Flame-retardant antistatic polyester fiber and preparation method thereof
Through a combination of specific processes and materials, the prepared flame-retardant and anti-static polyester fiber solves the shortcomings of polyester fiber in flame-retardant and anti-static properties, and achieves multiple performance improvements, which are suitable for a variety of application scenarios.
Patent Information
- Application Number
- CN202510788036.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-13
- Publication Date
- 2025-08-19
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
When using halogen and phosphorus flame retardants, the existing polyester fibers have problems of combustion releasing highly toxic gases or attenuation of performance, and the coating is prone to falling off, making it difficult to achieve good antistatic properties at the same time.
Flame-retardant anti-static polyester fibers are prepared by mixing and stirring, melt extrusion and spinning processes, and functional additives are prepared by microfluidic chip coating and granulation technology and ultrasonic treatment. Functional additives are prepared by adding liquid crystal and graphene quantum dots to improve performance.
The prepared flame-retardant and anti-static polyester fiber has excellent flame-retardant, anti-static, anti-bacterial and radiation-proof properties, ensuring product quality and quality and broadening market application prospects.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of polyester fibers, in particular to a flame-retardant and antistatic polyester fiber and a preparation method thereof. Background Art
[0002] Polyester fiber, also known as polyester fiber, is made from purified terephthalic acid or dimethyl terephthalate and ethylene glycol as raw materials. It is a polyethylene terephthalate (PET) polymer made by esterification or ester exchange and polycondensation reaction, and then the fiber is made by spinning and post-processing.
[0003] In existing technologies, polyester fibers are mostly treated with halogenated flame retardants (such as decabromodiphenyl ether) or phosphorus-nitrogen synergistic flame retardants (such as ammonium polyphosphate APP). Although these materials can increase the limiting oxygen index (LOI), halogenated flame retardants release highly toxic gases such as dioxins when burned, and phosphorus-based flame retardants are easily hydrolyzed, resulting in performance degradation. At the same time, in order to improve the antistatic properties of polyester fibers, conductive polymers such as polypyrrole and polyaniline are used to coat the fiber surface, but the coating is easy to fall off.
[0004] Based on this, the present invention provides a flame-retardant and antistatic polyester fiber and a preparation method thereof to solve the above-mentioned technical problems. Summary of the Invention
[0005] The purpose of the present invention is to provide a flame retardant and antistatic polyester fiber and a preparation method thereof. The prepared flame retardant and antistatic polyester fiber not only has good flame retardant and antistatic properties, but also has excellent antibacterial and radiation protection properties, effectively ensuring its quality.
[0006] To achieve the above object, the present invention provides the following technical solutions: The first aspect of the present invention provides a flame-retardant antistatic polyester fiber, which is composed of the following raw materials in parts by weight: 30 to 40 parts of PET polyester chips, 3 to 6 parts of functional additives, 3 to 5 parts of synergistic additives and 2 to 5 parts of antioxidants.
[0007] The present invention is further configured as follows: the preparation process of the functional additive is as follows: The first preform is placed in a 1% by mass 3-methacrylic acid ethanol solution at a dosage ratio of 0.05 to 0.12 g / mL and ultrasonically treated for 20 to 30 minutes to obtain a second preform; Liquid crystal 5CB and cholesterol nonanoate are mixed in a mass ratio of 30 to 40:1 and heated to 85°C for melting. A second prefabricated material containing 5% by mass of liquid crystal 5CB is added thereto and stirred for 50 to 60 minutes. The mixture is then subjected to a constant temperature treatment at 85°C for 100 to 120 minutes in a 5T superconducting magnetic field to obtain a third prefabricated material. Polyimide was placed in N,N-dimethylformamide at a dosage ratio of 0.18 to 0.24 g / mL and ultrasonically treated for 10 to 15 minutes, montmorillonite (0.2% by weight of the polyimide) and aluminum hypophosphite (0.4% by weight of the polyimide) were added thereto, and the ultrasonic treatment was continued for 20 to 30 minutes to obtain a fourth preform; The two syringes are connected to the dual channels of the microfluidic chip respectively, and then the third preform and the fourth preform are respectively introduced through the dual channels of the microfluidic chip. The mixed preforms in the reaction process are then coated and granulated by a microfluidic electrostatic integrated machine to prepare a functional additive; The flow rate of the third preform is 0.1 mL / min, and the flow rate of the fourth preform is 0.3 mL / min.
