Antibacterial high-elasticity composite yarn and preparation method thereof
By preparing polyester chips and blending them with cotton fibers, functional monomers are introduced to improve the antibacterial properties and elasticity of the composite yarn. This solves the problems of poor antibacterial properties and insufficient elasticity of the composite yarn during long-term use, achieving long-lasting antibacterial properties and excellent elastic repair.
Patent Information
- Application Number
- CN202511889291.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-15
- Publication Date
- 2026-01-20
AI Technical Summary
Existing composite yarns have poor antibacterial properties and insufficient elasticity during long-term use, making it difficult to meet the complex needs of sportswear and medical protective equipment.
Polyester chips were prepared using terephthalic acid, functional monomers, and ethylene glycol as the main raw materials and then blended with cotton fibers. By introducing functional monomers, including long-chain ether bonds and dynamic reversible structures, into the polyester fibers, the antibacterial and elastic repair capabilities of the yarn were improved.
It achieves durable antibacterial properties and excellent elasticity repair capabilities in composite yarns, solving the problems of bacterial growth and loss of elasticity during long-term use.
Smart Images

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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of fabric fibers, in particular to an antibacterial high-elasticity composite yarn and a preparation method thereof. BACKGROUND
[0002] In the process of the textile industry moving towards the deep integration of intelligence and functionality, the dual demands of consumers for health protection and wearing comfort are driving the yarn technology to break through in the direction of compounding. Traditional single-function yarns have been difficult to meet the needs of complex scenarios, especially in the fields of sports clothing, medical protection and special workwear, composite yarns with antibacterial protection and dynamic elasticity have become the focus of industry research and development. Behind this technical evolution is the superimposed driving of three trends: the increasing risk of microbial pollution, the functional segmentation of sports scenarios, and the intelligentization of wearable devices.
[0003] The problem of microbial pollution is becoming the core pain point of textile health hazards. Research shows that ordinary textiles can breed 1200 times more bacteria on the surface after 72 hours of continuous use, and pathogenic bacteria such as Staphylococcus aureus and Escherichia coli account for more than 65%. In the medical field, if medical clothes, surgical dressings and other fabrics lack long-term antibacterial mechanisms, they are likely to become a medium for cross-infection; in the sports field, the humid environment formed by sweat and fabric friction can accelerate bacterial reproduction, leading to odor and skin inflammation. Therefore, many researchers have developed antibacterial fibers, for example, patent number CN113106589B discloses "an antibacterial and moth-resistant heating composite yarn and a preparation method thereof", which comprises the following steps: S1. Defatted wool fibers are dissolved and centrifuged, then nano-silver and nano-titanium dioxide are added, stirred uniformly to obtain a spinning solution; the generated fibers are attached to the surface of the fine wool yarn to form a primary yarn; S2. The primary yarn obtained in step S1 is fed into a vortex spinning device and mixed with cotton fibers to form the antibacterial and moth-resistant heating composite yarn. The composite yarn not only has the characteristics of traditional wool yarns such as good moisture absorption, excellent elasticity and good warmth retention, but also has the advantages of antibacterial and moth-resistant, self-heating under far infrared radiation. However, the compatibility of inorganic antibacterial agents with fibers is relatively poor, which may affect the long-term antibacterial performance.
[0004] Therefore, it is urgent to develop a composite yarn with good antibacterial performance, stable long-term use and good elasticity. SUMMARY
[0005] The purpose of the present application is to provide an antibacterial high-elasticity composite yarn and a preparation method thereof, to solve the problems of poor long-term antibacterial performance and poor elasticity of the current composite yarn.
[0006] To achieve the above-mentioned purpose, the present application adopts the following technical solutions: The application provides an antibacterial high-elasticity composite yarn, and comprises the following steps: (1) terephthalic acid, a functional monomer and ethylene glycol are configured into slurry with an auxiliary agent and a catalyst under nitrogen protection, and are added into an esterification reactor, pressure control is 0.1-0.2 MPa, temperature control is 220-250 DEG C, and stirring is carried out for 2-3 hours, then the catalyst is added, temperature is raised to 250-290 DEG C, pressure is reduced to 60-80 Pa, and reaction is carried out for 2-4 hours, and polyester chips are obtained through underwater granulation after the reaction is completed; (2) the polyester chips obtained in the step (1) are blended with an antioxidant and a dispersant, and are melt-extruded to prepare polyester fibers, and then the polyester fibers are blended with cotton fibers to obtain the antibacterial high-elasticity composite yarn.
