Medical antibacterial antistatic modified polyester cotton type fabric and preparation method thereof
By introducing modified lignin and antibacterial flame retardant monomers into polyester fabrics, the problems of static electricity, poor hygroscopicity and insufficient antibacterial performance of polyester fabrics in the medical field are solved, and the antistatic, flame retardant, antibacterial and anti-light aging properties of the fabrics are improved.
Patent Information
- Application Number
- CN202510731587.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-03
- Publication Date
- 2025-09-12
AI Technical Summary
Existing polyester fabrics have problems such as static electricity, poor moisture absorption and insufficient antibacterial properties when used in the medical field.
Pre-modified lignin is prepared by reacting pretreated lignin with p-aminosalicylic acid, which is then reacted with aniline and p-aminosalicylic acid to generate modified lignin, which is combined with methyldiethanolamine and diethyl chloromethyl phosphate to obtain an antibacterial flame retardant monomer, and finally reacted with terephthalic acid and ethylene glycol to obtain modified polyester, which is then extruded and spun into medical antibacterial and antistatic modified polyester cotton fabric.
The fabric has good anti-static, flame retardant, antibacterial and anti-light aging properties, and has improved the comprehensive performance of medical fabrics.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of fiber fabrics, in particular to a medical antibacterial and antistatic modified polyester cotton fabric and a preparation method thereof. Background Art
[0002] Polyester, also known as polyester fiber, is a synthetic fiber made from organic dibasic acids and diols through chemical polycondensation. It is a type of polymer compound and is currently the most predominant type of synthetic fiber. Polyester offers many advantages. First, it exhibits excellent wrinkle resistance and shape retention, making clothing less prone to wrinkling and retaining its original shape during wear. Second, polyester fiber possesses high strength and elastic recovery, making the resulting fabric durable and able to quickly return to its original shape. Furthermore, polyester is abrasion-resistant and lint-resistant, giving the fabric a more polished appearance. Polyester is widely used in textile and apparel manufacturing, bringing convenience and comfort to our daily lives.
[0003] While polyester has many advantages, it also suffers from poor hygroscopicity and prone to static electricity. Medical fabrics also have high requirements for antibacterial properties. The medical antibacterial and antistatic modified polyester cotton fabric prepared by the present invention has excellent antistatic, flame retardant, antibacterial, and light aging resistance properties, and has broad market prospects. Summary of the Invention
[0004] The purpose of the present invention is to provide a method for preparing a medical antibacterial and antistatic modified polyester cotton fabric to solve the problems existing in the prior art.
[0005] In order to solve the above technical problems, the present invention provides the following technical solutions:
[0006] A medical antibacterial and antistatic modified polyester cotton fabric is prepared by reacting pretreated lignin and p-aminosalicylic acid to obtain premodified lignin; reacting premodified lignin, aniline, and p-aminosalicylic acid to obtain modified lignin; reacting methyldiethanolamine and diethyl chloromethyl phosphate to obtain an antibacterial and flame-retardant monomer; reacting terephthalic acid, ethylene glycol, and an antibacterial and flame-retardant monomer to obtain modified polyester; and extruding the modified polyester and modified lignin through an extruder, spinning, and weaving the resulting fabric.
[0007] A method for preparing a medical antibacterial and antistatic modified polyester cotton fabric comprises the following steps:
[0008] (1) Pretreated lignin, para-aminosalicylic acid, and 0.1 mol / L sulfuric acid solution were mixed in a mass ratio of 1:(2-4):(1-1.2), stirred at 80-90°C and 600-800 r / min for 4-6 hours, filtered, and the filter residue was washed with deionized water for 3-5 times to obtain pre-modified lignin;
[0009] (2) Mixing 2.4 to 2.6 times the mass of aniline with ammonium persulfate, 1.4 to 1.6 times the mass of aniline with a mass concentration of 98% concentrated sulfuric acid, and 10 to 20 times the mass of aniline with deionized water to prepare an initiator solution; mixing aniline, pre-modified lignin, para-aminosalicylic acid, 98% concentrated sulfuric acid, and deionized water, stirring at 200 to 300 r / min at 0°C for 25 to 35 minutes, dripping the initiator solution within 30 minutes, continuing stirring for 20 to 24 hours, filtering, washing the filter residue with anhydrous ethanol and deionized water for 3 to 5 times, respectively, and vacuum drying at 70 to 80°C for 4 to 6 hours to prepare modified lignin;
[0010] (3) Terephthalic acid, ethylene glycol, antibacterial flame retardant monomer, and ethylene glycol antimony are reacted to obtain modified polyester; the modified polyester and modified lignin are mixed in a mass ratio of 1: (0.2-0.4), melt-extruded and spun through a twin-screw extruder, left to stand for 2-4 hours, and spun on a spinning machine and then cooled to room temperature through a side-blown air tunnel to obtain polyester fiber; the polyester fiber and cotton fiber are blended to obtain blended yarn, and the blended yarn is warped on a warping machine and then woven into a plain fabric using a fully automatic rapier loom, with a warp density of 600 threads / 10 cm and a weft density of 500 threads / 10 cm, to obtain a medical antibacterial and antistatic modified polyester cotton fabric.