[0008] The present invention is further configured as follows: the preparation process of the first prefabricated material is as follows: The composite material is placed in the composite liquid at a dosage ratio of 0.18-0.22 g / mL, and magnetically stirred at 50-60°C for 120-140 minutes. The temperature is then raised to 190-200°C and constant temperature treated for 12-14 hours. The mixture is cooled to room temperature and centrifuged at 10,000-12,000 r / min for 15-20 minutes. The precipitate is collected and the resulting precipitate is placed in cyclohexane at a dosage ratio of 0.15-0.2 g / mL. A 4.12-4.52% by mass tetrachloroauric acid aqueous solution is added thereto, wherein the amount of the tetrachloroauric acid aqueous solution added is 40-50% by volume of the cyclohexane. A sodium borohydride aqueous solution at a mass fraction of 90-100% of the tetrachloroauric acid aqueous solution is then added dropwise thereto, wherein the mass fraction of the sodium borohydride aqueous solution is 12%. The mixture is ultrasonically treated at 6-8°C for 15-20 minutes. After the ultrasonication is completed, the mixture is centrifuged at 10,000 to 12,000 r / min for 15 to 20 minutes, the obtained precipitate is washed with deionized water 2 to 4 times, and the obtained precipitate product is placed in cyclohexane at a dosage ratio of 0.15 to 0.2 g / mL. A graphene quantum dot GQDs aqueous solution with a volume of 70 to 80% of cyclohexane is added thereto and ultrasonically treated for 20 to 30 minutes, wherein the mass fraction of the graphene quantum dot GQDs aqueous solution is 0.5 to 0.8%, and then vacuum dried to obtain a first preform.
[0009] The present invention is further configured as follows: the composite material is formed by mixing bismuth nitrate pentahydrate and tellurium dioxide in a mass ratio of 2.1 to 2.5:1.
[0010] The present invention is further configured as follows: the compound liquid is prepared by mixing oleic acid and oleylamine in a volume ratio of 1:1.
[0011] The present invention is further configured as follows: the preparation process of the synergistic aid is as follows: L-cystine and D-cystine are mixed in a mass ratio of 1:1 to obtain a first mixture, and the first mixture is placed in water at a dosage ratio of 0.05 to 0.08 g / mL. After evacuating the air, the mixture is heated to 374 to 380°C at a rate of 5°C / min and pressurized to 22.1 to 22.5 MPa for 100 to 120 minutes. The mixture is cooled to room temperature and centrifuged at 8,000 to 10,000 r / min for 10 to 15 minutes. The supernatant is dialyzed through a 10 kDa dialysis bag for 46 to 48 hours, with the water being changed every 6 hours during the dialysis period, and then freeze-dried to obtain a powder. Under a nitrogen atmosphere and at 60-64° C., dimethyl 3,3'-dithiodipropionate, diarylethene DAE, and tetrahydrofuran are stirred for 5-6 hours, then irradiated with light at 254 nm and 20 mW / cm² for 10-15 minutes, then cured in a room temperature for 24-26 hours, crushed, immersed in tetrahydrofuran for 12-14 hours, and vacuum-dried to prepare a base material. The powder and the base material are mixed in a mass ratio of 0.3 to 0.4:1 to obtain a second mixture, and then the second mixture is ultrasonically treated in ethanol at a dosage ratio of 0.4 to 0.5 g / mL for 10 to 20 minutes and ball-milled for 4 to 6 hours. The ball-milled product is washed with ethanol 2 to 4 times and vacuum-dried to obtain a synergistic additive.
[0012] The present invention is further configured as follows: the mixing mass ratio of the dimethyl 3,3'-dithiodipropionate, diarylethene DAE and tetrahydrofuran is 1:0.3-0.5:80-85.
[0013] The present invention is further configured as follows: the antioxidant is selected from any one of antioxidant 1010, antioxidant 1076, and antioxidant CA.
[0014] The second aspect of the present invention also provides a method for preparing the flame retardant and antistatic polyester fiber, comprising the following steps: Step 1, accurately weighing PET polyester chips, functional additives, synergistic additives and antioxidants, and putting the PET polyester chips, functional additives, synergistic additives and antioxidants into a mixing device for mixing and stirring. After being evenly mixed, the chips are fed into a twin-screw extruder through a feed port, and the temperature of each zone is controlled at: 250-260° C. in zone 1, 270-280° C. in zone 2, 270-280° C. in zone 3, and 275-280° C. in zone 4. The screw speed is set at 80-100 r / min, and the chips are melt-extruded and pelletized to obtain PET pellets. Step 2: Place the PET pellets in a melt spinning machine, control the spinning temperature to 270-280°C, the screw speed to 450-500r / min, and the winding speed to 500-700m / min, perform melt spinning, and then undergo stretching and winding processes to obtain a flame-retardant and antistatic polyester fiber product.
