃, making liquid additives highly susceptible to volatilization, decomposition, and carbonization. This not only directly leads to the failure of flame retardant and antistatic functions but also causes problems such as yarn breakage and melt carbonization defects, severely disrupting the stability of spinning production. To address the challenges of high-temperature failure and difficulty in spinning liquid additives, the industry has developed traditional liquid-carrying technologies such as microencapsulation and porous powder adsorption. However, these technologies generally suffer from low liquid loading, with effective loading typically below 10 wt%, making it difficult to achieve satisfactory flame-retardant effects. While ionic liquids exhibit excellent thermal stability, current technologies often treat them as part of polymer chains, requiring complex polycondensation processes for preparation. Furthermore, single ionic liquids require large amounts for flame retardancy and have poor spinnability, making them suitable only for low-level functional modifications such as antistatic agents.
[0005] Patent CN121045759A discloses a method for preparing a long-lasting antistatic polymer masterbatch for core-spun polyester. The method uses dimethyl terephthalate and 1,4-butanediol as hard segments, compounded with aliphatic polyethers, polyaniline, ionic liquids, and other soft segment components, and prepares the antistatic masterbatch through transesterification and high-vacuum polycondensation. However, the polycondensation process is complex and requires extremely sophisticated equipment.
[0006] Patent CN121853202A discloses a microcapsule-doped chemical fiber and its preparation method. It uses a flame-retardant core material composed of chitosan, ammonium polyphosphate, and zirconium aminophosphate organic framework, which is then encapsulated in microcapsules and melt-spun with polyester chips. However, the microcapsule preparation process is complex, costly, and has a low loading capacity. The spinning temperature setting process window is narrow, and excessive microcapsule addition can easily lead to a decrease in the fiber's mechanical properties.
[0007] Patent CN121700575A discloses an antistatic, high flame-retardant polyester fabric for automobiles and its preparation method. It utilizes reactive flame-retardant copolymer chips blended with a multifunctional masterbatch containing graphene, carbon nanotubes, and aluminum diethylphosphinate for spinning to obtain antistatic, high flame-retardant polyester fibers. However, this technology essentially still involves melt blending powdered additives with polyester chips. The components have poor compatibility and are difficult to disperse. The additive content is as high as 20%, significantly impacting the physical properties of the fiber and making industrial production difficult.
[0008] Therefore, it is of great significance to overcome the limitations of existing technologies and develop a polyester fiber with good compatibility between components, low requirements for process equipment, antistatic properties, and excellent flame retardant and mechanical properties. Summary of the Invention
[0009] In view of the above-mentioned problems in the prior art, the present invention provides a flame-retardant and antistatic polyester fiber and its preparation method, which can produce polyester fiber that is antistatic and has excellent flame-retardant and mechanical properties.
[0010] To achieve the above objectives, the technical solution provided by the present invention is as follows: In a first aspect, this application provides a method for preparing flame-retardant and antistatic polyester fiber, comprising: A modified flame retardant was prepared by surface modification of diethyl aluminum hypophosphite with 1-[3-(triethoxysilyl)propyl]-3-methylimidazolium chloride. The modified flame retardant was then dispersed in a phosphorus-containing imidazolium ionic liquid to obtain a modified dispersion. The modified dispersion was adsorbed using polyethylene terephthalate-1,4-cyclohexanediethanol ester as an adsorption carrier, and the modified PETG was obtained after drying. Modified PETG was mixed with polyethylene terephthalate and then melt-spun to obtain the flame-retardant and antistatic polyester fiber.
[0011] Optionally, the surface modification is performed at 40~60℃.
[0012] Optionally, the condensation reaction includes: first, sonication for 20-50 min, followed by stirring for 2-2.5 h.
[0013] Optionally, the amount of 1-[3-(triethoxysilyl)propyl]-3-methylimidazolium chloride is 2% to 3% of the mass fraction of aluminum diethylphosphite.
[0014] Optionally, the solvent is a mixture of ethanol and water, wherein water accounts for 20% to 30% of the total volume of the solvent.
[0015] Optionally, the modified flame retardant accounts for 10% to 30% of the mass of the modified dispersion.