[0011] As an optimization, the preparation method of the pretreated lignin in step (1) is: mixing lignin, p-aminophenol and anhydrous ethanol in a mass ratio of 1: (2-4): (10-20), stirring at 80-90°C and 200-300 r / min for 2-4 hours, filtering, washing the filter residue with anhydrous ethanol 3-5 times, and vacuum drying at 60-70°C for 4-6 hours to obtain the product.
[0012] As an optimization, the mass ratio of the aniline, pre-modified lignin, p-aminosalicylic acid, concentrated sulfuric acid with a mass concentration of 98%, and deionized water in step (2) is 1: (0.2-0.3): (0.1-0.2): (1.4-1.6): (20-30).
[0013] As an optimization, the preparation method of the antibacterial flame retardant monomer in step (3) is: methyldiethanolamine, diethyl chloromethyl phosphate, and anhydrous ethanol are mixed in a mass ratio of 1: (1.4-1.6): (15-25), stirred at 80-90°C and 400-600 r / min for 20-24h, and rotary evaporated at 55-65°C for 20-30min.
[0014] As an optimization, the reaction process of the antibacterial flame retardant monomer in step (3) is as follows:
[0015]
[0016] As an optimization, the preparation method of the modified polyester in step (3) is as follows: terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to a reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, 0.0003 to 0.0007 times the mass of terephthalic acid is added to ethylene glycol antimony, and the mixture is stirred at 180 to 200° C. and a speed of 200 to 400 r / min for 1 to 2 hours, and the temperature is raised to 195 to 205° C. to continue the reaction. When the esterification water is no longer distilled, the pressure is adjusted to 90 to 110 Pa within 30 minutes, the temperature is raised to 225 to 235° C., the speed is adjusted to 50 to 70 r / min, and the mixture is stirred until the reaction terminates. Nitrogen is introduced to restore the pressure to normal pressure, and the mixture is cooled to room temperature. The obtained product is obtained by discharging.
[0017] As an optimization, the temperature of the twin-screw extruder in step (3) is: zone 1 temperature 260-270°C, zone 2 temperature 265-275°C, zone 3 temperature 270-280°C, zone 4 temperature 270-280°C, and die head temperature 260-270°C.
[0018] As an optimization, the spinning machine process parameters in step (3) are: spinning box temperature 275-285°C, spinneret aperture 0.24 mm, spinneret aperture aspect ratio 2, and winding speed 3000 m / min.
[0019] Compared with the prior art, the present invention has the following beneficial effects:
[0020] When preparing the medical antibacterial and antistatic modified polyester cotton-type fabric, the present invention comprises the following steps: reacting pretreated lignin and p-aminosalicylic acid to obtain premodified lignin; reacting the premodified lignin, aniline, and p-aminosalicylic acid to obtain modified lignin; reacting methyldiethanolamine and diethyl chloromethyl phosphate to obtain an antibacterial and flame-retardant monomer; reacting terephthalic acid, ethylene glycol, and an antibacterial and flame-retardant monomer to obtain modified polyester; and extruding the modified polyester and the modified lignin through an extruder, spinning and weaving the resulting fabric to obtain the medical antibacterial and antistatic modified polyester cotton-type fabric.
[0021] First, pre-modified lignin is prepared by reacting lignin with p-aminosalicylic acid, and a salicylate structure is introduced into the fabric. Under the irradiation of ultraviolet light, the ester bond on the salicylate undergoes a photolysis reaction to generate free radicals, which are rearranged to generate a 2-hydroxybenzophenone structure with ultraviolet absorption effect, effectively improving the anti-aging properties of the antibacterial and antistatic modified polyester cotton fabric; modified lignin is prepared by reacting pre-modified lignin, aniline, and p-aminosalicylic acid, and the p-aminosalicylic acid added during the polymerization process of polyaniline introduces a carboxyl group, which forms an electrostatic bond with the quaternary ammonium salt cation on the antibacterial flame retardant monomer, effectively improving the mechanical properties of the antibacterial and antistatic modified polyester cotton fabric, and polyaniline is formed by polymerization on the lignin-modified salicylic acid. Polyaniline has good conductive properties and can improve the antistatic properties of the medical antibacterial and antistatic modified polyester cotton fabric.
