Preparation method of an anion antibacterial modified colored DTY low elastic yarn

Abstract

The present invention belongs to the technical field of chemical fibers, and particularly relates to a preparation method of an anion antibacterial modified colored DTY low elastic yarn, which includes: performing high-temperature pre-crystallization on polyethylene terephthalate chips, then drying them, and obtaining pre-crystallized polyethylene terephthalate fine powder after ball milling; adding modified anion fine powder, color masterbatch and strengthening filler to the pre-crystallized polyethylene terephthalate fine powder, mixing them evenly, and then adding them into a twin-screw extruder for melt extrusion to obtain a mixed melt; adding the mixed melt into a spinning box, and uniformly cooling it with ring blowing to form POY, and obtaining the anion antibacterial modified colored DTY low elastic yarn after texturing treatment. The present invention solves the problem of poor antibacterial stability of existing polyester low elastic yarns, forms an anion release system by using bamboo charcoal particles, and cooperates with the formation of a silicon-oxygen mesoporous release channel and barrier property on the surface of the bamboo charcoal particles to ensure the antibacterial property and stability of the polyester low elastic yarn.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical fibers, and particularly relates to a method for preparing an anion antibacterial modified colored DTY low elastic yarn. Background Art

[0002] Polyester low elastic yarn, also known as DTY, is a type of deformed yarn of polyester chemical fiber. It is made from polyester chips (PET) as raw materials through high-speed spinning, drawing and false twisting processes. It has the advantages of high breaking strength, good resilience, heat resistance, light resistance, and corrosion resistance of polyester materials, and is widely used in fields such as clothing fabrics, bedding, and decorative items.

[0003] With the improvement of people's living standards, the quality requirements for fabrics are getting higher and higher. Among them, antibacterial properties have gradually become a conventional property of polyester low elastic yarn. The antibacterial properties of existing polyester low elastic yarns are obtained by coating the surface with antibacterial agents after the formation of the yarn. However, this antibacterial property only exists on the surface of the polyester low elastic yarn, with poor persistence and easy breakage. Summary of the Invention

[0004] Aiming at the problems in the prior art, the present invention provides a method for preparing an anion antibacterial modified colored DTY low elastic yarn, which solves the problem of poor antibacterial stability of existing polyester low elastic yarns. By using bamboo charcoal particles to form an anion release system, combined with the formation of a silicon oxide mesoporous release channel and barrier properties on the surface of the bamboo charcoal particles, the antibacterial property and stability of the polyester low elastic yarn are ensured.

[0005] To achieve the above technical objectives, the technical solution of the present invention is as follows:

[0006] A method for preparing an anion antibacterial modified colored DTY low elastic yarn, comprising the following steps:

[0007] Step 1, subject the polyethylene terephthalate chips to high-temperature pre-crystallization, then drying treatment, and obtain pre-crystallized polyethylene terephthalate fine powder after ball milling treatment. The temperature of the high-temperature pre-crystallization is 170 - 175 °C, the temperature of the drying treatment is 180 - 185 °C, and the time is 5 - 7 h; the pressure of the ball milling treatment is 0.4 - 0.6 MPa, and the temperature is 5 - 10 °C; this step uses high-temperature pre-crystallization to convert the polyethylene terephthalate chips into spherical crystals and forms a fine powder structure after ball milling treatment;

[0008] Step 2, add the modified negative ion fine powder, masterbatch and reinforcing filler into the pre-crystallized polyethylene terephthalate fine powder and mix evenly, then add them into a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is: 180-200 parts of pre-crystallized polyethylene terephthalate fine powder, 8-10 parts of modified negative ion fine powder, 3-5 parts of masterbatch, and 5-10 parts of reinforcing filler; the modified negative ion fine powder uses modified bamboo charcoal particles, the masterbatch uses one or several of magenta masterbatch, cyan masterbatch and yellow masterbatch, and the reinforcing filler uses porous silicon oxygen filler; the temperature of the melt extrusion is 280-290 °C and the pressure is 7-8 MPa; in this step, the modified negative ion fine powder, masterbatch, reinforcing filler and pre-crystallized polyethylene terephthalate fine powder are blended to achieve sufficient mixing, and during the melt extrusion process, the modified negative ion fine powder, masterbatch and reinforcing filler are promoted to be fully dispersed in the pre-crystallized polyethylene terephthalate fine powder to obtain a mixed melt;

[0009] Step 3, add the mixed melt into the spinning box and cool it evenly with ring blowing to obtain POY-, and then obtain the negative ion antibacterial modified colored DTY low elastic yarn through texturing treatment. The temperature of the spinning is 285-295 °C, the temperature of the ring blowing is 22-25 °C, the wind speed is 0.5-0.7 m / s, and the humidity is 65-85%; the texturing treatment is to pass the spun yarn through a pre-network nozzle, a wire guide, a first roller, a false twister, a second roller, a final network, a third roller and a winding roller in sequence, thereby obtaining the polyester low elastic yarn.