[0016] Optionally, the phosphorus-containing imidazole ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate.
[0017] Optionally, the adsorption conditions are: stirring the reaction at 55~70℃ for 30~50 min.
[0018] Optionally, the mass ratio of polyethylene terephthalate-1,4-cyclohexanediol ester to the modified dispersion is (65~75):(25~35).
[0019] Optionally, the modified flame retardant accounts for 2.5% to 10.5% of the total mass of the modified dispersion and PETG, and the phosphorus-containing imidazole ionic liquid accounts for 17.5% to 31.5% of the total mass of the modified dispersion and PETG.
[0020] Optionally, the mass fraction of modified PETG in the mixture of modified PETG and polyethylene terephthalate is 3% to 10%.
[0021] Optionally, the spinning zone temperature is 250-270℃, zone 2 temperature is 270-285℃, zone 3 temperature is 270-285℃, zone 4 temperature is 280-290℃, zone 5 temperature is 280-290℃, and the die head temperature is 280-290℃.
[0022] Secondly, this application also provides a flame-retardant and antistatic polyester fiber, which is prepared by the method described in the first aspect.
[0023] Thirdly, this application also provides a polyester fabric comprising the flame-retardant and antistatic polyester fibers described in the second aspect.
[0024] Compared with the prior art, the present invention has at least the following beneficial effects: In its unmodified state, aluminum diethylphosphonate (ADP) exhibits high interfacial tension with the hydrophobic phosphorus-containing imidazole ionic liquid (YL-404), along with strong van der Waals forces, hydrogen bonds, and capillary interactions between particles. Furthermore, the lack of sufficient electrostatic repulsion or steric hindrance on the surface makes it prone to flocculation and difficult to disperse uniformly. This invention modifies the surface of aluminum diethylphosphonate (ADP) with 1-[3-(triethoxysilyl)propyl]-3-methylimidazolium chloride (Si-ImCl). The -Si(OEt)3 end of Si-ImCl hydrolyzes under ultrasonic conditions, undergoing a condensation reaction with a small amount of Al-OH on the ADP surface to form stable Si-O-Al covalent bonds, firmly anchoring the imidazole onium cationic segments to the ADP particle surface. After modification, the outward-extending imidazolium cations reduce the surface energy of ADP, changing it from hydrophilic to hydrophobic / organophilic, thus solving the wetting problem in the ionic liquid YL-404. Furthermore, the outward-extending imidazolium cations and flexible carbon chains form a dual defense of "electrostatic + steric hindrance". Relying on the mutual repulsion of like charges and the separation of particle spacing by the long outer carbon chains, the van der Waals attraction between ADP particles is weakened, improving the dispersion stability of ADP in phosphorus-containing imidazolium ionic liquids. This solves the problem of easy flocculation and difficulty in uniform dispersion of traditional flame retardants in ionic liquids.
[0025] This invention combines phosphorus-containing imidazole ionic liquids with ADP to form a phosphorus-nitrogen synergistic system. ADP decomposes at high temperatures to generate phosphorus-containing free radicals, which capture highly reactive ·OH and ·H free radicals in the flame, interrupting the combustion chain reaction. Simultaneously, its decomposition produces non-combustible gases such as water vapor, which dilute the oxygen concentration and inhibit the combustion reaction. Pure ADP-retarded polyethylene terephthalate (PET) does not significantly improve char residue, and the char layer is brittle and loosely structured, making it difficult to form an effective physical barrier. However, at high temperatures, the nitrogen-containing free radicals and small molecular fragments generated by the cleavage of nitrogen-containing heterocycles in the phosphorus-containing imidazole ionic liquid act as dehydration and crosslinking promoters, inducing dehydration, crosslinking, and aromatization reactions in the PET molecular chains, thereby generating a denser and stronger graphitized char layer than the pure ADP system. This expanded char layer can encapsulate the high-viscosity melt, significantly increasing the strength and viscosity of the PET melt, thus fundamentally suppressing dripping; it also isolates oxygen and heat transfer, improving the flame-retardant effect.