[0022] Secondly, methyldiethanolamine and diethyl chloromethyl phosphate are reacted to prepare an antibacterial flame retardant monomer, and the tertiary amine on the methyldiethanolamine reacts with the chloromethyl on the diethyl chloromethyl phosphate to form a quaternary ammonium salt. The quaternary ammonium salt, as a cation, can form an electrostatic bond with the carboxyl group on the modified lignin, effectively improving the mechanical properties of the antibacterial and antistatic modified polyester cotton fabric. In addition, the quaternary ammonium salt, as a cationic antibacterial structure, has good antibacterial properties and can improve the antibacterial properties of the medical antibacterial and antistatic modified polyester cotton fabric. On the other hand, the antibacterial flame retardant monomer prepared by the reaction of methyldiethanolamine and diethyl chloromethyl phosphate introduces a large amount of phosphorus element, which has a good carbonization-promoting effect, effectively improving the flame retardant properties of the medical antibacterial and antistatic modified polyester cotton fabric. DETAILED DESCRIPTION
[0023] 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 creative efforts are within the scope of protection of the present invention.
[0024] Example 1:
[0025] A method for preparing a medical antibacterial and antistatic modified polyester cotton fabric comprises the following steps:
[0026] (1) Lignin, p-aminophenol, and anhydrous ethanol were mixed in a mass ratio of 1:2:10, stirred at 80°C and 200 r / min for 2 h, filtered, and the filter residue was washed with anhydrous ethanol three times and vacuum dried at 60°C for 4 h to prepare pretreated lignin;
[0027] (2) Pretreated lignin, para-aminosalicylic acid, and 0.1 mol / L sulfuric acid solution were mixed in a mass ratio of 1:2:1, stirred at 80°C and 600 r / min for 4 h, filtered, and the filter residue was washed three times with deionized water to obtain pre-modified lignin;
[0028] (3) Mix 2.4 times the mass of ammonium persulfate of aniline, 1.4 times the mass of aniline with a mass concentration of 98% concentrated sulfuric acid, and 10 times the mass of aniline with a mass concentration of deionized water to prepare an initiator solution; mix aniline, pre-modified lignin, para-aminosalicylic acid, 98% concentrated sulfuric acid, and deionized water in a mass ratio of 1:0.2:0.1:1.4:20, stir at 200 r / min at 0°C for 25 minutes, drip the initiator solution within 30 minutes, continue stirring for 20 hours, filter, wash the filter residue with anhydrous ethanol and deionized water three times, respectively, and dry it in a vacuum at 70°C for 4 hours to prepare modified lignin;
[0029] (4) Methyldiethanolamine, diethyl chloromethyl phosphate, and anhydrous ethanol were mixed in a mass ratio of 1:1.4:15, stirred at 80°C and 400 r / min for 20 h, and rotary evaporated at 55°C for 20 min to prepare an antibacterial flame retardant monomer;
[0030] (5) Terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to the reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, and ethylene glycol antimony 0.0003 times the mass of terephthalic acid is added. The mixture is stirred at a speed of 200 r / min at 180°C for 1 hour, and the temperature is raised to 195°C to continue the reaction. When the esterification water is no longer distilled, the pressure is adjusted to 90 Pa within 30 minutes, the temperature is raised to 225°C, the speed is adjusted to 50 r / min, and the mixture is stirred until the reaction is terminated. Nitrogen is introduced to restore the pressure to normal pressure, and the mixture is cooled to room temperature. The modified polyester is obtained by discharging the modified polyester and the modified lignin in a mass ratio of 1:0.2, and the mixture is extruded through a twin-screw extruder. Melt extrusion spinning, zone one temperature 260°C, zone two temperature 265°C, zone three temperature 270°C, zone four temperature 270°C, machine head temperature 260°C, standing for 2h, spinning box temperature 275°C, spinneret aperture 0.24mm, spinneret aperture aspect ratio 2, winding rate 3000m / min, cooling to room temperature through a side-blown air tunnel to obtain polyester fiber; polyester fiber and cotton fiber are blended to obtain blended yarn, the blended yarn is warped with a warping machine and then spun into plain fabric with a fully automatic rapier loom, with a warp density of 600 pieces / 10cm and a weft density of 500 pieces / 10cm, to obtain medical antibacterial and antistatic modified polyester cotton fabric.