[0015] Compared with the prior art, the present invention has the following beneficial effects: In the present invention, PET polyester chips, functional additives, synergistic additives and antioxidants are used as raw materials. The PET polyester chips, functional additives, synergistic additives and antioxidants are put into a mixing device for mixing and stirring. After being evenly mixed, the PET chips are fed into a twin-screw extruder through a feed port, melt-extruded, and pelletized to obtain PET pellets. The PET pellets are then placed in a melt spinning machine for melt spinning, and then subjected to a drawing and winding process to obtain a finished flame-retardant antistatic polyester fiber. The flame-retardant antistatic polyester fiber prepared by the present invention not only has good flame retardancy and antistatic properties, but also has excellent antibacterial and radiation protection properties, effectively ensuring its quality. The flame-retardant antistatic polyester fiber and its preparation method provided by the present invention have a broader market prospect and are more suitable for promotion. DETAILED DESCRIPTION
[0016] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.
[0017] Example 1: This example provides a flame-retardant and antistatic polyester fiber, which is composed of the following raw materials in parts by weight: 30 parts of PET polyester chips, 3 parts of functional additives, 3 parts of synergistic additives and 2 parts of antioxidants.
[0018] The preparation process of the functional additive is as follows: The first preform was placed in a 1% by mass 3-methacrylic acid ethanol solution at a dosage ratio of 0.05 g / mL and ultrasonically treated for 20 minutes to obtain a second preform; Liquid crystal 5CB and cholesterol nonanoate were mixed in a mass ratio of 30:1 and heated to 85°C to melt. A second prefabricated material containing 5% by mass of liquid crystal 5CB was added thereto and stirred for 50 minutes. The mixture was then subjected to a constant temperature treatment at 85°C for 100 minutes in a 5T superconducting magnetic field to obtain a third prefabricated material. Polyimide was placed in N,N-dimethylformamide at a dosage ratio of 0.18 g / mL and ultrasonically treated for 10 minutes. Montmorillonite (0.2% by weight of the polyimide) and aluminum hypophosphite (0.4% by weight of the polyimide) were added thereto, and the ultrasonic treatment was continued for 20 minutes to obtain a fourth preform. The two syringes are connected to the dual channels of the microfluidic chip respectively, and then the third preform and the fourth preform are respectively introduced through the dual channels of the microfluidic chip. The mixed preforms in the reaction process are then coated and granulated by a microfluidic electrostatic integrated machine to prepare a functional additive; The flow rate of the third preform is 0.1 mL / min, and the flow rate of the fourth preform is 0.3 mL / min.
[0019] Furthermore, the preparation process of the first prefabricated material is as follows: The composite material was placed in the composite liquid at a dosage ratio of 0.18 g / mL, magnetically stirred at 50°C for 120 minutes, then heated to 190°C and kept at this temperature for 12 hours, cooled to room temperature, and centrifuged at 10,000 r / min for 15 minutes. The precipitate was collected and placed in cyclohexane at a dosage ratio of 0.15 g / mL. A 4.12% by mass aqueous solution of tetrachloroauric acid was added thereto, wherein the amount of the tetrachloroauric acid aqueous solution added was 40% by volume of the cyclohexane. Then, a sodium borohydride aqueous solution with a mass fraction of 90% of the tetrachloroauric acid aqueous solution was added dropwise thereto, wherein the mass fraction of the sodium borohydride aqueous solution was 12%, and ultrasonic treatment was performed at 6°C for 15 minutes. After the ultrasonication is completed, the mixture is centrifuged at 10,000 r / min for 15 minutes, the obtained precipitate is washed twice with deionized water, and the obtained precipitate product is placed in cyclohexane at a dosage ratio of 0.15 g / mL. Then, a graphene quantum dot GQDs aqueous solution with a volume ratio of 70% of cyclohexane is added thereto and ultrasonically treated for 20 minutes, wherein the mass fraction of the graphene quantum dot GQDs aqueous solution is 0.5%, and then vacuum dried to obtain a first preform.
