Antibacterial regenerated polyester fiber and preparation method thereof

Abstract

The invention relates to an antibacterial regenerated polyester fiber and a preparation method thereof, and belongs to the technical field of textile. The antibacterial regenerated polyester fiber is prepared by taking waste polyester fiber, ethylene glycol, an alcoholysis catalyst, a flame-retardant bacteriostatic agent, a polycondensation catalyst and a heat stabilizer as raw materials, and the preparation method comprises the following steps: firstly, carrying out alcoholysis on the waste polyester fiber by using the ethylene glycol and the alcoholysis catalyst, and purifying an alcoholysis product; the preparation method comprises the following steps: preparing a flame-retardant antibacterial agent, reacting ethylene glycol with the flame-retardant antibacterial agent to prepare an intermediate, carrying out condensation polymerization on the intermediate, an alcoholysis product, a condensation polymerization catalyst and a heat stabilizer to obtain antibacterial PET, and adding the antibacterial PET into a double-screw extruder for melt extrusion spinning to obtain the antibacterial regenerated polyester fiber. According to the antibacterial regenerated polyester fiber and the preparation method thereof disclosed by the invention, the used raw material is the waste polyester fiber, so that the antibacterial regenerated polyester fiber conforms to the environment-friendly concept, has good antibacterial and flame-retardant effects, can take effect for a long time, and can be widely applied to the field of textiles and garments.

Description

Technical Field

[0001] The invention belongs to the field of textile technology, and specifically relates to an antibacterial regenerated polyester fiber and a preparation method thereof. Background Art

[0002] Polyester fiber, also known as dacron, is an important synthetic fiber with high strength, good heat resistance, strong light resistance, acid and alkali resistance, good color fastness, washability, sun resistance, and not easy to fade. It is durable and widely used in the production of clothing, bedding and other skin-contact textiles. However, polyester fiber itself does not have antibacterial properties and lacks protection for the human body. In the prior art, antibacterial agents are often added during preparation for antibacterial treatment to improve this shortcoming. However, even after antibacterial treatment of polyester fibers, their antibacterial agents may gradually lose their effectiveness over time. Daily care processes such as washing and sun exposure may accelerate the loss of antibacterial agents, resulting in a decrease in the antibacterial effect and failure to take effect for a long time.

[0003] In addition, in recent years, with the continuous increase in the annual output of polyester fibers, the storage of waste polyester textiles has continued to grow, causing serious waste of resources and solid waste pollution problems. Based on this, the present invention provides an antibacterial regenerated polyester fiber and a preparation method thereof, which uses waste polyester fibers to prepare an antibacterial polyester fiber that can be effective for a long time. Summary of the invention

[0004] The object of the present invention is to provide an antibacterial regenerated polyester fiber and a preparation method thereof, so as to solve the problems mentioned in the above background technology.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 80-100 parts of waste polyester fiber, 168-224 parts of ethylene glycol, 0.3-0.4 parts of alcoholysis catalyst, 4-12 parts of flame retardant and antibacterial agent, 0.2-0.25 parts of polycondensation catalyst, and 0.08-0.1 parts of heat stabilizer;

[0007] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0008] The first step is to weigh the raw materials according to the mass proportions: 80-100 parts of waste polyester fiber, 168-224 parts of ethylene glycol, 0.3-0.4 parts of alcoholysis catalyst, 4-12 parts of flame retardant and antibacterial agent, 0.2-0.25 parts of polycondensation catalyst, and 0.08-0.1 parts of heat stabilizer;

[0009] The second step is to put the waste polyester fiber, ethylene glycol and alcoholysis catalyst into a nitrogen-protected reflux reaction vessel, and carry out alcoholysis reaction at a temperature of 185-215°C. After the reaction is completed, the temperature of the system in the container is reduced to 150°C, and the solid is filtered and removed. Then, deionized water is added to the filtrate and cooled to room temperature. The filter cake is vacuum filtered and washed with deionized water and then dried to obtain an alcoholysis product.