[0010] Among them, the modified bamboo charcoal particles use silicon oxygen-coated bamboo charcoal particles, and there are gaps between the bamboo charcoal particles and the silicon oxygen coating layer. The bamboo charcoal particles have a loose and porous structure, which not only has good and super adsorption capacity, but also can generate negative ions to achieve the effect of preventing mildew and bacteria; however, the bamboo charcoal particles also have the problem of moisture absorption and humidity adjustment, which will not only affect the moisture absorption of the polyester low elastic yarn, but also affect the antibacterial effect. To solve this problem, the silicon oxygen-coated bamboo charcoal particles use the silicon oxygen coating layer to coat the bamboo charcoal particles to achieve a good barrier effect, and at the same time do not affect the release of negative ions.

[0011] The preparation method of the silicon oxygen-coated bamboo charcoal particles includes the following steps: a1, wet grind the bamboo charcoal particles for 2-4 h, and evaporate to obtain bamboo charcoal fine powder; the wet grinding uses ether as a solvent, and the mass ratio of the bamboo charcoal particles to ether is 3-5:1, and the grinding pressure is 0.3-0.5 MPa; the evaporation temperature is 40-50 °C; this step uses the wet grinding method to refine the bamboo charcoal particles, and at the same time uses ether as a buffer to quickly absorb heat and reduce the influence of friction temperature.

[0012] a2. Put ethyl cellulose into ether to form a solution, and add fine bamboo charcoal powder. After ultrasonic treatment for 1 - 2 h, filter and dry to obtain coated bamboo charcoal particles. The concentration of ethyl cellulose in ether is 20 - 30 g / L, the concentration of fine bamboo charcoal powder in the solution is 10 - 15 g / L, the ultrasonic frequency of ultrasonic treatment is 60 - 80 kHz, the temperature is 5 - 10 °C, and the drying temperature is 40 - 50 °C. This step utilizes the solubility of ethyl cellulose in ether to form a low-concentration dispersion liquid, and coats the surface of fine bamboo charcoal powder. When filtering, an ethyl cellulose-ether liquid film is formed on the surface of fine bamboo charcoal powder, and ether is removed during drying, thereby ensuring that an ethyl cellulose liquid film is deposited on the surface of fine bamboo charcoal powder.

[0013] a3. Blend methyltrichlorosilane with ether to form a dilution liquid, and then spray it on the surface of coated bamboo charcoal particles to form a liquid film. After drying, standing, and heating and standing, prefabricated modified bamboo charcoal particles are obtained. The volume ratio of methyltrichlorosilane to ether is 1:3 - 5, the spraying speed is 3 - 5 mL / min, the spraying time is 2 - 4 s, the drying temperature is 40 - 45 °C, the standing atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10 - 12:1, and the heating and standing temperature is 80 - 100 °C. This step utilizes the compatibility of methyltrichlorosilane and ether to dilute methyltrichlorosilane, and then sprays it on the surface of coated bamboo charcoal particles to form a liquid film. Ether is removed during drying to form a methyltrichlorosilane surface film, which in-situ hydrolyzes with water vapor to form methyltrihydroxysilane, and methyltrihydroxysilane undergoes a polycondensation reaction during heating and standing to obtain a silicon-oxygen polycondensation layer containing methyl.

[0014] a4. Irradiate the prefabricated modified bamboo charcoal particles with ultraviolet light for 2 - 3 h, and then purge with nitrogen to obtain modified bamboo charcoal particles. The power of ultraviolet light irradiation is 200 - 300 W, the nitrogen temperature for nitrogen purging is 80 - 100 °C, and the speed is 10 - 20 mL / min. This step utilizes ultraviolet light irradiation to degrade ethyl cellulose, and the light transmittance of the silicon-oxygen polycondensation layer ensures the complete removal of ethyl cellulose and also ensures the exposure of the surface of fine bamboo charcoal powder.

[0015] The surface of the modified bamboo charcoal particles prepared by this method contains a silicon-oxygen condensation layer, which contains methyl groups, improving the surface unevenness and having good stability in physical fixation. At the same time, the silicon-oxygen condensation layer contains reactive silicon hydroxyl groups, showing a certain electronegativity, which is the same as the electrical property on the surface of most bacteria. Therefore, the silicon-oxygen condensation layer can achieve a good antibacterial effect; the silicon-oxygen condensation layer has a self-owned silicon-oxygen mesoporous structure, providing a negative ion release channel for the bamboo charcoal particles, and the silicon-oxygen mesoporous structure can play a water-blocking effect, ensuring the internal stability and long-term effectiveness; the negative ions released by the bamboo charcoal particles have the same electrical property as that of the silicon hydroxyl groups, showing a certain repulsion, ensuring the outward release of negative ions without accumulation. Therefore, the modified bamboo charcoal particles not only have physical and chemical connection stability on the surface, but also form an antibacterial and sterilization effect by using the negative ions of the bamboo charcoal particles and the electronegativity of silicon-oxygen.

[0016] Among them, the reinforcing filler uses a porous silicon-oxygen filler, which forms structural gaps by using its own porous structure, ensuring the penetration of polyethylene terephthalate and achieving the effect of physical clamping, greatly improving the physical stability. Moreover, the porous silicon-oxygen filler has a self-owned silicon-oxygen stable structure and transparency, not only improving the mechanical stability and wear resistance of the DTY drawn textured yarn, but also being able to form good color transferability and ensuring the color stability of the DTY drawn textured yarn.