[0007] The polyester fibers are widely used in daily necessities, for example, the polyester fibers are preferred materials for clothes, bed sheets and curtains, however, bacteria are bred in these articles, especially in close-fitting clothes, for a long time, which influences the health of users, and clothes subjected to long-term machine washing are more or less deformed and wrinkled, which is caused by the problem of poor elasticity in long-term use.
[0008] The application uses terephthalic acid, a functional monomer and ethylene glycol as main raw materials to prepare polyester chips, and then the polyester chips are blended with cotton fibers to obtain a composite yarn, which can not only solve the problem of bacterial breeding, but also improve the elasticity and elasticity repairability of the yarn.
[0009] In some embodiments, the antioxidant is one or more of antioxidant 1010, antioxidant 1076, antioxidant 1098 and antioxidant 168.
[0010] In some embodiments, the dispersant is polyoxyethylene and / or cationic polyacrylamide.
[0011] In some embodiments, the mass ratio of the polyester fibers to the cotton fibers is 1:(0.5-1).
[0012] In some embodiments, the molar ratio of the terephthalic acid, the functional monomer and the ethylene glycol is 1:(0.2-0.4):(1.1-1.4).
[0013] In some embodiments, the auxiliary agent is trimethyl phosphate.
[0014] In some embodiments, the catalyst is one or more of ethylene glycol antimony, antimony oxide and antimony acetate.
[0015] In some embodiments, the structure of the functional monomer is shown in formula I: (I); Wherein, X is Br, Cl or I; n is an integer from 0 to 5.
[0016] The application can prevent the weakening of the intermolecular force between the molecular chains due to the excessively long chain segment, and the decrease of the hard segment purity, thereby reducing the tensile strength of the polyester fiber by regulating the n value in the functional monomer structure.
[0017] In some embodiments, the method for preparing the functional monomer comprises the following steps: S1, under the atmosphere of inert protective gas, polyether polyol and maleimide are mixed and added into tetrahydrofuran, and the temperature is lowered to-10-0℃, then tetraphenylphosphonium palladium and diethyl azodicarboxylate are added thereto under constant temperature, and then the temperature is restored to room temperature and stirred for 24-26h, after which column chromatography purification is performed to obtain the compound shown as formula II (II); S2, 5-bromo-2-furoic acid and the compound shown as formula II in step S1 are mixed, then calcium chloride and deionized water are added and the temperature is raised to 50-60℃, and constant temperature stirring is performed for 6-8h, after which the compound shown as formula III is obtained (III); S3, allyl trimethyl ammonium halide, the compound shown as formula III in step S2, palladium acetate and tris(o-methylphenyl)phosphine are mixed and added into toluene, DIPEA is added, the temperature is raised to 70-80℃, constant temperature stirring is performed for 3-4h, after which neutralization is performed with 4-6wt% hydrochloric acid, the organic phase is dried under reduced pressure, and column chromatography is performed to obtain the compound shown as formula I, i.e. the functional monomer.
[0018] The application can not only improve the antibacterial ability of the final composite yarn, but also improve the elasticity and elastic recovery ability of the composite yarn by introducing the self-prepared functional monomer into the molecular structure of the polyester fiber, and the reasons may be as follows: on the one hand, the functional monomer structure contains long-chain ether bonds, the introduction of the long-chain ether bonds increases the flexibility of the molecular chain, so that the molecular chain is more likely to change in conformation when stretched by external force, thereby increasing the entropy value of the system, and after the external force is removed, the molecular chain tends to return to the state with a larger entropy value, i.e. to the original shape, so it exhibits good elastic recovery performance, and gives the polyester fiber a certain elasticity; on the other hand, the functional monomer is obtained by Diels-Alder reaction of the compound shown as formula II with 5-bromo-2-furoic acid, and the polyester fiber can absorb energy by bond rupture and recombination when the yarn is stressed, thereby avoiding material rupture caused by stress concentration, and this dynamic reversible structure not only maintains the strength of the covalent bond, but also gives the yarn excellent elasticity through dynamic reversibility; on the third hand, the functional monomer structure contains a large amount of quaternary ammonium salt structure, which improves the antibacterial ability of the yarn.