[0010] The third step is to put the flame retardant and antibacterial agent and ethylene glycol into a reaction container and react at a temperature of 80°C, then put the alcoholysis product, polycondensation catalyst and thermal stabilizer in the second step into the container, and evacuate the air in the container to reduce the pressure to 0.01MPa, and then carry out polycondensation reaction at a temperature of 260-280°C to obtain antibacterial PET;

[0011] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber.

[0012] Furthermore, the alcoholysis catalyst used is zinc acetate.

[0013] Furthermore, the polycondensation catalyst used is antimony trioxide.

[0014] Furthermore, the thermal stabilizer is trimethyl phosphate.

[0015] Furthermore, the alcoholysis reaction time in the second step is 8-10 hours, and the amount of ethylene glycol used in the second step is twice that of the waste polyester fiber in terms of mass fraction.

[0016] Furthermore, in the third step, the reaction time of the flame retardant and antibacterial agent with ethylene glycol is 1-1.5 hours, the polycondensation reaction time is 2.5-3 hours, and the amount of ethylene glycol used in the third step is twice that of the flame retardant polyester fiber in terms of mass fraction.

[0017] Furthermore, in the fourth step, the parameters of the twin-screw extruder are set to 280°C in zone 1, 285°C in zone 2, 285°C in zone 3, 295°C in zone 4, 290°C in zone 5, and 290°C in zone 6, the screw speed is 40-50rpm, and the spinning is cooled by side wind, and the wind speed of the side wind cooling is 0.4-0.5m / s.

[0018] Furthermore, the flame retardant and antibacterial agent is prepared by the following steps.

[0019] Step 1, ethyl methyl hypophosphite, methyl 4-aminonicotinate, benzaldehyde, iodine, and cyclopentyl methyl ether are mixed in a three-necked flask, a condenser and a thermometer are installed, magnetic stirring is turned on, and the reaction is carried out at a temperature of 30-40° C. for 15-40 minutes. After the reaction is completed, deionized water is added to the three-necked flask, and extracted with dichloromethane, and then the organic layer is separated with a separatory funnel. The organic layer is rotary evaporated and then subjected to silica gel column chromatography to obtain intermediate 1;

[0020] Step 2, mix the intermediate 1, dodecane bromide and acetonitrile in a three-necked flask, install a condenser and a thermometer, start magnetic stirring, react at a temperature of 60-80°C for 18-24h, and after the reaction is completed, rotary evaporate to obtain the intermediate 2;

[0021] Step 3, the intermediate 2 and hydrochloric acid are mixed in a three-necked flask, a condenser and a thermometer are installed, magnetic stirring is turned on, and the reaction is carried out at a temperature of 80°C for 6-8h. After the reaction is completed, the solvent is removed by rotary evaporation, and the remaining solid is subjected to silica gel column chromatography to obtain the flame retardant and antibacterial agent.

[0022] Furthermore, the dosage ratio of ethyl methyl hypophosphite, 4-aminonicotinate methyl ester, benzaldehyde, iodine and cyclopentyl methyl ether used in step 1 is 0.2-0.3 mol: 0.1-0.12 mol: 0.1 mol: 0.06 mol: 60-80 mL.

[0023] Furthermore, the amount ratio of the intermediate 1, bromododecane and acetonitrile used in step 2 is 0.08 mol: 0.1-0.12 mol: 40-60 mL.

[0024] Furthermore, the hydrochloric acid used in step 3 is a hydrochloric acid aqueous solution with a mass fraction of 20%.

[0025] Furthermore, the dosage ratio of the intermediate 2 and the hydrochloric acid used in step 3 is 0.07 mol: 60-80 mL.

[0026] Beneficial effects of the present invention:

[0027] 1) The present invention uses waste polyester fiber, ethylene glycol, alcoholysis catalyst, flame retardant and antibacterial agent, polycondensation catalyst and thermal stabilizer as raw materials to prepare an antibacterial regenerated polyester fiber. The present invention firstly uses ethylene glycol and alcoholysis catalyst to alcoholyze the waste polyester fiber and purifies the alcoholysis product, then reacts ethylene glycol with the flame retardant and antibacterial agent to prepare an intermediate, finally causes the intermediate and the alcoholysis product, polycondensation catalyst and thermal stabilizer to undergo polycondensation reaction to obtain antibacterial PET, and finally adds the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber; the preparation method of the present invention combines the hypophosphite group and the carboxyl group in the flame retardant and antibacterial agent with polyethylene glycol through copolymerization, so that migration will not occur and the flame retardant and antibacterial effects can be exerted for a long time.