[0026] This invention uses polyethylene terephthalate-1,4-cyclohexanediol ester (PETG) as an adsorbent carrier, leveraging its excellent toughness and microporous structure to firmly seal the modified dispersion within the carrier. During the subsequent high-temperature melt spinning process at 250-285°C, the PETG carrier acts as a physical barrier, effectively inhibiting the thermal motion of the ionic liquid. Furthermore, the excellent thermal stability of the ionic liquid successfully solves the core problem of liquid functional additives' inability to withstand high-temperature polyester spinning, enabling the stable application of high-addition liquid flame-retardant systems in polyester spinning. Simultaneously, this invention eliminates the lengthy traditional process of "functional powder → twin-screw granulation → dry spinning." Modified PETG requires no additional granulation and can be directly dry-mixed with PET chips for melt spinning. This not only saves on the investment and energy consumption of granulation equipment and avoids the loss of functional components during pre-processing, but also ensures the stability of fiber mechanical properties by utilizing the good interfacial compatibility between PETG and PET. Attached Figure Description
[0027] Figure 1 These are optical images showing the dispersion stability of the modified dispersion in Example 1 after being left for different periods of time. Figure 2 The thermal stability of the modified dispersion in Example 1; Figure 3 The images show optical images of the prepared polyester fabric during vertical burning tests, where a is Comparative Example 1 and b is Example 1. Detailed Implementation
[0028] The present invention will now be described in further detail with reference to the accompanying drawings: Unless otherwise specified, the experimental methods used in the embodiments of this invention are all conventional methods.
[0029] All reagents and materials used in this example can be purchased routinely. The quantitative experiments involved in the examples were all repeated at least three times, and the results were averaged.
[0030] Raw material source: The phosphorus-containing imidazole ionic liquid YL-404: 1-butyl-3-methylimidazolium hexafluorophosphate, was purchased from Hunan Yuanli New Materials Co., Ltd. PETG: Purchased from Sinopec Yizheng Chemical Fiber Co., Ltd., grade FG703; PET: Sanfangxiang Group Co., Ltd., brand name PET CZ-318.
[0031] Example 1
[0032] A flame-retardant and antistatic polyester fiber, the preparation method of which is as follows: S1: Weigh Si-ImCl and ADP, add them to a solvent, the amount of Si-ImCl is 2% of the mass fraction of ADP, the solvent is a mixture of water and ethanol (volume ratio of 3:7), at 40℃, first sonicate for 30 min, then stir at 40℃ for 2 h to carry out the condensation reaction, after the reaction is completed, dry it at 80℃ to obtain the modified flame retardant; gradually add the modified flame retardant to the phosphorus-containing imidazole ionic liquid YL-404, stir at 600 r / min for 30 min to obtain the modified dispersion, wherein the mass ratio of the modified flame retardant to YL-404 is 3:7.
[0033] S2: Add the modified dispersion to PETG, wherein the mass ratio of the modified dispersion to PETG is 35:65 (the modified flame retardant accounts for 10.5% of the total mass of the modified dispersion and PETG, and YL-404 accounts for 24.5% of the total mass of the modified dispersion and PETG). Place it in an oil bath and stir at 60℃ for 30 min. After stirring, place the mixture in a 60℃ forced-air oven and dry for 9 h to obtain modified PETG.
[0034] S3: Dry PET in a vacuum oven at 140℃ for 8 hours. After the material is fully dried, mix it with modified PETG at a mass ratio of 90:10 in a sealed container. Then, feed the blended material into a melt spinning machine. Set the spinning zone temperatures to 250℃, 280℃, 281℃, 282℃, and 282℃ respectively, with the die head temperature at 282℃. Spin at a speed of 2800 m / min (the modified flame retardant content in the fiber is 1.05%, and the content of phosphorus-containing imidazole ionic liquid YL-404 is 2.45%) to obtain flame-retardant and antistatic polyester fiber. The spun flame-retardant and antistatic polyester fibers were stretched at a draw ratio of 2.5, and the twist was controlled at 20 to complete the spinning process. Finally, the subsequent weaving process was carried out, with the warp density controlled at 22 threads / cm and the weft density at 16 threads / cm, to obtain a polyester fabric with flame-retardant and antistatic functions.