[0020] The composite material is prepared by mixing bismuth nitrate pentahydrate and tellurium dioxide in a mass ratio of 2.1:1.
[0021] The compound solution is prepared by mixing oleic acid and oleylamine in a volume ratio of 1:1.
[0022] In addition, the preparation process of the synergist is as follows: L-cystine and D-cystine were mixed in a mass ratio of 1:1 to obtain a first mixture, and the first mixture was placed in water at a dosage of 0.05-0.08 g / mL. After evacuating the air, the mixture was heated to 374°C at a rate of 5°C / min and pressurized to 22.1 MPa for 100 min. The mixture was cooled to room temperature and centrifuged at 8000 rpm for 10 min. The supernatant was dialyzed through a 10 kDa dialysis bag for 46 h, with the water being changed every 6 h during the dialysis period, and then freeze-dried to obtain a powder. Dimethyl 3,3'-dithiodipropionate, diarylethene (DAE), and tetrahydrofuran were stirred at 60°C in a nitrogen atmosphere for 5 hours, then irradiated with light at 254 nm and 20 mW / cm² for 10 minutes, and then cured in a room temperature for 24 hours. The mixture was crushed, immersed in tetrahydrofuran for 12 hours, and vacuum-dried to obtain a base material. The powder and the base material were mixed in a mass ratio of 0.3:1 to obtain a second mixture. The second mixture was then ultrasonically treated in ethanol at a dosage ratio of 0.4 g / mL for 10 minutes and ball-milled for 4 hours. The ball-milled product was washed twice with ethanol and vacuum-dried to obtain a synergistic additive.
[0023] The mixing mass ratio of dimethyl 3,3'-dithiodipropionate, diarylethene DAE and tetrahydrofuran is 1:0.3:80.
[0024] Antioxidant 1010 was selected as the antioxidant.
[0025] In addition, this embodiment also provides a method for preparing the flame-retardant and antistatic polyester fiber, comprising the following steps: Step 1. Accurately weigh PET polyester chips, functional additives, synergistic additives, and antioxidants, and place the PET polyester chips, functional additives, synergistic additives, and antioxidants into a mixing device for mixing and stirring. After being uniformly mixed, the chips are fed into a twin-screw extruder through a feed port. The temperatures of each zone are controlled at: 250° C. in zone 1, 270° C. in zone 2, 270° C. in zone 3, and 275° C. in zone 4. The screw speed is set at 80 r / min, and the chips are melt-extruded and pelletized to obtain PET pellets. Step 2: Place the PET pellets in a melt spinning machine, control the spinning temperature to 270°C, the screw speed to 450r / min, and the winding speed to 500m / min, perform melt spinning, and then undergo stretching and winding processes to obtain a flame retardant and antistatic polyester fiber product.
[0026] Example 2: The preparation method of the flame-retardant antistatic polyester fiber provided in this example is basically the same as that in Example 1, except that the specific raw material composition and specific preparation method of the flame-retardant antistatic polyester fiber in this example are different; the specific raw material composition and specific preparation method of the flame-retardant antistatic polyester fiber in this example are as follows: Disclosed is a flame-retardant and antistatic polyester fiber, which is composed of the following raw materials in parts by weight: 35 parts of PET polyester chips, 4 parts of functional additives, 4 parts of synergistic additives, and 4 parts of antioxidants.
[0027] The preparation process of the functional additive is as follows: The first preform was placed in a 1% by mass 3-methacrylic acid ethanol solution at a dosage ratio of 0.07 g / mL and subjected to ultrasonic treatment for 25 minutes to obtain a second preform; Liquid crystal 5CB and cholesterol nonanoate were mixed in a mass ratio of 35:1 and heated to 85°C to melt. A second prefabricated material containing 5% by mass of liquid crystal 5CB was added thereto and stirred for 55 minutes. The mixture was then subjected to a constant temperature treatment at 85°C for 110 minutes in a 5T superconducting magnetic field to obtain a third prefabricated material. Polyimide was placed in N,N-dimethylformamide at a dosage ratio of 0.21 g / mL and ultrasonically treated for 12 minutes. Montmorillonite (0.2% by weight of the polyimide) and aluminum hypophosphite (0.4% by weight of the polyimide) were added thereto, and ultrasonic treatment was continued for 25 minutes to obtain a fourth preform. The two syringes are connected to the dual channels of the microfluidic chip respectively, and then the third preform and the fourth preform are respectively introduced through the dual channels of the microfluidic chip. The mixed preforms in the reaction process are then coated and granulated by a microfluidic electrostatic integrated machine to prepare a functional additive; The flow rate of the third preform is 0.1 mL / min, and the flow rate of the fourth preform is 0.3 mL / min.