[0019] In some embodiments, in step S1, the molar ratio of the polyether polyol and the maleimide is 1: (2.1-2.5).
[0020] Preferably, in step S1, the molar ratio of the polyether polyol and the maleimide is 1:2.3.
[0021] In some embodiments, in step S1, the molar ratio of the tetrakis(triphenylphosphine)palladium and the polyether polyol is (1.9-2.2):1.
[0022] In some embodiments, in step S2, the molar ratio of the 5-bromo-2-furoic acid and the compound of formula II is 1: (2.2-2.4).
[0023] Preferably, in step S2, the molar ratio of the 5-bromo-2-furoic acid and the compound of formula II is 1:2.3.
[0024] In some embodiments, in step S3, the molar ratio of the allyltrimethylammonium bromide and the compound of formula III is (2.1-2.4):1.
[0025] Preferably, in step S3, the molar ratio of the allyltrimethylammonium bromide and the compound of formula III is 2.2:1.
[0026] In some embodiments, in step S3, the molar ratio of the palladium acetate and the compound of formula III is (0.03-0.06):1.
[0027] In some embodiments, in step S3, the molar ratio of the tris(o-methylphenyl)phosphine and the compound of formula III is (0.09-0.12):1.
[0028] In some embodiments, in step S3, the molar ratio of the DIPEA and the compound of formula III is (1.9-2.3):1.
[0029] Another aspect of the present application provides an antibacterial high-elasticity composite yarn prepared by any of the above preparation methods.
[0030] Compared with the prior art, the present application has the following beneficial effects: (1) The present application uses terephthalic acid, a functional monomer and ethylene glycol as main raw materials to prepare polyester chips, and then the polyester chips are made into fibers and blended with cotton fibers to obtain a composite yarn. The composite yarn can not only solve the problem of bacterial breeding, but also improve the elasticity and elastic recovery of the yarn.
[0031] (2) The functional monomer structure of the application contains long chain ether bond, which gives the polyester fiber certain elasticity, in addition, the structure of the functional monomer contains dynamic reversible structure, which gives the yarn excellent elasticity and elastic recovery ability, and the structure of the functional monomer contains a large number of quaternary ammonium salt structures, which improves the antibacterial ability of the yarn. DETAILED DESCRIPTION
[0032] The technical solutions of the application will be described clearly and completely in combination with the specific embodiments below, but those skilled in the art will understand that the following described embodiments are part of the embodiments of the application, not all the embodiments, and are only used to illustrate the application, and should not be regarded as limiting the scope of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the application. If the specific conditions are not specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer are used. If the reagents or instruments used are not specified by the manufacturer, they are all conventional products that can be purchased on the market.
[0033] Unless otherwise specified, the post-treatment operations such as "stirring", "mixing", "warming", "reduced pressure drying", "column chromatography", "granulation", "melt extrusion", "blending" and the like described below can be selected by those skilled in the art according to the actual situation, and are not further limited.
[0034] In the following examples and comparative examples, polyethylene oxide is purchased from Shandong Hongquan Chemical Technology Co., Ltd.; commercially available polyester chips are purchased from Suzhou Xirunqian International Trade Co., Ltd.