[0035] Figure 1 Optical images showing the dispersion stability of the modified dispersion after different standing times. In this invention, the modified dispersion was uniformly milky white after standing for 7 days and 28 days without obvious stratification or precipitation, indicating that this method can produce a stable and long-lasting flame-retardant dispersion suitable for use in spinning processes.
[0036] Figure 2 To assess the thermal stability of the modified dispersion, the conventional spinning temperature for PET is 260-290℃. This sample did not exhibit significant weight loss until 320℃, forming a thermally stable safe range exceeding 30℃. Figure 2 As can be seen, the overall melt temperature of the modified dispersion prepared in this embodiment is consistently below 290℃ during steady-state extrusion, avoiding the temperature range of PET decomposition. Furthermore, its main DTG decomposition peak is located between 380-420℃, a significant gap from the spinning temperature range, indicating that the flame-retardant component does not undergo large-scale thermal decomposition during processing. The thermal stability of the modified dispersion is far higher than that of PET spinning temperature, and it will not thermally decompose during spinning, making it suitable for PET melt spinning.
[0037] Figure 3 The optical images of the vertical burning test of the above-mentioned polyester fabric show that after ignition, the polyester fabric of Example 1 quickly forms a dense and continuous char layer, which isolates oxygen and heat transfer, inhibits the longitudinal extension of molten droplets and flame, and the damaged length is only 11.9 cm. The polyester fabric obtained in Comparative Example 1 lacks an effective char barrier layer, the flame continues to spread, and the damaged length is as high as 22 cm. The polyester fiber obtained by the method of the present invention has a flame-retardant effect.
[0038] Example 2
[0039] A flame-retardant and antistatic polyester fiber, the preparation method of which is as follows: S1: Weigh Si-ImCl and ADP, add them to a solvent, the amount of Si-ImCl is 2% of the mass fraction of ADP, the solvent is a mixture of water and ethanol (volume ratio of 3:7), at 40℃, first sonicate for 30 min, then stir at 40℃ for 2 h to carry out the condensation reaction, after the reaction is completed, dry it at 80℃ to obtain the modified flame retardant; gradually add the modified flame retardant to the phosphorus-containing imidazole ionic liquid YL-404, stir at 600 r / min for 30 min to obtain the modified dispersion, wherein the mass ratio of the modified flame retardant to YL-404 is 3:7.
[0040] S2: Add the modified dispersion to PETG, wherein the mass ratio of the modified dispersion to PETG is 35:65 (the modified flame retardant accounts for 10.5% of the total mass of the modified dispersion and PETG, and YL-404 accounts for 24.5% of the total mass of the modified dispersion and PETG). Place it in an oil bath and stir at 60℃ for 30 min. After stirring, place the mixture in a 60℃ forced-air oven and dry for 9 h to obtain modified PETG.
[0041] S3: Dry PET in a vacuum oven at 140 ℃ for 8 h. After the material is fully dried, mix it with modified PETG at a mass ratio of 90:10. Place the mixture in a sealed container and shake it thoroughly to ensure uniform mixing. Then, feed the blend into a melt spinning machine. Set the spinning zone temperatures to 250 ℃, 280 ℃, 281 ℃, 282 ℃, and 282 ℃, and the die head temperature to 282 ℃. Spin at a speed of 2800 m / min (to achieve a modified flame retardant content of 0.525% and a YL-404 content of 1.225%) to obtain flame-retardant and antistatic polyester fiber. Flame-retardant and antistatic polyester fibers were stretched at a ratio of 2.5, and the twist was controlled at 20 to complete the spinning process. Finally, subsequent weaving was carried out, with the warp density controlled at 22 threads / cm and the weft density at 16 threads / cm, to obtain a polyester fabric with flame-retardant and antistatic functions.
[0042] Example 3
[0043] The difference between this embodiment and Embodiment 1 is that PET and modified PETG are mixed at a mass ratio of 97:3 and then spun.
[0044] Comparative Example 1 The difference between this comparative example and Example 1 is that no modified PETG was added, and the PET was directly dried and then spun.