[0017] The preparation method of the porous silicon-oxygen filler includes the following steps: b1, adding dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane into ether and stirring evenly to form a mixed solution, and then adding ethyl cellulose and performing ultrasonic treatment for 20 - 30 min to obtain a mixed dispersion. The molar ratio of dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane is 1:1 - 2:2 - 4. The concentration of dodecyltrimethoxysilane in ether is 40 - 80 g / L, the stirring speed is 300 - 500 r / min, the concentration of ethyl cellulose in ether is 70 - 100 g / L, the temperature of the ultrasonic treatment is 5 - 10 °C, and the ultrasonic frequency is 80 - 100 kHz; this step utilizes the good solubility of ethyl cellulose, dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane in ether, and can be homogenously dispersed under the action of ultrasonic waves.

[0018] b2. Spray the mixed dispersion liquid into the reaction kettle. After deposition and purging, hydrolyzed particles are obtained. The spraying speed is 5 - 10 L / min. The atmosphere in the reaction kettle is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 8 - 10:1, and the temperature is 40 - 50 °C. The deposition temperature is 100 - 110 °C. The purging uses dry nitrogen at 80 - 90 °C, and the purging speed is 5 - 10 mL / min. In this step, the droplets are dispersed into the reaction kettle by spraying, and composite particles are formed during the evaporation of ether. And the atmosphere contains water vapor to ensure the in-situ hydrolysis of dodecyltrimethoxysilane, cetyltrimethoxysilane, and butyltriethoxysilane. After deposition treatment, the hydrolysis products will undergo a polycondensation reaction to obtain silicon-oxygen composite particles containing long and short chains.

[0019] b3. Put the hydrolyzed particles into ethanol and perform ultrasonic treatment for 1 - 2 h. After filtration, wash 1 - 3 times, and obtain porous silicon-oxygen filler by spray drying. The concentration of the hydrolyzed particles in ethanol is 100 - 300 g / L. The temperature of ultrasonic treatment is 30 - 40 °C, and the frequency is 70 - 90 kHz. The washing uses ethanol, and the temperature of spray drying is 100 - 120 °C. The porous silicon-oxygen filler prepared by this method not only contains the porous structure formed by ethyl cellulose to form pores, but also has mesopores formed by the condensation of silicon hydroxyl groups. At the same time, the porous structure of the porous silicon-oxygen filler contains active silicon hydroxyl groups, forming an antibacterial effect of an electronegative system, and also has a long-chain - short-chain fixed structure located outside the porous structure.

[0020] As can be seen from the above description, the present invention has the following advantages:

[0021] 1. The present invention solves the problem of poor antibacterial stability of existing polyester drawn textured yarn. By using bamboo charcoal particles to form a negative ion release system, combined with the formation of a silicon-oxygen mesoporous release channel and barrier on the surface of bamboo charcoal particles, the antibacterial property and stability of polyester drawn textured yarn are ensured.

[0022] 2. The present invention uses porous silicon-oxygen filler as a reinforcing filler, which not only forms a physical permeable fixing effect, but also ensures the color transfer of the masterbatch by using the transparency of the silicon-oxygen material.

[0023] 3. The present invention uses silicon-oxygen to wrap bamboo charcoal particles and porous silicon-oxygen filler as a dopant to form the mechanical property enhancement of the silicon-oxygen material. At the same time, the silicon hydroxyl groups brought by the silicon-oxygen material can form a fixation with the hydrophilic groups in polyethylene terephthalate, ensuring the stability of polyester drawn textured yarn. Specific Embodiments

[0024] The present invention will be described in detail in combination with embodiments, but no limitation is made to the claims of the present invention. Example 1

[0025] A preparation method of an anion antibacterial modified colored DTY low elastic yarn, comprising the following steps:

[0026] Step 1, subject the polyethylene terephthalate chips to high-temperature pre-crystallization, then drying treatment, and obtain pre-crystallized polyethylene terephthalate fine powder after ball milling treatment. The temperature of the high-temperature pre-crystallization is 170 °C, the temperature of the drying treatment is 180 °C, and the time is 5 h; the pressure of the ball milling treatment is 0.4 MPa, and the temperature is 5 °C;

[0027] Step 2, add the modified anion fine powder, color masterbatch and reinforcing filler into the pre-crystallized polyethylene terephthalate fine powder and mix evenly, then add them into a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is: 180 parts of pre-crystallized polyethylene terephthalate fine powder, 8 parts of modified anion fine powder, 3 parts of color masterbatch, and 5 parts of reinforcing filler; the modified anion fine powder uses modified bamboo charcoal particles, the color masterbatch uses magenta masterbatch, and the reinforcing filler uses porous silicon oxygen filler; the temperature of the melt extrusion is 280 °C, and the pressure is 7 MPa;

[0028] Step 3, add the mixed melt into the spinning box, and evenly cool it into POY with ring blowing, and obtain the anion antibacterial modified colored DTY low elastic yarn after texturing treatment. The temperature of the spinning is 285 °C, the temperature of the ring blowing is 22 °C, the wind speed is 0.5 m / s, and the humidity is 65%; the texturing treatment is to pass the spun yarn through a pre-network nozzle, a wire guide, a first roller, a false twister, a second roller, a final network, a third roller and a winding roller in sequence, so as to obtain the polyester low elastic yarn.