[0031] Example 2:
[0032] A method for preparing a medical antibacterial and antistatic modified polyester cotton fabric comprises the following steps:
[0033] (1) Lignin, p-aminophenol, and anhydrous ethanol were mixed in a mass ratio of 1:3:15, stirred at 85°C and 250 r / min for 3 h, filtered, and the filter residue was washed with anhydrous ethanol 4 times and vacuum dried at 65°C for 5 h to prepare pretreated lignin;
[0034] (2) Pretreated lignin, para-aminosalicylic acid, and 0.1 mol / L sulfuric acid solution were mixed in a mass ratio of 1:3:1.1, stirred at 85°C and 700 r / min for 5 h, filtered, and the filter residue was washed with deionized water 4 times to obtain pre-modified lignin;
[0035] (3) Mix 2.5 times the mass of ammonium persulfate of aniline, 1.5 times the mass of aniline with a mass concentration of 98% concentrated sulfuric acid, and 15 times the mass of aniline with a mass concentration of deionized water to prepare an initiator solution; mix aniline, pre-modified lignin, para-aminosalicylic acid, 98% concentrated sulfuric acid, and deionized water in a mass ratio of 1:0.25:0.15:1.5:25, stir at 250 r / min at 0°C for 30 minutes, drip the initiator solution within 30 minutes, continue stirring for 22 hours, filter, wash the filter residue with anhydrous ethanol and deionized water for 4 times, respectively, and dry it in a vacuum at 75°C for 5 hours to prepare modified lignin;
[0036] (4) Methyldiethanolamine, diethyl chloromethyl phosphate, and anhydrous ethanol were mixed in a mass ratio of 1:1.5:20, stirred at 85°C and 500 r / min for 22 h, and rotary evaporated at 60°C for 25 min to prepare an antibacterial flame retardant monomer;
[0037] (5) Terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to the reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, and ethylene glycol antimony 0.0005 times the mass of terephthalic acid is added. The mixture is stirred at a speed of 300 r / min at 190°C for 1.5 hours, and the temperature is raised to 200°C to continue the reaction. When the esterification water is no longer distilled, the pressure is adjusted to 100 Pa within 30 minutes, the temperature is raised to 230°C, the speed is adjusted to 60 r / min, and the mixture is stirred until the reaction is terminated. Nitrogen is introduced to restore the pressure to normal pressure, and the mixture is cooled to room temperature. The modified polyester and modified lignin are mixed in a mass ratio of 1:0.3 and extruded by a twin-screw extruder. The yarn was melt-extruded and spun out of the machine, with the temperature of zone 1 being 265°C, zone 2 being 270°C, zone 3 being 275°C, zone 4 being 275°C, and the head being at 265°C. The yarn was allowed to stand for 3 hours, the temperature of the spinning box being 280°C, the aperture of the spinneret being 0.24 mm, the aspect ratio of the spinneret being 2, the winding rate being 3000 m / min, and cooled to room temperature through a side-blown air tunnel to obtain polyester fiber; the polyester fiber was blended with cotton fiber to obtain blended yarn, which was warped on a warping machine and then spun into plain fabric using a fully automatic rapier loom, with a warp density of 600 pieces / 10 cm and a weft density of 500 pieces / 10 cm, to obtain medical antibacterial and antistatic modified polyester cotton fabric.
[0038] Example 3:
[0039] A method for preparing a medical antibacterial and antistatic modified polyester cotton fabric comprises the following steps:
[0040] (1) Lignin, p-aminophenol, and anhydrous ethanol were mixed in a mass ratio of 1:4:20, stirred at 90°C and 300 r / min for 4 h, filtered, and the filter residue was washed with anhydrous ethanol 5 times and vacuum dried at 70°C for 6 h to prepare pretreated lignin;
[0041] (2) Pretreated lignin, para-aminosalicylic acid, and 0.1 mol / L sulfuric acid solution were mixed in a mass ratio of 1:4:1.2, stirred at 90°C and 800 r / min for 6 h, filtered, and the filter residue was washed with deionized water 5 times to obtain pre-modified lignin;
[0042] (3) Mix 2.6 times the mass of ammonium persulfate of aniline, 1.6 times the mass of aniline with a mass concentration of 98% concentrated sulfuric acid, and 20 times the mass of aniline with deionized water to prepare an initiator solution; mix aniline, pre-modified lignin, para-aminosalicylic acid, 98% concentrated sulfuric acid, and deionized water in a mass ratio of 1:0.3:0.2:1.6:25, stir at 250 r / min at 0°C for 35 minutes, drip the initiator solution within 30 minutes, continue stirring for 24 hours, filter, wash the filter residue with anhydrous ethanol and deionized water for 5 times, respectively, and dry it in a vacuum at 80°C for 6 hours to prepare modified lignin;
[0043] (4) Methyldiethanolamine, diethyl chloromethyl phosphate, and anhydrous ethanol were mixed in a mass ratio of 1:1.6:25, stirred at 90°C and 600 r / min for 24 h, and rotary evaporated at 65°C for 30 min to prepare an antibacterial flame retardant monomer;