[0035] Preparation Example 1 The preparation method of the functional monomer comprises the following steps: S1, under N2 atmosphere, 0.1 mol of tetraethylene glycol, 0.2 mol of maleimide is mixed into 400 ml of tetrahydrofuran, cooled to-5℃, and 0.2 mol of tetrakis triphenylphosphine palladium and 0.1 mol of azobisdimethylate are added thereto under constant temperature, then restored to room temperature and stirred for 25 h, after the end, column chromatography purification (dichloromethane / petroleum ether system) is carried out to obtain the compound shown in formula II (II); After detection, 1H NMR (400 MHz, DMSO-d6) as follows: δ 3.49 (4H, t, J = 7.28 Hz), 3.58-3.71 (8H, 3.64 (t, J = 4.21 Hz), 3.65 (t, J = 4.21 Hz)), 3.96 (4H, t, J = 7.28 Hz), 7.45 (4H, d, J = 10.18 Hz); S2, 0.05 mol of 5-bromo-2-furoic acid and 0.13 mol of the compound represented by formula II in step S1 were mixed, then 0.2 mol of calcium chloride and 500 ml of deionized water were added, and the mixture was stirred at 55°C for 7 h. After the reaction was completed, the compound represented by formula III was obtained (III); After detection, 1 H NMR (400 MHz, Chloroform-d) as follows: δ 3.41-3.54 (4H, 3.47 (dd, J = 6.29, 6.29 Hz), 3.47 (dd, J = 6.29, 6.29 Hz)), 3.59-3.71 (8H, 3.65 (dd, J = 4.18, 4.18 Hz), 3.65 (dd, J = 4.18, 4.18 Hz), 3.65 (dd, J = 4.18, 4.18 Hz), 3.65 (dd, J = 4.18, 4.18 Hz)), 3.73-3.96 (4H, 3.79 (d, J = 8.06 Hz), 3.90 (d, J = 8.06 Hz)), 4.05-4.18 (4H, 4.11 (dd, J = 6.29, 6.29 Hz), 4.11 (dd, J = 6.29, 6.29 Hz)), 6.32 (2H, d, J = 7.73 Hz), 6.85 (2H, d, J = 7.73 Hz); S3, 0.31 mmol of allyl trimethylammonium bromide, 0.15 mmol of the compound represented by formula III in step S2, 0.0078 mmol of palladium acetate and 0.015 mmol of tris (o-methylphenyl) phosphorus were mixed and added to toluene, 0.31 mmol of DIPEA was added, and the mixture was stirred at 75°C for 3 h. After the reaction was completed, the pH was neutralized to 7 with 5 wt% hydrochloric acid, the organic phase was dried under reduced pressure, and the compound represented by formula I, i.e. the functional monomer, was obtained by C18 reverse column chromatography (acetonitrile / deionized water system) (I).
[0036] Upon testing, 1 H NMR (400 MHz, Deuterium Oxide) as follows: δ 2.84 (18H, s), 3.41-3.54 (4H, 3.47 (dd, J = 6.28, 6.28 Hz), 3.47 (dd, J = 6.28, 6.28 Hz)), 3.59-3.82 (16H, 3.65 (dd, J = 4.16, 4.16 Hz), 3.65 (dd, J = 4.16, 4.16 Hz), 3.65(dd, J = 4.16, 4.16 Hz), 3.65 (dd, J = 4.16, 4.16 Hz), 3.71 (d, J = 8.06 Hz),3.72 (d, J = 8.06 Hz), 3.76 (d, J = 7.37 Hz), 3.76 (d, J = 7.37 Hz)), 4.05-4.18 (4H, 4.11 (dd, J = 6.28, 6.28 Hz), 4.11 (dd, J = 6.28, 6.28 Hz)), 5.59(2H, d, J = 15.50 Hz), 6.08-6.30 (6H, 6.17 (ddd, J = 15.50, 7.37, 7.37 Hz),6.23 (d, J = 7.50 Hz), 6.24 (d, J = 7.50 Hz))。
[0037] Preparation Example 2 The method for preparing the functional monomer is the same as that in Preparation Example 1, except that equimolar 1,14-tetradecanediol is used instead of trioxa tetraethylene glycol.
[0038] Preparation Example 3 The method for preparing the functional monomer is the same as that in Preparation Example 1, except that equimolar 1,14-tetradecanediol is used instead of trioxa tetraethylene glycol.
[0039] Preparation Example 4 The method for preparing the functional monomer comprises the following steps: Under N2 atmosphere, 0.1 mol of trioxa tetraethylene glycol is mixed with 0.2 mol of phthalic anhydride and added to 400 ml of dichloromethane, cooled to 3°C, then 0.4 mol of triethylamine is added, stirred for 9 h, filtered, extracted (dichloromethane / deionized water), the organic phase is combined and concentrated under reduced pressure, dried to obtain the functional monomer.