[0029] Among them, the modified bamboo charcoal particles are bamboo charcoal particles wrapped with silicon oxide, and there are gaps between the bamboo charcoal particles and the silicon oxide coating layer. The preparation method of the silicon oxide-coated bamboo charcoal particles includes the following steps: a1, wet-grind the bamboo charcoal particles for 2 h, and obtain bamboo charcoal fine powder after evaporation; the wet-grinding uses ether as a solvent, and the mass ratio of the bamboo charcoal particles to ether is 3:1, and the grinding pressure is 0.3 MPa; the evaporation temperature is 40 °C; a2, put ethyl cellulose into ether to form a solution, and put the bamboo charcoal fine powder into it. After ultrasonic treatment for 1 h, filter and dry to obtain coated bamboo charcoal particles. The concentration of ethyl cellulose in ether is 20 g / L, the concentration of the bamboo charcoal fine powder in the solution is 10 g / L, the ultrasonic frequency of the ultrasonic treatment is 60 kHz, the temperature is 5 °C, and the drying temperature is 40 °C; a3, blend methyltrichlorosilane and ether to form a dilution solution, and then spray it on the surface of the coated bamboo charcoal particles to form a liquid film. After drying, standing and heating and standing, obtain prefabricated modified bamboo charcoal particles. The volume ratio of methyltrichlorosilane to ether is 1:3, the spraying speed is 3 mL / min, the spraying time is 2 s, the drying temperature is 40 °C, the standing atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10:1, and the heating and standing temperature is 80 °C; a4, irradiate the prefabricated modified bamboo charcoal particles with ultraviolet light for 2 h, and then purge with nitrogen to obtain modified bamboo charcoal particles. The power of the ultraviolet light treatment is 200 W, the nitrogen temperature of the nitrogen purge is 80 °C, and the speed is 10 mL / min.

[0030] Among them, the reinforcing filler uses porous silicon oxide filler, and the preparation method of the porous silicon oxide filler includes the following steps: b1, adding dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane into diethyl ether and stirring evenly to form a mixed solution, then adding ethyl cellulose and performing ultrasonic treatment for 20 min to obtain a mixed dispersion. The molar ratio of dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane is 1:1:2. The concentration of dodecyltrimethoxysilane in diethyl ether is 40 g / L, the stirring speed is 300 r / min, the concentration of ethyl cellulose in diethyl ether is 70 g / L, the temperature of the ultrasonic treatment is 5 °C, and the ultrasonic frequency is 80 kHz; b2, spraying the mixed dispersion into a reaction kettle, and obtaining hydrolyzed particles through deposition and purging. The spraying speed is 5 L / min, the atmosphere in the reaction kettle is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 8:1, and the temperature is 40 °C; the deposition temperature is 100 °C, the purging uses dry nitrogen at 80 °C, and the purging speed is 5 mL / min; b3, putting the hydrolyzed particles into ethanol and performing ultrasonic treatment for 1 h, filtering and washing once, and obtaining the porous silicon oxide filler through spray drying. The concentration of the hydrolyzed particles in ethanol is 100 g / L, the temperature of the ultrasonic treatment is 30 °C, the frequency is 70 kHz, the washing uses ethanol, and the temperature of the spray drying is 100 °C. Example 2

[0031] A preparation method of an anion antibacterial modified colored DTY low elastic yarn includes the following steps:

[0032] Step 1, performing high-temperature pre-crystallization on polyethylene terephthalate chips, then performing drying treatment, and obtaining pre-crystallized polyethylene terephthalate fine powder through ball milling treatment. The temperature of the high-temperature pre-crystallization is 175 °C, the temperature of the drying treatment is 185 °C, and the time is 7 h; the pressure of the ball milling treatment is 0.6 MPa, and the temperature is 10 °C;

[0033] Step 2, adding modified anion fine powder, color masterbatch and reinforcing filler into the pre-crystallized polyethylene terephthalate fine powder and mixing evenly, then adding them into a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is: 200 parts of pre-crystallized polyethylene terephthalate fine powder, 10 parts of modified anion fine powder, 5 parts of color masterbatch, and 10 parts of reinforcing filler; the modified anion fine powder uses modified bamboo charcoal particles, the color masterbatch uses a cyan color masterbatch, and the reinforcing filler uses porous silicon oxide filler; the temperature of the melt extrusion is 290 °C, and the pressure is 8 MPa;

[0034] Step 3: Add the mixed melt into the spinning box and evenly cool it into POY with ring blowing, and obtain negatively charged antibacterial modified colored DTY low elastic yarn through texturing treatment. The spinning temperature is 295°C, the temperature of the ring blowing is 25°C, the wind speed is 0.7 m / s, and the humidity is 85%; the texturing treatment is to pass the spun yarn through a pre-network nozzle, a wire guide, a first roller, a false twister, a second roller, a final network, a third roller, and a winding roller in sequence to obtain polyester low elastic yarn.