[0044] (5) Terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to the reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, and ethylene glycol antimony (0.0007 times the mass of terephthalic acid) is added. The mixture is stirred at a speed of 400 r / min at 200°C for 2 hours, and the temperature is raised to 205°C to continue the reaction. When the esterification water is no longer distilled, the pressure is adjusted to 110 Pa within 30 minutes, the temperature is raised to 235°C, the speed is adjusted to 70 r / min, and the mixture is stirred until the reaction is terminated. Nitrogen is introduced to restore the pressure to normal pressure, and the mixture is cooled to room temperature. The modified polyester and modified lignin are mixed in a mass ratio of 1:0.4 and extruded by a twin-screw extruder. The polyester fiber was prepared by melt extrusion spinning, with the temperature of zone 1 at 270°C, zone 2 at 275°C, zone 3 at 280°C, zone 4 at 280°C, and the head temperature at 270°C. The yarn was allowed to stand for 4 hours, the temperature of the spinning box at 285°C, the spinneret aperture at 0.24mm, the spinneret aperture aspect ratio at 2, the winding rate at 3000m / min, and the yarn was cooled to room temperature through a side-blown air tunnel. The polyester fiber was blended with cotton fiber to prepare a blended yarn, which was warped with a warping machine and then spun into a plain fabric using a fully automatic rapier loom. The warp density on the machine was 600 pieces / 10cm, and the weft density on the machine was 500 pieces / 10cm, to prepare a medical antibacterial and antistatic modified polyester cotton fabric.
[0045] Comparative Example 1:
[0046] The preparation method of the medical antibacterial and antistatic modified polyester cotton fabric of Comparative Example 1 is different from that of Example 2 in that step (4) is not performed, and step (5) is modified as follows: terephthalic acid and ethylene glycol are added to a reactor in a molar ratio of 1:1, nitrogen is introduced, 0.0005 times the mass of terephthalic acid is added to ethylene glycol antimony, stirred at 190°C at a speed of 300r / min for 1.5h, heated to 200°C and continued to react, when esterification water is no longer distilled, the pressure is adjusted to 100Pa within 30min, the temperature is raised to 230°C, the speed is adjusted to 60r / min and stirred until the reaction is terminated, nitrogen is introduced to restore the pressure to normal pressure, cooled to room temperature, and the modified polyester is obtained by discharging; the modified polyester and modified wood are separated. The raw materials were mixed in a mass ratio of 1:0.3, melt-extruded and spun through a twin-screw extruder at a temperature of 265°C in the first zone, 270°C in the second zone, 275°C in the third zone, and 275°C in the fourth zone, with a die head temperature of 265°C. The fibers were allowed to stand for 3 hours, the spinning manifold temperature was 280°C, the spinneret aperture was 0.24 mm, the spinneret aperture aspect ratio was 2, and the winding rate was 3000 m / min. The fibers were cooled to room temperature through a side-blown air tunnel to produce polyester fibers. The polyester fibers were blended with cotton fibers to produce blended yarns, which were warped using a warping machine and then woven into plain weave fabrics using a fully automatic rapier loom with a warp density of 600 yarns / 10 cm and a weft density of 500 yarns / 10 cm, thereby producing medical antibacterial and antistatic modified polyester cotton fabrics. The remaining steps were the same as in Example 2.
[0047] Comparative Example 2:
[0048] The preparation method of the medical antibacterial and antistatic modified polyester cotton fabric of Comparative Example 2 is different from that of Example 2 in that step (3) is not performed, and step (5) is modified as follows: terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to a reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, 0.0003 to 0.0007 times the mass of adipic acid of ethylene glycol antimony is added, and the mixture is stirred at a speed of 200 to 400 r / min at 180 to 200 ° C for 1 to 2 hours, and the temperature is raised to 195 to 205 ° C to continue the reaction. When the esterification water is no longer distilled, the pressure is adjusted to 90 to 110 Pa within 30 minutes, the temperature is raised to 225 to 235 ° C, the speed is adjusted to 50 to 70 r / min, and the mixture is stirred until the reaction is terminated. Nitrogen is introduced to restore the pressure to normal pressure, and the mixture is cooled to room temperature. The modified polyester is discharged. The pre-modified lignin is mixed in a mass ratio of 1:(0.2-0.4), melt-extruded and spun through a twin-screw extruder, with the temperature of zone one at 260-270°C, zone two at 265-275°C, zone three at 270-280°C, zone four at 270-280°C, and a die head at 260-270°C. The fiber is allowed to stand for 2-4 hours, the temperature of the spinning box at 275-285°C, the spinneret aperture at 0.24 mm, the spinneret aperture aspect ratio at 2, the winding rate at 3000 m / min, and cooled to room temperature through a side-blowing air tunnel to obtain polyester fiber; the polyester fiber is blended with cotton fiber to obtain blended yarn, the blended yarn is warped by a warping machine, and then spun into a plain weave fabric by a fully automatic rapier loom, with a warp density of 600 yarns / 10 cm and a weft density of 500 yarns / 10 cm, to obtain a medical antibacterial and antistatic modified polyester cotton fabric. The remaining steps are the same as in Example 2.