[0028] Furthermore, the preparation process of the first prefabricated material is as follows: The composite material was placed in the composite liquid at a dosage ratio of 0.2 g / mL, magnetically stirred at 55°C for 130 minutes, then heated to 195°C and kept at this temperature for 13 hours, cooled to room temperature, and centrifuged at 10,000-12,000 r / min for 17 minutes. The precipitate was collected and placed in cyclohexane at a dosage ratio of 0.17 g / mL. A 4.37% by mass aqueous solution of tetrachloroauric acid was added thereto, wherein the amount of the tetrachloroauric acid aqueous solution added was 45% of the volume of the cyclohexane. Then, a sodium borohydride aqueous solution with a mass fraction of 95% of the tetrachloroauric acid aqueous solution was added dropwise thereto, wherein the mass fraction of the sodium borohydride aqueous solution was 12%, and ultrasonic treatment was performed at 7°C for 17 minutes. After the ultrasonication is completed, the mixture is centrifuged at 11000 r / min for 17 minutes, and the obtained precipitate is washed three times with deionized water. The obtained precipitate product is placed in cyclohexane at a dosage ratio of 0.17 g / mL, and then a graphene quantum dot GQDs aqueous solution with a volume ratio of 75% of cyclohexane is added thereto and ultrasonically treated for 25 minutes, wherein the mass fraction of the graphene quantum dot GQDs aqueous solution is 0.7%, and then vacuum dried to obtain a first preform.
[0029] The composite material is prepared by mixing bismuth nitrate pentahydrate and tellurium dioxide in a mass ratio of 2.3:1.
[0030] The compound solution is prepared by mixing oleic acid and oleylamine in a volume ratio of 1:1.
[0031] In addition, the preparation process of the synergist is as follows: L-cystine and D-cystine were mixed in a mass ratio of 1:1 to obtain a first mixture, and the first mixture was placed in water at a dosage of 0.06 g / mL. After evacuating the air, the mixture was heated to 377°C at a rate of 5°C / min and pressurized to 22.3 MPa for 110 min. The mixture was cooled to room temperature and centrifuged at 9000 rpm for 12 min. The supernatant was dialyzed through a 10 kDa dialysis bag for 47 h, with the water changed every 6 h during the dialysis period, and then freeze-dried to obtain a powder. Dimethyl 3,3'-dithiodipropionate, diarylethene (DAE), and tetrahydrofuran were stirred under a nitrogen atmosphere at 62°C for 6 hours, then irradiated with light at 254 nm and 20 mW / cm² for 12 minutes, and then cured in a room temperature for 25 hours. The mixture was crushed, immersed in tetrahydrofuran for 13 hours, and vacuum-dried to obtain a base material. The powder and the base material were mixed in a mass ratio of 0.4:1 to obtain a second mixture. The second mixture was then ultrasonically treated in ethanol at a dosage ratio of 0.5 g / mL for 15 minutes and ball-milled for 5 hours. The ball-milled product was washed three times with ethanol and vacuum-dried to obtain a synergistic additive.
[0032] The mixing mass ratio of dimethyl 3,3'-dithiodipropionate, diarylethene DAE and tetrahydrofuran is 1:0.4:82.
[0033] Antioxidant 1076 was selected as the antioxidant.
[0034] In addition, this embodiment also provides a method for preparing the flame-retardant and antistatic polyester fiber, comprising the following steps: Step 1. Accurately weigh PET polyester chips, functional additives, synergistic additives, and antioxidants, and place the PET polyester chips, functional additives, synergistic additives, and antioxidants into a mixing device for mixing and stirring. After being uniformly mixed, the chips are fed into a twin-screw extruder through a feed port. The temperatures of each zone are controlled at: 255° C. in zone 1, 275° C. in zone 2, 275° C. in zone 3, and 280° C. in zone 4. The screw speed is set at 90 r / min, and the chips are melt-extruded and pelletized to obtain PET pellets. Step 2: Place the PET pellets in a melt spinning machine, control the spinning temperature to 275°C, the screw speed to 475r / min, and the winding speed to 600m / min, perform melt spinning, and then undergo stretching and winding processes to obtain a flame-retardant and antistatic polyester fiber product.