[0035] Among them, the modified bamboo charcoal particles are bamboo charcoal particles wrapped with silicon oxide, and there are gaps between the bamboo charcoal particles and the silicon oxide coating layer. The preparation method of the silicon oxide-coated bamboo charcoal particles includes the following steps: a1, wet grind the bamboo charcoal particles for 4 h and obtain bamboo charcoal fine powder after evaporation; the wet grinding uses ether as the solvent, and the mass ratio of the bamboo charcoal particles to ether is 5:1, and the grinding pressure is 0.5 MPa; the evaporation temperature is 50°C; a2, put ethyl cellulose into ether to form a solution, and put the bamboo charcoal fine powder into it. After ultrasonic treatment for 2 h, filter and dry to obtain coated bamboo charcoal particles. The concentration of ethyl cellulose in ether is 30 g / L, the concentration of the bamboo charcoal fine powder in the solution is 15 g / L, the ultrasonic frequency of the ultrasonic treatment is 80 kHz, the temperature is 10°C, and the drying temperature is 50°C; a3, blend methyltrichlorosilane and ether to form a dilution solution, and then spray it on the surface of the coated bamboo charcoal particles to form a liquid film. After drying, standing, and heating and standing, obtain prefabricated modified bamboo charcoal particles. The volume ratio of methyltrichlorosilane to ether is 1:5, the spraying speed is 5 mL / min, the spraying time is 4 s, the drying temperature is 45°C, the standing atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 12:1, and the heating and standing temperature is 100°C; a4, irradiate the prefabricated modified bamboo charcoal particles with ultraviolet light for 3 h, and then purge with nitrogen to obtain modified bamboo charcoal particles. The power of the ultraviolet light irradiation treatment is 300 W, the nitrogen temperature of the nitrogen purge is 100°C, and the speed is 20 mL / min.

[0036] Among them, the reinforcing filler uses porous silicon oxide filler, and the preparation method of the porous silicon oxide filler includes the following steps: b1, adding dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane into ether and stirring evenly to form a mixed solution, then adding ethyl cellulose and performing ultrasonic treatment for 30 min to obtain a mixed dispersion. The molar ratio of dodecyltrimethoxysilane, cetyltrimethoxysilane and butyltriethoxysilane is 1:2:4. The concentration of dodecyltrimethoxysilane in ether is 80 g / L, the stirring speed is 500 r / min, the concentration of ethyl cellulose in ether is 100 g / L, the temperature of the ultrasonic treatment is 10°C, and the ultrasonic frequency is 100 kHz; b2, spraying the mixed dispersion into a reaction kettle, and obtaining hydrolyzed particles through deposition and purging. The spraying speed is 10 L / min. The atmosphere in the reaction kettle is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10:1, and the temperature is 50°C; the deposition temperature is 110°C, the purging uses dry nitrogen at 90°C, and the purging speed is 10 mL / min; b3, putting the hydrolyzed particles into ethanol and performing ultrasonic treatment for 2 h, filtering and washing 3 times, and obtaining the porous silicon oxide filler through spray drying. The concentration of the hydrolyzed particles in ethanol is 300 g / L, the temperature of the ultrasonic treatment is 40°C, the frequency is 90 kHz, the washing uses ethanol, and the temperature of the spray drying is 120°C. Example 3

[0037] A preparation method of an anion antibacterial modified colored DTY low elastic yarn includes the following steps:

[0038] Step 1, performing high-temperature pre-crystallization on polyethylene terephthalate chips, then drying, and obtaining pre-crystallized polyethylene terephthalate fine powder through ball milling. The temperature of the high-temperature pre-crystallization is 175°C, the temperature of the drying is 185°C, and the time is 6 h; the pressure of the ball milling is 0.5 MPa, and the temperature is 8°C;

[0039] Step 2, adding modified anion fine powder, color masterbatch and reinforcing filler into the pre-crystallized polyethylene terephthalate fine powder and mixing evenly, then adding them into a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is: 190 parts of pre-crystallized polyethylene terephthalate fine powder, 9 parts of modified anion fine powder, 4 parts of color masterbatch, and 8 parts of reinforcing filler; the modified anion fine powder uses modified bamboo charcoal particles, the color masterbatch uses yellow color masterbatch, and the reinforcing filler uses porous silicon oxide filler; the temperature of the melt extrusion is 285°C, and the pressure is 8 MPa;

[0040] Step 3: Add the mixed melt into the spinning box and evenly cool it into POY with ring blowing, and obtain negatively charged antibacterial modified colored DTY low elastic yarn through texturing treatment. The spinning temperature is 290°C, the temperature of the ring blowing is 24°C, the wind speed is 0.6 m / s, and the humidity is 80%. The texturing treatment is to pass the spun yarn through a pre-network nozzle, a wire guide, a first roller, a false twister, a second roller, a final network, a third roller, and a winding roller in sequence, thereby obtaining polyester low elastic yarn.