[0049] Comparative Example 3:
[0050] The preparation method of the medical antibacterial and antistatic modified polyester cotton fabric of Comparative Example 2 differs from that of Example 2 in that steps (1) and (2) are not performed, and step (3) is modified as follows: ammonium persulfate (2.4 to 2.6 times the mass of aniline), concentrated sulfuric acid (98% by mass) (1.4 to 1.6 times the mass of aniline), and deionized water (10 to 20 times the mass of aniline) are mixed to prepare an initiator solution; aniline, para-aminosalicylic acid, concentrated sulfuric acid (98% by mass), and deionized water are mixed in a mass ratio of 1: (0.1 to 0.2): (1.4 to 1.6): (20 to 30), stirred at 200 to 300 r / min at 0°C for 25 to 35 minutes, the initiator solution is dripped in 30 minutes, stirring is continued for 20 to 24 hours, and the filter residue is washed 3 to 5 times with anhydrous ethanol and deionized water, respectively, and vacuum dried at 70 to 80°C for 4 to 6 hours to prepare modified lignin. The remaining steps are the same as in Example 2.
[0051] Test Example 1:
[0052] Anti-static performance test:
[0053] Moisture regain test method: Moisture regain tests were conducted on the examples and comparative examples in accordance with GB / T6503-2017 "Test method for moisture regain of chemical fibers." The results are shown in Table 1.
[0054] Conductivity Test Method: Resistivity was tested using an ST2253 digital four-probe tester manufactured by Suzhou Jingge Electronics Co., Ltd. The fabric was crushed into a powder, passed through a 100-mesh sieve, and pressed into a thin sheet under 50 kg pressure. The results are shown in Table 1.
[0055] Table 1
[0056] Moisture regain Resistivity (kΩ·cm) Moisture regain Resistivity (kΩ·cm) Example 1 7.81% 42.2 Comparative Example 1 5.94% 42.3 Example 2 7.87% 41.9 Comparative Example 2 7.69% 69.1 Example 3 7.79% 42.6 Comparative Example 3 6.83% 42.5
[0057] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 1, it can be found that the medical antibacterial and antistatic modified polyester cotton fabric prepared by the present invention has good antistatic performance.
[0058] Comparative Example 1 differs from Example 2 in that no antibacterial flame-retardant monomer is added. By comparison, the moisture regains of Examples 1 to 3 are greater than that of Comparative Example 1, indicating that the antibacterial flame-retardant monomer is produced by the reaction of methyldiethanolamine and diethyl chloromethyl phosphate, and the tertiary amine on the methyldiethanolamine reacts with the chloromethyl group on the diethyl chloromethyl phosphate to form a quaternary ammonium salt. The quaternary ammonium salt has good hydrophilicity, thereby improving the antibacterial properties of the medical antibacterial and antistatic modified polyester cotton fabric. Comparative Example 3 differs from Example 2 in that no lignin-modified salicylic acid is added. By comparison, the moisture regains of Examples 1 to 3 are greater than that of Comparative Example 3, indicating that pretreated lignin is produced by the reaction of lignin and p-aminophenol, and the amino group on the p-aminophenol reacts with the aldehyde group on the lignin to form a Schiff base structure with good hydrophilicity, thereby improving the antibacterial properties of the medical antibacterial and antistatic modified polyester cotton fabric.
[0059] The difference between Comparative Example 2 and Example 2 is that polyaniline is not added. By comparison, the resistivity of Examples 1 to 3 is greater than that of Comparative Example 1, indicating that polyaniline is formed by polymerization on lignin-modified salicylic acid, and polyaniline has good conductive properties, thereby improving the antistatic properties of the medical antibacterial and antistatic modified polyester cotton fabric.
[0060] Test Example 2:
[0061] Flame retardant performance test:
[0062] Test method: The examples and comparative examples were melted at 180°C to prepare standard bars according to GB / T 2406.2, and the limiting oxygen index of the standard bars was tested. The results are shown in Table 2.
[0063] Table 2
[0064] Limiting oxygen index (%) Limiting oxygen index (%) Example 1 32.8 Comparative Example 1 27.2 Example 2 32.7 Comparative Example 2 32.5 Example 3 33.1 Comparative Example 3 32.9
[0065] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 2, it can be found that the medical antibacterial and antistatic modified polyester cotton fabric prepared by the present invention has good flame retardant properties.