[0028] 2) The present invention uses methyl ethyl phosphite, 4-aminonicotinoic acid methyl ester and benzaldehyde as raw materials, and a Kabachn i kFields reaction occurs under the catalytic action of elemental iodine to obtain an intermediate 1, and then uses the intermediate 1 and dodecane bromide as raw materials to obtain an intermediate 2 by a quaternary ammonium salt reaction, and finally the phosphate ester and carboxylate ester parts of the intermediate 2 are hydrolyzed in an acidic environment to obtain a flame retardant and antibacterial agent; the flame retardant and antibacterial agent of the present invention contains a pyridyl quaternary ammonium salt structure, which can adsorb bacteria and puncture bacterial cell membranes to cause bacterial death, and has a good antibacterial effect. In addition, the flame retardant and antibacterial agent of the present invention also has a phosphate structure, which can generate phosphate after high-temperature degradation, and forms a dense carbonized layer on the surface of the substrate, thereby having a good flame retardant effect. In addition, the flame retardant and antibacterial agent of the present invention also has an aromatic ring structure, has good thermal stability and oxidation stability, and is not easily affected by the environment.

[0029] 3) The antibacterial regenerated polyester fiber prepared by the present invention and the preparation method thereof use waste polyester fiber as raw material, which conforms to the concept of environmental protection, has good antibacterial and flame retardant effects, and can be effective for a long time, and can be widely used in the field of textiles and clothing. DETAILED DESCRIPTION

[0030] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0031] Example 1

[0032] A flame retardant and antibacterial agent is prepared by the following steps:

[0033] Step 1, 0.2 mol ethyl methyl hypophosphite, 0.1 mol 4-aminonicotinic acid methyl ester, 0.1 mol benzaldehyde, 0.06 mol iodine, and 60 mL cyclopentyl methyl ether were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the mixture was reacted at 30° C. for 15 min. After the reaction was completed, deionized water was added to the three-necked flask, and the mixture was extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated and subjected to silica gel column chromatography to obtain intermediate 1;

[0034] Step 2, 0.08 mol intermediate 1, 0.1 mol bromododecane, and 40 mL acetonitrile were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 60°C for 18 hours. After the reaction was completed, the intermediate 2 was obtained by rotary evaporation;

[0035] Step 3, 0.07 mol intermediate 2 and 60 mL of 20% hydrochloric acid aqueous solution were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 80°C for 6 hours. After the reaction was completed, the solvent was removed by rotary evaporation, and the remaining solid was subjected to silica gel column chromatography to obtain the flame retardant and antibacterial agent.

[0036] Example 2

[0037] A flame retardant and antibacterial agent is prepared by the following steps:

[0038] Step 1, 0.25 mol ethyl methyl hypophosphite, 0.11 mol 4-aminonicotinic acid methyl ester, 0.1 mol benzaldehyde, 0.06 mol iodine, 70 mL cyclopentyl methyl ether were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the mixture was reacted at 35° C. for 27 min. After the reaction was completed, deionized water was added to the three-necked flask, and the mixture was extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated and subjected to silica gel column chromatography to obtain intermediate 1;

[0039] Step 2, 0.08 mol intermediate 1, 0.11 mol bromododecane, and 50 mL acetonitrile were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 70°C for 21 hours. After the reaction was completed, the intermediate 2 was obtained by rotary evaporation;

[0040] Step 3, 0.07 mol intermediate 2 and 70 mL of 20% hydrochloric acid aqueous solution were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 80°C for 7 hours. After the reaction was completed, the solvent was removed by rotary evaporation, and the remaining solid was subjected to silica gel column chromatography to obtain the flame retardant and antibacterial agent.