[0041] Among them, the modified bamboo charcoal particles are bamboo charcoal particles wrapped with silicon oxide, and there are gaps between the bamboo charcoal particles and the silicon oxide coating layer. The preparation method of the silicon oxide-coated bamboo charcoal particles includes the following steps: a1, wet grind the bamboo charcoal particles for 3 h and obtain bamboo charcoal fine powder after evaporation. The wet grinding uses ether as the solvent, and the mass ratio of the bamboo charcoal particles to ether is 4:1, and the grinding pressure is 0.4 MPa. The evaporation temperature is 45°C; a2, put ethyl cellulose into ether to form a solution, and put the bamboo charcoal fine powder into it. After ultrasonic treatment for 2 h, filter and dry to obtain coated bamboo charcoal particles. The concentration of ethyl cellulose in ether is 25 g / L, the concentration of the bamboo charcoal fine powder in the solution is 13 g / L, the ultrasonic frequency of the ultrasonic treatment is 70 kHz, the temperature is 8°C, and the drying temperature is 45°C; a3, blend methyltrichlorosilane and ether to form a dilution solution, and then spray it on the surface of the coated bamboo charcoal particles to form a liquid film. After drying, standing, and heating and standing, obtain prefabricated modified bamboo charcoal particles. The volume ratio of methyltrichlorosilane to ether is 1:4, the spraying speed is 4 mL / min, the spraying time is 3 s, the drying temperature is 43°C, the standing atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 11:1, and the heating and standing temperature is 90°C; a4, subject the prefabricated modified bamboo charcoal particles to ultraviolet light treatment for 3 h, and then purge with nitrogen to obtain modified bamboo charcoal particles. The power of the ultraviolet light treatment is 250 W, the nitrogen temperature of the nitrogen purge is 90°C, and the speed is 15 mL / min.

[0042] Among them, the reinforcing filler uses porous silicon oxide filler, and the preparation method of the porous silicon oxide filler includes the following steps: b1, adding dodecyltrimethoxysilane, cetyltrimethoxysilane, and butyltriethoxysilane into diethyl ether and stirring evenly to form a mixed solution, then adding ethyl cellulose and performing ultrasonic treatment for 25 min to obtain a mixed dispersion. The molar ratio of dodecyltrimethoxysilane, cetyltrimethoxysilane, and butyltriethoxysilane is 1:2:3. The concentration of dodecyltrimethoxysilane in diethyl ether is 60 g / L, the stirring speed is 400 r / min, the concentration of ethyl cellulose in diethyl ether is 80 g / L, the temperature of the ultrasonic treatment is 8 °C, and the ultrasonic frequency is 90 kHz; b2, spraying the mixed dispersion into a reaction kettle, obtaining hydrolyzed particles through deposition and purging. The spraying speed is 8 L / min, the atmosphere in the reaction kettle is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 9:1, and the temperature is 45 °C; the deposition temperature is 105 °C, the purging uses dry nitrogen at 85 °C, and the purging speed is 8 mL / min; b3, putting the hydrolyzed particles into ethanol and performing ultrasonic treatment for 2 h, filtering and washing twice, and obtaining the porous silicon oxide filler through spray drying. The concentration of the hydrolyzed particles in ethanol is 200 g / L, the temperature of the ultrasonic treatment is 35 °C, the frequency is 80 kHz, the washing uses ethanol, and the temperature of the spray drying is 110 °C. Example 4

[0043] A preparation method of a negative ion antibacterial modified colored DTY low elastic yarn includes the following steps:

[0044] Step 1, performing high-temperature pre-crystallization on polyethylene terephthalate chips, then performing drying treatment, and obtaining pre-crystallized polyethylene terephthalate fine powder through ball milling. The temperature of the high-temperature pre-crystallization is 175 °C, the temperature of the drying treatment is 185 °C, and the time is 6 h; the pressure of the ball milling treatment is 0.5 MPa, and the temperature is 8 °C;

[0045] Step 2, adding modified negative ion fine powder, color masterbatch, and reinforcing filler into the pre-crystallized polyethylene terephthalate fine powder and mixing evenly, then adding them into a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is: 190 parts of pre-crystallized polyethylene terephthalate fine powder, 9 parts of modified negative ion fine powder, 4 parts of color masterbatch, and 8 parts of reinforcing filler; the modified negative ion fine powder uses modified bamboo charcoal particles, the color masterbatch uses yellow color masterbatch, and the reinforcing filler uses silicon dioxide particles; the temperature of the melt extrusion is 285 °C, and the pressure is 8 MPa;

[0046] Step 3: Add the mixed melt into the spinning box and uniformly cool it into POY with ring blowing, and then obtain the anion antibacterial modified colored DTY low-elastic yarn through texturing treatment. The spinning temperature is 290°C, the temperature of the ring blowing is 24°C, the wind speed is 0.6 m / s, and the humidity is 80%. The texturing treatment is to pass the spun yarn through a pre-network nozzle, a wire guide, a first roller, a false twister, a second roller, a final network, a third roller, and a winding roller in sequence to obtain the polyester low-elastic yarn.