[0066] The difference between Comparative Example 1 and Example 2 is that no antibacterial flame retardant monomer is added. By comparison, the limiting oxygen index of Examples 1 to 3 is greater than the limiting oxygen index of Comparative Example 1, indicating that a large amount of phosphorus is introduced into the antibacterial flame retardant monomer prepared by the reaction of methyldiethanolamine and diethyl chloromethyl phosphate. Phosphorus has a good effect of promoting carbonization, which effectively improves the flame retardant properties of the medical antibacterial and antistatic modified polyester cotton fabric.
[0067] Test Example 3:
[0068] Antibacterial performance test: The antibacterial rate of each example and comparative example against Staphylococcus aureus was tested using the Quine test method. The results are shown in Table 3.
[0069] Table 3
[0070]
[0071]
[0072] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 3, it can be found that the medical antibacterial and antistatic modified polyester cotton fabric prepared by the present invention has good antibacterial properties.
[0073] The difference between Comparative Example 1 and Example 2 is that no antibacterial flame retardant monomer is added. By comparison, the antibacterial rate of Examples 1 to 3 is significantly greater than that of Comparative Example 1, indicating that the antibacterial flame retardant monomer is prepared by the reaction of methyldiethanolamine and diethyl chloromethyl phosphate, and the tertiary amine on methyldiethanolamine reacts with the chloromethyl on diethyl chloromethyl phosphate to form a quaternary ammonium salt. The quaternary ammonium salt has good antibacterial properties as a cationic antibacterial structure, thereby improving the antibacterial properties of the medical antibacterial and antistatic modified polyester cotton fabric.
[0074] Test Example 4:
[0075] Mechanical Properties Test: Standard specimens were prepared by cutting the fabrics of each embodiment and each comparative example according to GB / T3923.1 standard, and the breaking strength was measured. The results are shown in Table 4.
[0076] Anti-aging performance test: A xenon lamp was used to simulate sunlight. The fabrics of each embodiment and test example were placed in a xenon lamp accelerated aging test chamber. The aging time was 360 hours. The experimental atmosphere was air, the temperature was 65°C, the light source was 25 cm away from the sample, and the radiation intensity was 550W / m 2 Measure the breaking strength again. Calculate the performance retention rate = breaking strength after aging / initial breaking strength * 100%. See Table 4 for the results.
[0077] Table 4
[0078]
[0079]
[0080] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 4, it can be found that the medical antibacterial and antistatic modified polyester cotton fabric prepared by the present invention has good mechanical properties and light aging resistance.
[0081] By comparison, the breaking strength of Examples 1 to 3 is significantly greater than that of Comparative Example 1, indicating that the antibacterial flame retardant monomer is prepared by the reaction of methyldiethanolamine and diethyl chloromethyl phosphate, and the tertiary amine on the methyldiethanolamine reacts with the chloromethyl on the diethyl chloromethyl phosphate to form a quaternary ammonium salt. The quaternary ammonium salt, as a cation, can form an electrostatic bond with the carboxyl group on the modified lignin, effectively improving the mechanical properties of the antibacterial and antistatic modified polyester cotton fabric; the breaking strength of Examples 1 to 3 is significantly greater than that of Comparative Example 2, indicating that the p-aminosalicylic acid added during the polymerization of polyaniline introduces a carboxyl group, which forms an electrostatic bond with the quaternary ammonium salt cation on the antibacterial flame retardant monomer, effectively improving the mechanical properties of the antibacterial and antistatic modified polyester cotton fabric.
[0082] The difference between Comparative Example 3 and Example 2 is that no pre-modified lignin is added. By comparison, the performance retention rate of Examples 1 to 3 is significantly greater than that of Comparative Example 3, indicating that the pre-modified lignin introduces a salicylate structure into the fabric. Under ultraviolet light, the ester bond on the salicylate undergoes a photolysis reaction to generate free radicals, which are rearranged to form a 2-hydroxybenzophenone structure with ultraviolet absorption effect, effectively improving the anti-aging properties of the antibacterial and antistatic modified polyester cotton fabric.
[0083] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A medical antibacterial and antistatic modified polyester cotton fabric, characterized in that: The medical antibacterial and antistatic modified polyester cotton fabric is prepared by extruding modified polyester and modified lignin through an extruder and then spinning and weaving the resulting fabric. The modified polyester is prepared by reacting methyldiethanolamine and diethyl chloromethyl phosphate to obtain an antibacterial flame retardant monomer; and reacting terephthalic acid, ethylene glycol and an antibacterial flame retardant monomer. The modified lignin is prepared by reacting pretreated lignin and p-aminosalicylic acid to obtain pre-modified lignin; and reacting the pre-modified lignin, aniline and p-aminosalicylic acid to obtain the modified lignin.