[0041] Example 3

[0042] A flame retardant and antibacterial agent is prepared by the following steps:

[0043] Step 1, 0.3 mol ethyl methyl hypophosphite, 0.12 mol 4-aminonicotinic acid methyl ester, 0.1 mol benzaldehyde, 0.06 mol iodine, 80 mL cyclopentyl methyl ether were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the mixture was reacted at 40° C. for 40 min. After the reaction was completed, deionized water was added to the three-necked flask, and the mixture was extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated and subjected to silica gel column chromatography to obtain intermediate 1;

[0044] Step 2, 0.08 mol intermediate 1, 0.12 mol bromododecane, and 60 mL acetonitrile were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 80°C for 24 hours. After the reaction was completed, the intermediate 2 was obtained by rotary evaporation;

[0045] Step 3, 0.07 mol intermediate 2 and 80 mL of 20% hydrochloric acid aqueous solution were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 80°C for 8 hours. After the reaction was completed, the solvent was removed by rotary evaporation, and the remaining solid was subjected to silica gel column chromatography to obtain the flame retardant and antibacterial agent.

[0046] Example 4

[0047] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 80 parts of waste polyester fiber, 168 parts of ethylene glycol, 0.3 parts of zinc acetate, 4 parts of the flame retardant and antibacterial agent obtained in Example 1, 0.2 parts of antimony trioxide, and 0.08 parts of trimethyl phosphate;

[0048] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0049] The first step is to weigh 80 parts of waste polyester fibers, 168 parts of ethylene glycol, 0.3 parts of zinc acetate, 4 parts of the flame retardant and antibacterial agent obtained in Example 1, 0.2 parts of antimony trioxide, and 0.08 parts of trimethyl phosphate according to the mass ratio of each raw material;

[0050] Step 2: Put the waste polyester fiber, ethylene glycol and zinc acetate into a nitrogen-protected reflux reaction vessel, react at 185°C for 8 hours, and after the reaction is completed, reduce the temperature of the system in the container to 150°C, filter and remove the solid, then add deionized water to the filtrate and cool it to room temperature, vacuum filter, wash the filter cake with deionized water and dry it to obtain an alcoholysis product. In this step, the amount of ethylene glycol is twice that of the waste polyester fiber in terms of mass fraction;

[0051] The third step is to put the flame retardant and antibacterial agent obtained in Example 1 and ethylene glycol into a reaction container, react at a temperature of 80°C for 1 hour, then put the alcoholysis product, antimony trioxide and trimethyl phosphate in the second step into the container, and evacuate the air in the container to reduce the pressure to 0.01MPa, and then react at a temperature of 260°C for 2.5 hours to obtain antibacterial PET. In this step, the amount of ethylene glycol is twice that of the flame retardant and antibacterial agent in terms of mass fraction;

[0052] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber, wherein the parameters of the twin-screw extruder are set as 280°C for zone 1, 285°C for zone 2, 285°C for zone 3, 295°C for zone 4, 290°C for zone 5, and 290°C for zone 6, the screw speed is 40rpm, and the spinning is cooled by side wind, and the wind speed of the side wind cooling is 0.4m / s.

[0053] Example 5

[0054] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 90 parts of waste polyester fiber, 196 parts of ethylene glycol, 0.3 parts of zinc acetate, 8 parts of the flame retardant and antibacterial agent obtained in Example 2, 0.22 parts of antimony trioxide, and 0.09 parts of trimethyl phosphate;

[0055] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0056] The first step is to weigh the raw materials according to the mass fractions: 90 parts of waste polyester fiber, 196 parts of ethylene glycol, 0.3 parts of zinc acetate, 8 parts of the flame retardant and antibacterial agent obtained in Example 2, 0.22 parts of antimony trioxide, and 0.09 parts of trimethyl phosphate;

[0057] Step 2: Put the waste polyester fiber, ethylene glycol and zinc acetate into a nitrogen-protected reflux reaction vessel, react at 198°C for 9 hours, and after the reaction is completed, reduce the temperature of the system in the container to 150°C, filter and remove the solid, then add deionized water to the filtrate and cool it to room temperature, vacuum filter and wash the filter cake with deionized water and dry it to obtain an alcoholysis product. In this step, the amount of ethylene glycol is twice that of the waste polyester fiber in terms of mass fraction;