[0045] The steps are as follows: PET is dried in a 140℃ vacuum oven for 8 hours. After the material is fully dried, it is fed into a melt spinning machine. The spinning zone temperatures are set to 284℃ for zone 1, 285℃ for zone 2, 285℃ for zone 3, 285℃ for zone 4, 285℃ for zone 5, and 285℃ for the die head. Spinning is performed at a speed of 2800 m / min (resulting in a modified flame retardant content of 0.525% and a YL-404 content of 1.225%) to obtain flame-retardant and antistatic polyester fiber. The flame-retardant and antistatic polyester fiber is stretched using a 2.5 times draw ratio, and the twist is controlled at 20 to complete the spinning preparation. Finally, subsequent weaving processing is carried out, controlling the warp density at 22 threads / cm and the weft density at 16 threads / cm to obtain a polyester fabric with flame-retardant and antistatic functions.
[0046] Result: The PET showed no flame retardant or antistatic properties.
[0047] Comparative Example 2 The difference between this comparative example and Example 1 is that Si-ImCl was not added in S1.
[0048] The steps are as follows: S1: ADP was gradually added to imidazole ionic liquid YL-404 and stirred at 600 r / min for 30 min to obtain a dispersion, wherein the mass ratio of ADP to YL-404 was 3:7.
[0049] S2: Add the dispersion to PETG, wherein the mass ratio of dispersion to PETG is 35:65 (ADP accounts for 10.5% of the total mass of dispersion and PETG, and YL-404 accounts for 24.5% of the total mass of dispersion and PETG). Place it in an oil bath and stir at 60℃ for 30 min. After stirring, place the mixture in a 60℃ forced-air oven and dry for 9 h to obtain modified PETG.
[0050] S3: PET was dried in a vacuum oven at 140℃ for 8 hours. After the material was fully dried, it was mixed with modified PETG at a mass ratio of 90:10. The mixture was then thoroughly shaken in a sealed container to ensure homogeneity. The blend was then fed into a melt spinning machine. The spinning temperatures were set as follows: Zone 1: 250℃; Zone 2: 280℃; Zone 3: 281℃; Zone 4: 282℃; Zone 5: 282℃; and the die head temperature: 282℃. Spinning was performed at a speed of 2800 m / min (resulting in an ADP content of 0.525% and a YL-404 content of 1.225%), yielding flame-retardant and antistatic polyester fiber. The flame-retardant and antistatic polyester fiber was stretched using a 2.5 times draw ratio, and the twist was controlled at 20 to complete the spinning process. Finally, subsequent weaving was carried out, controlling the warp density at 22 threads / cm and the weft density at 16 threads / cm to obtain a polyester fabric with flame-retardant and antistatic properties.
[0051] Dispersion results: ADP could not be stably dispersed in YL-404 for a long period of time, and obvious stratification occurred after 1 day. Furthermore, the uneven dispersion severely affected the strength. The vertical burning damage length was 13.8 cm, and the limiting oxygen index was 28.5%, but molten droplets were generated and ignited the absorbent cotton. The antistatic rating reached Class A.
[0052] Comparative Example 3 The difference between this comparative example and Example 1 is that the phosphorus-containing imidazole ionic liquid YL-404 (1-butyl-3-methylimidazolium hexafluorophosphate) in step 1 is replaced with the same mass of tributylmethylammonium bis(trifluoromethanesulfonyl)imide salt (BIL-02), while the other steps are the same.
[0053] Results: The fabric obtained in this comparative example had poor flame retardant effect (damage length exceeded 15cm, limiting oxygen index was 26.2%, not reaching 28%, and melt droplets were generated to ignite the degreased cotton), and its strength performance could not meet the strength requirements of conventional clothing fibers.
[0054] Comparative Example 4 The difference between this comparative example and Example 1 is that ADP and Si-ImCl were not added, and YL-404 was directly added to PETG.
[0055] S1: Add YL-404 to PETG at a mass ratio of 40:60, place it in an oil bath and stir at 60℃ for 30 min; after stirring, place the mixture in a 60℃ forced-air oven and dry for 9 h to obtain modified PETG.