2. A method for preparing a medical antibacterial and antistatic modified polyester cotton fabric, characterized in that: The method comprises the following preparation steps: (1) Pretreated lignin, para-aminosalicylic acid, and 0.1 mol / L sulfuric acid solution were mixed in a mass ratio of 1:(2-4):(1-1.2), stirred at 80-90°C and 600-800 r / min for 4-6 hours, filtered, and the filter residue was washed with deionized water for 3-5 times to obtain pre-modified lignin; (2) Mixing 2.4 to 2.6 times the mass of aniline with ammonium persulfate, 1.4 to 1.6 times the mass of aniline with a mass concentration of 98% concentrated sulfuric acid, and 10 to 20 times the mass of aniline with deionized water to prepare an initiator solution; mixing aniline, pre-modified lignin, para-aminosalicylic acid, 98% concentrated sulfuric acid, and deionized water, stirring at 200 to 300 r / min at 0°C for 25 to 35 minutes, dripping the initiator solution within 30 minutes, continuing stirring for 20 to 24 hours, filtering, washing the filter residue with anhydrous ethanol and deionized water for 3 to 5 times, respectively, and vacuum drying at 70 to 80°C for 4 to 6 hours to prepare modified lignin; (3) Terephthalic acid, ethylene glycol, antibacterial flame retardant monomer, and ethylene glycol antimony are reacted to obtain modified polyester; the modified polyester and modified lignin are mixed in a mass ratio of 1: (0.2-0.4), melt-extruded and spun through a twin-screw extruder, left to stand for 2-4 hours, and spun on a spinning machine and then cooled to room temperature through a side-blown air tunnel to obtain polyester fiber; the polyester fiber and cotton fiber are blended to obtain blended yarn, and the blended yarn is warped on a warping machine and then woven into a plain fabric using a fully automatic rapier loom, with a warp density of 600 threads / 10 cm and a weft density of 500 threads / 10 cm, to obtain a medical antibacterial and antistatic modified polyester cotton fabric.
3. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: The preparation method of the pretreated lignin in step (1) is as follows: lignin, p-aminophenol and anhydrous ethanol are mixed in a mass ratio of 1: (2-4): (10-20), stirred at 80-90°C and 200-300 r / min for 2-4 hours, filtered, and the filter residue is washed with anhydrous ethanol for 3-5 times, and vacuum dried at 60-70°C for 4-6 hours to obtain the product.
4. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: In step (2), the mass ratio of the aniline, pre-modified lignin, p-aminosalicylic acid, concentrated sulfuric acid with a mass concentration of 98%, and deionized water is 1: (0.2-0.3): (0.1-0.2): (1.4-1.6): (20-30).
5. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: The preparation method of the antibacterial flame retardant monomer in step (3) is as follows: methyldiethanolamine, diethyl chloromethyl phosphate and anhydrous ethanol are mixed in a mass ratio of 1: (1.4-1.6): (15-25), stirred at 400-600 r / min at 80-90° C. for 20-24 h, and rotary evaporated at 55-65° C. for 20-30 min.
6. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: The preparation method of the modified polyester in step (3) is as follows: terephthalic acid, ethylene glycol, and antibacterial flame retardant monomer are added to a reactor in a molar ratio of 1:0.6:0.4, nitrogen is introduced, ethylene glycol antimony (0.0003 to 0.0007 times the mass of terephthalic acid) is added, stirring at a speed of 200 to 400 r / min at 180 to 200° C. for 1 to 2 hours, heating to 195 to 205° C. and continuing the reaction, when esterification water no longer distills out, adjusting the pressure to 90 to 110 Pa within 30 minutes, heating to 225 to 235° C., adjusting the speed to 50 to 70 r / min, and stirring until the reaction terminates, introducing nitrogen to restore the pressure to normal pressure, cooling to room temperature, and discharging to obtain the product.
7. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: The temperature of the twin-screw extruder in step (3) is: zone 1 temperature 260-270°C, zone 2 temperature 265-275°C, zone 3 temperature 270-280°C, zone 4 temperature 270-280°C, and die head temperature 260-270°C.
8. The method for preparing a medical antibacterial and antistatic modified polyester cotton fabric according to claim 2, characterized in that: The process parameters of the spinning machine in step (3) are: spinning box temperature 275-285°C, spinneret aperture 0.24 mm, spinneret aperture aspect ratio 2, and winding speed 3000 m / min.
Citation Information
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CN121046981A