[0040] Preparation Example 5 A method for preparing a functional monomer, comprising the following steps: S1, under N2 atmosphere, 0.1 mol of tetraethylene glycol, 0.2 mol of maleimide is mixed into 400 ml of tetrahydrofuran, cooled to-5℃, and then 0.2 mol of tetrakis triphenylphosphine palladium and 0.1 mol of diethyl azodicarboxylate are added thereto, followed by stirring at room temperature for 25 h, and then column chromatography purification (dichloromethane / petroleum ether system) to obtain a compound represented by formula II (II); S2, 0.05 mol of furan acid and 0.13 mol of the compound represented by formula II in step S1 are mixed, and then 0.2 mol of calcium chloride and 500 ml of deionized water are added, and then stirred at 55℃ for 7 h to obtain a compound represented by formula III, i.e. a functional monomer (III).
[0041] After detection, 1 H NMR (400 MHz, Chloroform-d) as follows: δ 3.41-3.54 (4H, 3.47 (dd,J = 6.27, 6.27 Hz), 3.47 (dd, J = 6.27, 6.27 Hz)), 3.59-3.76 (12H, 3.65 (dd,J = 4.20, 4.20 Hz), 3.65 (dd, J = 4.20, 4.20 Hz), 3.65 (dd, J = 4.20, 4.20Hz), 3.65 (dd, J = 4.20, 4.20 Hz), 3.68 (d, J = 8.06 Hz), 3.69 (dd, J = 8.06,5.30 Hz)), 4.03-4.16 (4H, 4.10 (dd, J = 6.27, 6.27 Hz), 4.10 (dd, J = 6.27,6.27 Hz)), 4.70 (2H, dd, J = 5.30, 2.50 Hz), 6.08-6.25 (4H, 6.14 (d, J = 7.57Hz), 6.18 (dd, J = 7.57, 2.50 Hz))).
[0042] Example 1 A method for preparing an antibacterial high-elasticity composite yarn, comprising the following steps: (1) Under the protection of nitrogen, 0.1 mol of terephthalic acid, 0.03 mol of functional monomer and 0.13 mol of ethylene glycol are configured into a slurry with 0.3 g of trimethyl phosphate and 0.03 g of ethylene glycol antimony, and are added into an esterification reactor, the pressure is controlled at 0.15 MPa, the temperature is controlled at 230°C, and stirring is performed for 2.5 h, then 0.03 g of ethylene glycol antimony is added, the temperature is raised to 280°C, the pressure is reduced to 70 Pa, and reaction is performed for 3 h, after which underwater granulation is performed to obtain polyester chips; (2) The polyester chips obtained in step (1) are blended with 2.7 g of antioxidant 1010 and 4 g of polyethylene oxide, and are melt-extruded (at 220°C) to obtain polyester fibers, then the polyester fibers obtained are blended with cotton fibers at a mass ratio of 1:0.8 to obtain antibacterial high-elasticity composite yarns.
[0043] The functional monomer is prepared according to Preparation Example 1.
[0044] Example 2 A method for preparing antibacterial high-elasticity composite yarns, comprising the following steps: (1) Under the protection of nitrogen, 0.1 mol of terephthalic acid, 0.02 mol of functional monomer and 0.11 mol of ethylene glycol are configured into a slurry with 0.3 g of trimethyl phosphate and 0.03 g of ethylene glycol antimony, and are added into an esterification reactor, the pressure is controlled at 0.1 MPa, the temperature is controlled at 220°C, and stirring is performed for 3 h, then 0.03 g of ethylene glycol antimony is added, the temperature is raised to 250°C, the pressure is reduced to 80 Pa, and reaction is performed for 4 h, after which underwater granulation is performed to obtain polyester chips; (2) The polyester chips obtained in step (1) are blended with 2.7 g of antioxidant 1010 and 4 g of polyethylene oxide, and are melt-extruded (at 220°C) to obtain polyester fibers, then the polyester fibers obtained are blended with cotton fibers at a mass ratio of 1:0.5 to obtain antibacterial high-elasticity composite yarns.