[0058] The third step is to put the flame retardant and antibacterial agent obtained in Example 2 and ethylene glycol into a reaction container, react at a temperature of 80°C for 1.25 hours, then put the alcoholysis product, antimony trioxide and trimethyl phosphate in the second step into the container, and evacuate the air in the container to reduce the pressure to 0.01MPa, and then react at a temperature of 270°C for 2.75 hours to obtain antibacterial PET. In this step, the amount of ethylene glycol is twice that of the flame retardant and antibacterial agent in terms of mass fractions;

[0059] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber, wherein the parameters of the twin-screw extruder are set as 280°C for zone 1, 285°C for zone 2, 285°C for zone 3, 295°C for zone 4, 290°C for zone 5, 290°C for zone 6, the screw speed is 45rpm, and the spinning is side-wind cooled, and the wind speed of the side-wind cooling is 0.45m / s.

[0060] Example 6

[0061] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, 12 parts of the flame retardant and antibacterial agent obtained in Example 3, 0.25 parts of antimony trioxide, and 0.1 parts of trimethyl phosphate;

[0062] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0063] The first step is to weigh the raw materials according to their mass fractions: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, 12 parts of the flame retardant and antibacterial agent obtained in Example 3, 0.25 parts of antimony trioxide, and 0.1 parts of trimethyl phosphate;

[0064] Step 2: Put the waste polyester fiber, ethylene glycol and zinc acetate into a nitrogen-protected reflux reaction vessel, react at a temperature of 215°C for 10 hours, and after the reaction is completed, reduce the temperature of the system in the container to 150°C, filter and remove the solid, then add deionized water to the filtrate and cool it to room temperature, vacuum filter and wash the filter cake with deionized water and then dry to obtain an alcoholysis product. In this step, the amount of ethylene glycol is twice that of the waste polyester fiber in terms of mass fraction;

[0065] The third step is to put the flame retardant and antibacterial agent obtained in Example 3 and ethylene glycol into a reaction container, react at a temperature of 80°C for 1.5 hours, then put the alcoholysis product, antimony trioxide and trimethyl phosphate in the second step into the container, and evacuate the air in the container to reduce the pressure to 0.01MPa, and then react at a temperature of 280°C for 3 hours to obtain antibacterial PET. In this step, the amount of ethylene glycol is twice that of the flame retardant and antibacterial agent in terms of mass fraction;

[0066] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber, wherein the parameters of the twin-screw extruder are set as 280°C for zone 1, 285°C for zone 2, 285°C for zone 3, 295°C for zone 4, 290°C for zone 5, and 290°C for zone 6, the screw speed is 50rpm, and the spinning is cooled by side wind, and the wind speed of the side wind cooling is 0.5m / s.

[0067] Comparative Example 1

[0068] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, 0.25 parts of antimony trioxide, and 0.1 parts of trimethyl phosphate;

[0069] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0070] The first step is to weigh the raw materials according to the mass proportions: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, 0.25 parts of antimony trioxide, and 0.1 parts of trimethyl phosphate;

[0071] Step 2: Put the waste polyester fiber, ethylene glycol and zinc acetate into a nitrogen-protected reflux reaction vessel, react at a temperature of 215°C for 10 hours, and after the reaction is completed, reduce the temperature of the system in the container to 150°C, filter and remove the solid, then add deionized water to the filtrate and cool it to room temperature, vacuum filter and wash the filter cake with deionized water and then dry to obtain an alcoholysis product. In this step, the amount of ethylene glycol is twice that of the waste polyester fiber in terms of mass fraction;

[0072] Step 3: Add ethylene glycol, the alcoholysis product in the second step, antimony trioxide, and trimethyl phosphate into the reaction container, and evacuate the air in the container to reduce the pressure to 0.01 MPa, and then react at a temperature of 280° C. for 3 hours to obtain antibacterial PET. In this step, ethylene glycol is all the remaining polyethylene glycol.

[0073] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber, wherein the parameters of the twin-screw extruder are set as 280°C for zone 1, 285°C for zone 2, 285°C for zone 3, 295°C for zone 4, 290°C for zone 5, and 290°C for zone 6, the screw speed is 50rpm, and the spinning is cooled by side wind, and the wind speed of the side wind cooling is 0.5m / s.