[0035] Example 3: The preparation method of the flame-retardant antistatic polyester fiber provided in this example is basically the same as that in Example 1, except that the specific raw material composition and specific preparation method of the flame-retardant antistatic polyester fiber in this example are different; the specific raw material composition and specific preparation method of the flame-retardant antistatic polyester fiber in this example are as follows: Disclosed is a flame-retardant and antistatic polyester fiber, which is composed of the following raw materials in parts by weight: 40 parts of PET polyester chips, 6 parts of functional additives, 5 parts of synergistic additives and 5 parts of antioxidants.
[0036] The preparation process of the functional additive is as follows: The first preform was placed in a 1% by mass 3-methacrylic acid ethanol solution at a dosage ratio of 0.12 g / mL and ultrasonically treated for 30 minutes to obtain a second preform; Liquid crystal 5CB and cholesterol nonanoate were mixed in a mass ratio of 40:1 and heated to 85°C to melt. A second prefabricated material containing 5% by mass of liquid crystal 5CB was added thereto and stirred for 60 minutes. The mixture was then subjected to a constant temperature treatment at 85°C for 120 minutes in a 5T superconducting magnetic field to obtain a third prefabricated material. Polyimide was placed in N,N-dimethylformamide at a dosage ratio of 0.24 g / mL and ultrasonically treated for 15 minutes. Montmorillonite (0.2% by weight of the polyimide) and aluminum hypophosphite (0.4% by weight of the polyimide) were added thereto, and the ultrasonic treatment was continued for 30 minutes to obtain a fourth preform. The two syringes are connected to the dual channels of the microfluidic chip respectively, and then the third preform and the fourth preform are respectively introduced through the dual channels of the microfluidic chip. The mixed preforms in the reaction process are then coated and granulated by a microfluidic electrostatic integrated machine to prepare a functional additive; The flow rate of the third preform is 0.1 mL / min, and the flow rate of the fourth preform is 0.3 mL / min.
[0037] Furthermore, the preparation process of the first prefabricated material is as follows: The composite material was placed in the composite liquid at a dosage ratio of 0.22 g / mL, magnetically stirred at 60°C for 140 minutes, then heated to 200°C and kept at this temperature for 14 hours, cooled to room temperature, and centrifuged at 12,000 r / min for 20 minutes. The precipitate was collected and placed in cyclohexane at a dosage ratio of 0.2 g / mL. A 4.52% by mass aqueous solution of tetrachloroauric acid was added thereto, wherein the amount of the tetrachloroauric acid aqueous solution added was 50% of the volume of the cyclohexane. Then, a sodium borohydride aqueous solution with a mass fraction of 100% of the tetrachloroauric acid aqueous solution was added dropwise thereto, wherein the mass fraction of the sodium borohydride aqueous solution was 12%, and ultrasonic treatment was performed at 8°C for 20 minutes. After the ultrasonication is completed, the mixture is centrifuged at 12000 r / min for 20 minutes, the obtained precipitate is washed 4 times with deionized water, and the obtained precipitate product is placed in cyclohexane at a dosage ratio of 0.2 g / mL. Then, a graphene quantum dot GQDs aqueous solution with a volume ratio of 80% of cyclohexane is added thereto and ultrasonically treated for 30 minutes, wherein the mass fraction of the graphene quantum dot GQDs aqueous solution is 0.8%, and then vacuum dried to obtain a first preform.
[0038] The composite material is prepared by mixing bismuth nitrate pentahydrate and tellurium dioxide in a mass ratio of 2.5:1.
[0039] The compound solution is prepared by mixing oleic acid and oleylamine in a volume ratio of 1:1.