[0045] Example 3 A method for preparing antibacterial high-elasticity composite yarns, comprising the following steps: (1) Under the protection of nitrogen, 0.1 mol of terephthalic acid, 0.04 mol of functional monomer and 0.14 mol of ethylene glycol are configured into a slurry with 0.3 g of trimethyl phosphate and 0.03 g of ethylene glycol antimony, and are added into an esterification reactor, the pressure is controlled at 0.2 MPa, the temperature is controlled at 250°C, and stirring is performed for 2 h, then 0.03 g of ethylene glycol antimony is added, the temperature is raised to 290°C, the pressure is reduced to 60 Pa, and reaction is performed for 2 h, after which underwater granulation is performed to obtain polyester chips; (2) The polyester chips obtained in step (1) are blended with 2.7 g of antioxidant 1010 and 4 g of polyethylene oxide, and are melt-extruded (at 220°C) to obtain polyester fibers, then the polyester fibers obtained are blended with cotton fibers at a mass ratio of 1:1 to obtain antibacterial high-elasticity composite yarns.
[0046] The functional monomer is prepared according to Preparation Example 1.
[0047] Example 4 A method for preparing an antibacterial high-elasticity composite yarn, the specific implementation manner being the same as that of Example 1, except that the functional monomer is prepared according to Preparation Example 2.
[0048] Example 5 A method for preparing an antibacterial high-elasticity composite yarn, the specific implementation manner being the same as that of Example 1, except that the functional monomer is prepared according to Preparation Example 3.
[0049] Example 6 A method for preparing an antibacterial high-elasticity composite yarn, the specific implementation manner being the same as that of Example 1, except that the functional monomer is prepared according to Preparation Example 4.
[0050] Example 7 A method for preparing an antibacterial high-elasticity composite yarn, the specific implementation manner being the same as that of Example 1, except that the functional monomer is prepared according to Preparation Example 5.
[0051] Comparative Example 1 A method for preparing an antibacterial high-elasticity composite yarn, the specific implementation manner being the same as that of Example 1, except that commercially available polyester chips are used instead of the polyester chips in step (2).
[0052] Performance test; (1) Antibacterial test: the sample is prepared according to the relevant provisions of the first part agar plate diffusion method and the third part oscillation method in GB / T20944-2007 “Evaluation of antibacterial properties of textiles”, and Escherichia coli and Staphylococcus aureus are used for testing, and the antibacterial test is performed after washing for 50 times; (2) Elasticity test: the test is performed according to the test method of ASTM D3107-2007 (2015), the test equipment is Zwick / Roell ZO.5 tensile machine, the temperature is 25℃, the humidity is 62%, the sample length is 25cm, and the sample width is 7cm; (3) Elasticity repair test: the repeated stretching is performed until the radial elasticity recovery rate is less than 60%, the sample is soaked in hot water at 60℃ for 3h, and after being dried, the radial elasticity recovery rate is repeatedly tested; (4) Tensile strength test: the electronic fiber strength tester is used to test the composite paper yarn sample, the tensile speed is 20mm / min, and the pre-tension is 0.05cN.
[0053] Each example is tested according to the above method, and the results are shown in Table 1. According to the data in Table 1, the composite yarns prepared in Examples 1-3 have long-lasting antibacterial ability, tensile strength, elasticity and elastic recovery ability; in Example 4, equimolar octaethylene glycol is used instead of tetraethylene glycol in the preparation of the functional monomer, and the long ether bond segment leads to weakened intermolecular force, resulting in a decrease in the elastic recovery rate of the composite yarn; in Example 5, equimolar 1,14-tetradecanediol is used instead of tetraethylene glycol in the preparation of the functional monomer, and the monomer structure does not have a flexible ether bond, thereby reducing the tensile strength of the composite yarn, but the elasticity is not significantly improved; in Example 6, the preparation method of the functional monomer is changed, thereby leading to a decrease in the elastic recovery ability and antibacterial ability of the composite yarn; in Example 7, the quaternary ammonium salt structure is not introduced in the preparation of the functional monomer, leading to a decrease in the antibacterial performance of the composite yarn; in Comparative Example 1, commercially available polyester chips are used instead of the polyester chips in step (2), and the structure does not contain an ether bond, a quaternary ammonium salt structure and a dynamic reversible chemical bond, leading to a decrease in the antibacterial ability, tensile strength, elasticity and elastic recovery ability of the composite yarn.