[0047] Among them, the modified bamboo charcoal particles are bamboo charcoal particles wrapped with silicon oxide, and there are gaps between the bamboo charcoal particles and the silicon oxide coating layer. The preparation method of the silicon oxide-coated bamboo charcoal particles includes the following steps: a1, wet grind the bamboo charcoal particles for 3 h and obtain bamboo charcoal fine powder after evaporation. The wet grinding uses ether as the solvent, and the mass ratio of the bamboo charcoal particles to ether is 4:1, and the grinding pressure is 0.4 MPa. The evaporation temperature is 45°C; a2, put ethyl cellulose into ether to form a solution, and put the bamboo charcoal fine powder into it. After ultrasonic treatment for 2 h, filter and dry to obtain coated bamboo charcoal particles. The concentration of ethyl cellulose in ether is 25 g / L, the concentration of the bamboo charcoal fine powder in the solution is 13 g / L, the ultrasonic frequency of the ultrasonic treatment is 70 kHz, the temperature is 8°C, and the drying temperature is 45°C; a3, blend methyltrichlorosilane and ether to form a dilution solution, and then spray it on the surface of the coated bamboo charcoal particles to form a liquid film. After drying, standing, and heating and standing, obtain the prefabricated modified bamboo charcoal particles. The volume ratio of methyltrichlorosilane to ether is 1:4, the spraying speed is 4 mL / min, the spraying time is 3 s, the drying temperature is 43°C, the standing atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 11:1. The temperature of the heating and standing is 90°C; a4, subject the prefabricated modified bamboo charcoal particles to ultraviolet light irradiation treatment for 3 h, and then purge with nitrogen to obtain the modified bamboo charcoal particles. The power of the ultraviolet light irradiation treatment is 250 W, the nitrogen temperature of the nitrogen purge is 90°C, and the speed is 15 mL / min. Example 5

[0048] A preparation method of an anion antibacterial modified colored DTY low-elastic yarn, comprising the following steps:

[0049] Step 1: High-temperature pre-crystallize the polyethylene terephthalate chips, then perform drying treatment, and obtain pre-crystallized polyethylene terephthalate fine powder after ball milling treatment. The high-temperature pre-crystallization temperature is 175°C, the drying treatment temperature is 185°C, and the time is 6 h. The pressure of the ball milling treatment is 0.5 MPa, and the temperature is 8°C;

[0050] Step 2: Add the anion fine powder, color masterbatch, and reinforcing filler to the pre-crystallized polyethylene terephthalate fine powder and mix evenly. Then add them to a twin-screw extruder for melt extrusion to obtain a mixed melt. The mass ratio of the mixed melt is as follows: 190 parts of pre-crystallized polyethylene terephthalate fine powder, 9 parts of anion fine powder, 4 parts of color masterbatch, and 8 parts of reinforcing filler. The anion fine powder uses bamboo charcoal particles, the color masterbatch uses a yellow color masterbatch, and the reinforcing filler uses silicon dioxide particles. The temperature of the melt extrusion is 285°C and the pressure is 8 MPa.

[0051] Step 3: Add the mixed melt into the spinning box and evenly cool it into POY with a ring blower. After texturing treatment, obtain the anion antibacterial modified colored DTY low-elasticity yarn. The temperature of the spinning is 290°C, the temperature of the ring blower is 24°C, the wind speed is 0.6 m / s, and the humidity is 80%. The texturing treatment is to pass the spun yarn through a pre-network nozzle, a yarn guide, a first roller, a false twister, a second roller, a final network, a third roller, and a winding roller in sequence, thereby obtaining the polyester low-elasticity yarn.

[0052] Comparative Example

[0053] The comparative example uses a commercially available antibacterial DTY low-elasticity yarn, selected from the antibacterial polyester low-elasticity yarn of a new material company in Zhejiang.

[0054] Performance Testing

[0055] Use the products of Examples 1-5 and the comparative example as test samples for performance testing, and the results are as follows:

[0056] 1. Weave the DTY low-elasticity yarn into a 10 cm * 10 cm fabric and conduct an antibacterial test on the fabric.

[0057] Table 1 Antibacterial Test

[0058]

[0059] After washing the above fabric 50 times, conduct antibacterial stability.

[0060] Table 2 Antibacterial Stability Test

[0061]

[0062] As can be seen from Tables 1-2, the colored DTY low-elasticity yarn of this technical solution has good antibacterial properties, and the antibacterial stability comes from the anion system. Compared with the commercially available polyester low-elasticity yarn of the comparative example, the technical solution still maintains good antibacterial effects after multiple washings. The main reason is that the silicon-oxygen shell protects the bamboo charcoal particles, preventing the infiltration of distilled water while not affecting the release of anions.

[0063] 2. Mechanical property test of DTY low-elasticity yarn

[0064] Table 3 Mechanical Property Test

[0065]

[0066] As can be seen from Table 3, the DTY drawn textured yarn prepared by this technical solution has good mechanical properties, which are relatively close to those of the commercially available antibacterial polyester drawn textured yarn, meeting the current market demand.

[0067] It can be understood that the above specific description of the present invention is only for illustrating the present invention and is not limited to the technical solutions described in the embodiments of the present invention. Those of ordinary skill in the art should understand that the present invention can still be modified or equivalently replaced to achieve the same technical effect; as long as it meets the usage requirements, it is within the protection scope of the present invention.