[0040] In addition, the preparation process of the synergist is as follows: L-cystine and D-cystine were mixed in a mass ratio of 1:1 to obtain a first mixture, and the first mixture was placed in water at a dosage of 0.08 g / mL. After evacuating the air, the mixture was heated to 380°C at a rate of 5°C / min and pressurized to 22.5 MPa for 120 min. The mixture was cooled to room temperature and centrifuged at 10,000 rpm for 15 min. The supernatant was dialyzed through a 10 kDa dialysis bag for 48 h, with the water changed every 6 h during the dialysis period, and then freeze-dried to obtain a powder. Dimethyl 3,3'-dithiodipropionate, diarylethene (DAE), and tetrahydrofuran were stirred under a nitrogen atmosphere at 64°C for 6 hours, then irradiated with light at 254 nm and 20 mW / cm² for 15 minutes, and then cured in a room temperature for 26 hours. The mixture was crushed, immersed in tetrahydrofuran for 14 hours, and vacuum-dried to obtain a base material. The powder and the base material were mixed in a mass ratio of 0.4:1 to obtain a second mixture. The second mixture was then ultrasonically treated in ethanol at a dosage ratio of 0.5 g / mL for 20 minutes and ball-milled for 6 hours. The ball-milled product was washed four times with ethanol and vacuum-dried to obtain a synergistic additive.
[0041] The mixing mass ratio of dimethyl 3,3'-dithiodipropionate, diarylethene DAE and tetrahydrofuran is 1:0.5:85.
[0042] The antioxidant used is antioxidant CA.
[0043] In addition, this embodiment also provides a method for preparing the flame-retardant and antistatic polyester fiber, comprising the following steps: Step 1, accurately weighing PET polyester chips, functional additives, synergistic additives and antioxidants, and adding the PET polyester chips, functional additives, synergistic additives and antioxidants into a mixing device for mixing and stirring. After being evenly mixed, the chips are fed into a twin-screw extruder through a feed port, and the temperatures of each zone are controlled at: 260° C. in zone 1, 280° C. in zone 2, 270° C. in zone 3, and 280° C. in zone 4. The screw speed is set at 100 r / min, and the chips are melt-extruded and pelletized to obtain PET pellets. Step 2: Place the PET pellets in a melt spinning machine, control the spinning temperature to 280°C, the screw speed to 500r / min, and the winding speed to 700m / min, perform melt spinning, and then undergo stretching and winding processes to obtain a flame-retardant and antistatic polyester fiber product.
[0044] Comparative Example 1: The difference from Example 1 is that this example does not contain a functional additive.
[0045] Comparative Example 2: The difference from Example 1 is that this example does not contain a synergistic aid.
[0046] Comparative Example 3: The difference from Example 1 is that this example does not contain functional additives and synergistic additives.
[0047] Performance test: The flame retardant and antistatic polyester fiber samples provided in Examples 1 to 3 and Comparative Examples 1 to 3 are marked as Examples 1 to 3 and Comparative Examples 1 to 3, respectively; and the relevant properties of the flame retardant and antistatic polyester fibers provided in Examples 1 to 3 and Comparative Examples 1 to 3 are tested as follows: 1. Flame retardant test: The test method is Limiting Oxygen Index (LOI): GB / T 2406-2009; Vertical Burning Grade: UL94-2020.
[0048] 2. Antistatic test: The test method is to weave each group of flame retardant antistatic polyester fibers into fabrics with a specification of 220×220 (roots / inch) 2 ), and cut into 5cm×5cm sample cloth, test its surface conductivity, and evaluate its antistatic performance.
[0049] 3. Antibacterial test: The test method is ISO 20743:2021.
[0050] 4. Radiation protection test: The test method is X-ray shielding efficiency (100 keV): ASTM F2547-18.
[0051] The obtained test data are recorded in Tables 1 to 4 below: Table 1 Flame retardant performance test results of each group of flame retardant antistatic polyester fibers
[0052] Table 2 Conductivity test results of each group of flame retardant and antistatic polyester fibers
[0053] Table 3 Conductivity test results of each group of flame retardant and antistatic polyester fibers
[0054] Table 4 Radiation protection test results of each group of flame retardant and antistatic polyester fibers
[0055] Comparison and analysis of the relevant data in Tables 1 to 4 show that the flame-retardant, antistatic polyester fiber prepared by the present invention not only exhibits excellent flame retardancy and antistatic properties, but also possesses superior antibacterial and radiation protection properties, effectively guaranteeing its quality. This demonstrates that the flame-retardant, antistatic polyester fiber and its preparation method provided by the present invention have a broader market prospect and are more suitable for promotion.