[0056] S2: Dry PET in a vacuum oven at 140 ℃ for 8 h. After the material is fully dried, mix it with modified PETG at a mass ratio of 90:10. Place the mixture in a sealed container and shake it thoroughly to ensure uniform mixing. Then, feed the blend into a melt spinning machine. Set the spinning zone temperatures to 250 ℃, 280 ℃, 281 ℃, 282 ℃, and 282 ℃, and the die head temperature to 282 ℃. Spin at a speed of 2800 m / min (to achieve a modified flame retardant content of 0.525% and a YL-404 content of 1.225%) to obtain flame-retardant and antistatic polyester fiber. Flame-retardant and antistatic polyester fibers were stretched at a ratio of 2.5, and the twist was controlled at 20 to complete the spinning preparation. Finally, subsequent weaving was carried out, with the warp density controlled at 22 threads / cm and the weft density at 16 threads / cm, to obtain a polyester fabric with flame-retardant and antistatic functions.
[0057] Results: The polyester fibers obtained by this system only have antistatic properties and no good flame retardant effect (damage length exceeds 15cm, melt droplets are generated and ignite degreased cotton). The strength is very poor and does not meet the strength standard for clothing fibers.
[0058] The electrostatic voltage (kV) and half-life (s) of the flame-retardant and antistatic polyester fabric were tested according to GB / T12703-2008 "Textiles - Electrostatic Properties Test - Part 1: Static Voltage Half-Life". The flammability of the fabric was tested according to GB / T5455-2014 "Textiles - Determination of Vertical Destruction Length, Afterflame and Reignition Time". The limiting oxygen index of the fabric was tested according to GB / T5454-2008 "Textiles - Flammability Test - Oxygen Index Method". The mechanical properties of the polyester fiber were tested according to GB / T 14337-2022 "Test Method for Tensile Properties of Short Chemical Fibers". The test results are shown in Table 1.
[0059] Table 1. Performance test results of polyester fabrics
[0060] As shown in Table 1, the polyester fibers prepared by this invention all exhibit excellent antistatic properties. Furthermore, compared to Comparative Examples 1, 2, and 3, the flame-retardant properties of the polyester fabrics prepared in this application are significantly improved, with an oxygen index reaching 30.0% and a vertical burning damage length of 11.9 cm. They also possess excellent mechanical properties, with a breaking strength reaching 3.38 cN / dtex, still above 3.1-3.38 cN / dtex, which can meet the requirements for daily and general industrial applications.
Claims
1. A method for preparing flame-retardant and antistatic polyester fiber, characterized in that, include: The surface of aluminum diethylphosphite was modified with 1-[3-(triethoxysilyl)propyl]-3-methylimidazolium chloride, and the modified flame retardant was obtained after drying. Then, the modified flame retardant was dispersed in a phosphorus-containing imidazolium ionic liquid to obtain a modified dispersion. The modified dispersion was adsorbed using polyethylene terephthalate-1,4-cyclohexanediethanol ester as an adsorption carrier, and the modified PETG was obtained after drying. Modified PETG was mixed with polyethylene terephthalate and then melt-spun to obtain the flame-retardant and antistatic polyester fiber.
2. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The surface modification is carried out at 40~60℃.
3. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The amount of 1-[3-(triethoxysilyl)propyl]-3-methylimidazolium chloride used is 2% to 3% of the mass fraction of diethyl aluminum hypophosphite.
4. The method for preparing flame-retardant and antistatic polyester fiber according to claim 3, characterized in that, The surface modification is carried out in a solvent, which is a mixture of ethanol and water, wherein water accounts for 20% to 30% of the total volume of the solvent.
5. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The modified flame retardant accounts for 10% to 30% of the mass of the modified dispersion.
6. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The adsorption conditions are: stirring at 55~70℃ for 30~50 min.
7. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The mass ratio of polyethylene terephthalate-1,4-cyclohexanediethanol ester to the modified dispersion is (65~75):(25~35).
8. The method for preparing flame-retardant and antistatic polyester fiber according to claim 1, characterized in that, The mass fraction of modified PETG in the mixture of modified PETG and polyethylene terephthalate is 3% to 10%.
9. A flame-retardant and antistatic polyester fiber, characterized in that, It is prepared by the method described in any one of claims 1-8.
10. A polyester fabric, characterized in that, Includes the flame-retardant and antistatic polyester fiber as described in claim 9.
Citation Information
Patent Citations
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CN119243365B
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CN121045759A
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