[0054] The above description is only a preferred embodiment of the present application, and does not limit the present application in any form. Although the present application has been disclosed as above with reference to the preferred embodiments, the present application is not limited thereto. Any person skilled in the art can make some changes or modifications to the above disclosed technical contents without departing from the scope of the technical solutions of the present application, and any simple modification, equivalent change and modification made according to the technical essence of the present application to the above embodiments are still within the scope of the technical solutions of the present application.
Claims
1. A method of producing an antibacterial high-elasticity composite yarn, characterized by, It comprises the following steps: (1) Under the protection of nitrogen, terephthalic acid, functional monomer and ethylene glycol are configured into slurry with auxiliary agent and catalyst, added into esterification reactor, pressure is controlled at 0.1-0.2 MPa, temperature is controlled at 220-250℃, stirred for 2-3h, then catalyst is added, temperature is raised to 250-290℃, pressure is reduced to 60-80 Pa, reacted for 2-4h, after reaction, underwater granulation is carried out to obtain polyester chip; (2) The polyester chip obtained in step (1) is blended with antioxidant and dispersant, melt extruded to obtain polyester fiber, then the polyester fiber is blended with cotton fiber to obtain antibacterial high-elasticity composite yarn.
2. The method of making an antimicrobial, high-elasticity composite yarn according to claim 1, wherein, The molar ratio of terephthalic acid, functional monomer and ethylene glycol is 1:(0.2-0.4):(1.1-1.4).
3. The method of making an antimicrobial, high-elasticity composite yarn according to claim 1, wherein, The auxiliary agent is trimethyl phosphate.
4. The method of making an antimicrobial, high-elasticity composite yarn according to claim 1, wherein, The catalyst is one or more of ethylene glycol antimony, antimony oxide and antimony acetate.
5. The method of making an antimicrobial, high-elasticity composite yarn according to claim 1, wherein, The structure of the functional monomer is shown in formula I: (Ⅰ); In formula I, X is Br, Cl or I; n is an integer of 0-5.
6. The method of making an antimicrobial, high-elasticity composite yarn according to claim 5, wherein, The preparation method of the functional monomer comprises the following steps: S1, under the atmosphere of inert protective gas, polyether polyol and maleimide are mixed and added into tetrahydrofuran, temperature is lowered to -10-0℃, then tetraphenylphosphonium palladium and diethyl azodicarboxylate are added, then temperature is restored to room temperature, stirred for 24-26h, after reaction, column chromatography is carried out to purify to obtain the compound shown in formula II (Ⅱ); S2, 5-bromo-2-furoic acid and the compound shown in formula II in step S1 are mixed, then calcium chloride and deionized water are added, temperature is raised to 50-60℃, stirred for 6-8h, after reaction, the compound shown in formula III is obtained (Ⅲ); S3, allyl trimethyl ammonium halide, the compound shown in formula III in step S2, palladium acetate and tris(o-methylphenyl) phosphorus are mixed, added into toluene, DIPEA is added, temperature is raised to 70-80℃, stirred for 3-4h, after reaction, neutralized with 4-6wt% hydrochloric acid, organic phase is dried under reduced pressure, column chromatography is carried out to obtain the compound shown in formula I, i.e. the functional monomer.
7. The method of making an antimicrobial, high-elasticity composite yarn according to claim 6, wherein, In step S1, the molar ratio of polyether polyol and maleimide is 1:(2.1-2.5).
8. The method of making an antimicrobial, high-elasticity composite yarn according to claim 6, wherein, In step S2, the molar ratio of 5-bromo-2-furoic acid and the compound shown in formula II is 1:(2.2-2.4).
9. The method of making an antimicrobial, high-elasticity composite yarn according to claim 6, wherein, In step S3, the molar ratio of allyl trimethyl ammonium bromide and the compound shown in formula III is (2.1-2.4):
1.
10. The antibacterial high-elasticity composite yarn prepared by the preparation method of any one of claims 1-9.
Citation Information
Patent Citations
An antibacterial and insect-proof heat-generating composite yarn and its preparation method
CN113106589B