Claims

1. A method for preparing negative ion antibacterial modified colored DTY low-elastic yarn, characterized in that: The steps include: Step 1, pre-crystallizing polyethylene terephthalate slices at high temperature, then drying them, and obtaining pre-crystallized polyethylene terephthalate fine powder after ball milling; Step 2, adding modified anion fine powder, masterbatch and reinforcing filler to pre-crystallized polyethylene terephthalate fine powder and mixing them evenly, and then adding them to a twin-screw extruder for melt extrusion to obtain a mixed melt; the modified anion fine powder adopts modified bamboo charcoal particles; and the modified bamboo charcoal particles adopt silicon-oxygen wrapped bamboo charcoal particles, and there is a gap between the bamboo charcoal particles and the silicon-oxygen wrapped layer; Step 3, adding the mixed melt into a spinning box, and cooling it uniformly into POY by ring blowing, and obtaining anion antibacterial modified colored DTY low-elastic yarn by elastic treatment; The preparation method of silicon-oxygen coated bamboo charcoal particles comprises the following steps: a1, wet grinding bamboo charcoal particles for 2-4 hours, and obtaining bamboo charcoal fine powder after evaporation; a2, placing ethyl cellulose in ether to form a dissolving solution, and placing bamboo charcoal fine powder in it, and filtering and drying after ultrasonic treatment for 1-2 hours to obtain coated bamboo charcoal particles; a3, mixing methyltrichlorosilane with ether to form a diluent, and then spraying it on the surface of the coated bamboo charcoal particles to form a liquid film, and obtaining prefabricated modified bamboo charcoal particles after drying, standing and heating and standing; a4, treating the prefabricated modified bamboo charcoal particles with ultraviolet light for 2-3 hours, and then purging with nitrogen to obtain modified bamboo charcoal particles; in a1, the wet grinding uses ether as solvent, and the mass ratio of bamboo charcoal particles to ether is 3-5:1, and the grinding pressure is 0.3-0.5MPa; the evaporation temperature is 40-50°C; in a2, the The concentration of ethyl cellulose in ether is 20-30g / L, the concentration of the bamboo charcoal powder in the dissolving solution is 10-15g / L, the ultrasonic frequency of the ultrasonic treatment is 60-80kHz, the temperature is 5-10°C, and the drying temperature is 40-50°C; in a3, the volume ratio of methyltrichlorosilane to ether is 1:3-5, the spraying speed is 3-5mL / min, the spraying time is 2-4s, the drying temperature is 40-45°C, the static atmosphere is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 10-12:1, and the temperature of the heating and static is 80-100°C; in a4, the power of the ultraviolet light treatment is 200-300W, the nitrogen temperature of the nitrogen purge is 80-100°C, and the speed is 10-20mL / min; The mass ratio of the mixed melt in step 2 is: 180-200 parts of pre-crystallized polyethylene terephthalate fine powder, 8-10 parts of modified anion fine powder, 3-5 parts of masterbatch, and 5-10 parts of reinforcing filler; The reinforcing filler is a porous silica filler, and the preparation method of the porous silica filler comprises the following steps: b1, adding dodecyltrimethoxysilane, hexadecyltrimethoxysilane and butyltriethoxysilane to ether and stirring evenly to form a mixed solution, then adding ethyl cellulose and ultrasonically treating for 20-30 minutes to obtain a mixed dispersion, wherein the molar ratio of dodecyltrimethoxysilane, hexadecyltrimethoxysilane and butyltriethoxysilane is 1:1-2:2-4, the concentration of dodecyltrimethoxysilane in ether is 40-80g / L, the stirring speed is 300-500r / min, the concentration of ethyl cellulose in ether is 70-100g / L, the temperature of the ultrasonic treatment is 5-10°C, and the ultrasonic frequency is 80-100kHz; b2 , spray the mixed dispersion into the reactor, and obtain hydrolyzed particles through deposition and purging, the spraying speed is 5-10L / min, the atmosphere of the reactor is a mixed atmosphere of nitrogen and water vapor, and the volume ratio of nitrogen to water vapor is 8-10:1, and the temperature is 40-50°C; the deposition temperature is 100-110°C, the purging uses dry nitrogen at 80-90°C, and the purging speed is 5-10mL / min; b3, put the hydrolyzed particles into ethanol for ultrasonic treatment for 1-2h, filter and wash 1-3 times, and spray dry to obtain porous silica filler, the concentration of the hydrolyzed particles in ethanol is 100-300g / L, the temperature of ultrasonic treatment is 30-40°C, the frequency is 70-90kHz, ethanol is used for washing, and the temperature of spray drying is 100-120°C.

2. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The temperature of the high temperature pre-crystallization in step 1 is 170-175° C., the temperature of the drying treatment is 180-185° C., and the time is 5-7 hours.

3. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The ball milling process in step 1 is performed at a pressure of 0.4-0.6 MPa and a temperature of 5-10°C.

4. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The masterbatch is one or more of magenta masterbatch, cyan masterbatch and yellow masterbatch.

5. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The temperature of the melt extrusion in step 2 is 280-290° C. and the pressure is 7-8 MPa.

6. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The spinning temperature in step 3 is 285-295° C., the temperature of the annular air is 22-25° C., the wind speed is 0.5-0.7 m / s, and the humidity is 65-85%.

7. The method for preparing the negative ion antibacterial modified colored DTY low-elastic yarn according to claim 1, characterized in that: The texturing treatment in step 3 is to sequentially spin the yarn through a pre-netting nozzle, a yarn guide, a first roller, a false twister, a second roller, a final netting, a third roller and a winding roller, thereby obtaining polyester low-stretch yarn.

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