[0056] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
[0057] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A flame retardant antistatic polyester fiber, characterized in that: The invention is composed of the following raw materials in parts by weight: 30 to 40 parts of PET polyester chips, 3 to 6 parts of functional additives, 3 to 5 parts of synergistic additives and 2 to 5 parts of antioxidants; The preparation process of the functional additive is as follows: placing the first preform in a 3-methacrylic acid ethanol solution for ultrasonic treatment to obtain a second preform; Liquid crystal 5CB and cholesterol nonanoate are mixed and heated to melt, the second prefabricated material is added thereto and stirred, and then the mixture is subjected to constant temperature treatment in a 5T superconducting magnetic field to obtain a third prefabricated material; placing polyimide in N,N-dimethylformamide for ultrasonic treatment, adding montmorillonite and aluminum hypophosphite thereto, and continuing ultrasonic treatment to obtain a fourth preform; The two syringes are connected to the dual channels of the microfluidic chip respectively, and then the third preform and the fourth preform are respectively introduced through the dual channels of the microfluidic chip. The mixed preforms in the reaction process are then coated and granulated by a microfluidic electrostatic integrated machine to prepare a functional additive; The flow rate of the third preform is 0.1 mL / min, and the flow rate of the fourth preform is 0.3 mL / min.
2. The flame-retardant antistatic polyester fiber according to claim 1, characterized in that: The preparation process of the first prefabricated material is as follows: The composite material is placed in the composite liquid, magnetically stirred, then heated to a constant temperature, cooled to room temperature, centrifuged, and the precipitate is collected. The resulting precipitate is placed in cyclohexane, and then a tetrachloroauric acid aqueous solution is added thereto, and then a sodium borohydride aqueous solution is added thereto dropwise, and ultrasonic treatment is performed; After the ultrasonic treatment, the mixture was centrifuged and the obtained precipitate was washed with deionized water. The obtained precipitate product was placed in cyclohexane, and then a graphene quantum dot GQDs aqueous solution was added thereto for ultrasonic treatment, and then vacuum dried to obtain a first prefabricated material.
3. The flame-retardant antistatic polyester fiber according to claim 2, characterized in that: The composite material is prepared by mixing bismuth nitrate pentahydrate and tellurium dioxide in a mass ratio of 2.1 to 2.5:
1.
4. The flame-retardant antistatic polyester fiber according to claim 2, characterized in that: The compound liquid is prepared by mixing oleic acid and oleylamine in a volume ratio of 1:
1.
5. The flame-retardant and antistatic polyester fiber according to claim 1, characterized in that: The preparation process of the synergistic adjuvant is as follows: L-cystine and D-cystine are mixed to obtain a first mixture, and the first mixture is placed in water, after the air is evacuated, the temperature is increased and the pressure is applied simultaneously for 100 to 120 minutes, the mixture is cooled to room temperature, and the mixture is centrifuged. The supernatant is dialyzed through a 10 kDa dialysis bag for 46 to 48 hours, with the water being changed every 6 hours during the dialysis period, and the mixture is then freeze-dried to obtain a powder; Under a nitrogen atmosphere and at 60-64°C, dimethyl 3,3'-dithiodipropionate, diarylethene (DAE), and tetrahydrofuran are stirred, then irradiated with light at 254 nm and 20 mW / cm², solidified in a room temperature, crushed, immersed in tetrahydrofuran, and vacuum-dried to prepare a base material. The powder and the base material are mixed to obtain a second mixture, and the second mixture is then placed in ethanol for ultrasonic treatment and ball milled. The ball milled product is washed with ethanol and vacuum dried to obtain a synergistic auxiliary agent.
6. The flame-retardant antistatic polyester fiber according to claim 5, characterized in that: The mixing mass ratio of the dimethyl 3,3'-dithiodipropionate, diarylethene DAE and tetrahydrofuran is 1:0.3-0.5:80-85.
7. The flame-retardant and antistatic polyester fiber according to claim 1, characterized in that: The antioxidant is selected from any one of antioxidant 1010, antioxidant 1076, and antioxidant CA.
8. The method for preparing a flame-retardant and antistatic polyester fiber according to any one of claims 1 to 7, characterized in that: The following steps are involved: Step 1: Accurately weigh PET polyester chips, functional additives, synergistic additives, and antioxidants, and place them into a mixing device for mixing and stirring. After uniform mixing, the mixture is fed into a twin-screw extruder through a feed port, and the screw speed is set, melt-extruded, and pelletized to obtain PET pellets. Step 2: Place the PET pellets in a melt spinning machine for melt spinning, and then go through the drawing and winding processes to obtain a flame retardant and antistatic polyester fiber product.
Citation Information
Patent Citations
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