[0074] Comparative Example 2

[0075] An antibacterial regenerated polyester fiber, comprising the following raw materials in parts by weight: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, and 0.25 parts of antimony trioxide;

[0076] A method for preparing an antibacterial regenerated polyester fiber comprises the following steps:

[0077] The first step is to weigh the raw materials according to their mass fractions: 100 parts of waste polyester fiber, 224 parts of ethylene glycol, 0.4 parts of zinc acetate, and 0.25 parts of antimony trioxide;

[0078] Step 2: Put the waste polyester fiber, ethylene glycol and zinc acetate into a nitrogen-protected reflux reaction vessel, react at a temperature of 215°C for 10 hours, and after the reaction is completed, reduce the temperature of the system in the container to 150°C, filter and remove the solid, then add deionized water to the filtrate and cool it to room temperature, vacuum filter and wash the filter cake with deionized water and then dry to obtain an alcoholysis product. In this step, the amount of ethylene glycol is twice that of the waste polyester fiber in terms of mass fraction;

[0079] Step 3: Add ethylene glycol, the alcoholysis product in the second step, and antimony trioxide into the reaction container, and evacuate the air in the container to reduce the pressure to 0.01 MPa, and then react at a temperature of 280° C. for 3 hours to obtain antibacterial PET. In this step, ethylene glycol is all the remaining polyethylene glycol.

[0080] The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber, wherein the parameters of the twin-screw extruder are set as 280°C for zone 1, 285°C for zone 2, 285°C for zone 3, 295°C for zone 4, 290°C for zone 5, and 290°C for zone 6, the screw speed is 50rpm, and the spinning is cooled by side wind, and the wind speed of the side wind cooling is 0.5m / s.

[0081] Comparative Example 3

[0082] This comparative example is the flame-retardant polyester sold by Jiangsu Xinzhanjiang Fiber Technology Co., Ltd.

[0083] Comparative Example 4

[0084] This comparative example is the antibacterial polyester sold by Qingdao Xinwei Textile Development Co., Ltd.

[0085] The performance tests were performed on the regenerated polyester fibers in Examples 4-6 and Comparative Examples 1-2 and the commercially available polyester in Comparative Examples 3-4, respectively. The oxygen index was tested with reference to the national standard GB / T2406-93 "Plastic Combustion Performance Test Method Oxygen Index Method", and the antibacterial rates against Escherichia coli and Staphylococcus aureus were tested with reference to GB / T 20944.3-2007 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method". After washing 50 times, the test was repeated. The test results are shown in Table 1:

[0086] Table 1

[0087]

[0088] It can be seen from Table 1 that the limiting oxygen index and antibacterial rate of the antibacterial regenerated polyester fiber of the present invention in Examples 4-6 are better than those of the commercially available antibacterial polyester and flame-retardant polyester, indicating that the antibacterial regenerated polyester fiber of the present invention has good antibacterial and flame retardant effects. Comparative Examples 1-2 carried out control experiments on the flame retardant and antibacterial agent and the heat stabilizer used in the present invention. The results show that the antibacterial regenerated polyester fiber prepared without the flame retardant and antibacterial agent of the present invention does not have flame retardant and antibacterial effects, while the use of the heat stabilizer has almost no effect on the flame retardant and antibacterial effects of the antibacterial regenerated polyester fiber. In summary, the preparation method of the present invention prepares an antibacterial regenerated polyester fiber with good flame retardancy and antibacterial effects, is less affected by water washing, and can be effective for a long time.

[0089] The above is a detailed introduction to an antibacterial regenerated polyester fiber and a preparation method thereof provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core ideas, including the best mode, and also enables any technician in the field to practice the present invention, including the manufacture and use of any device or system, and the implementation of any combination method. It should be pointed out that for ordinary technicians in this technical field, the present invention can also be improved and modified without departing from the principles of the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed in the present invention can be combined with each other in any way. The reason why these combinations are not exhaustively described in this specification is only for the consideration of omitting space and saving resources. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.

Claims

1. An antibacterial regenerated polyester fiber, characterized in that: The invention comprises the following raw materials in parts by weight: 80-100 parts of waste polyester fiber, 168-224 parts of ethylene glycol, 0.3-0.4 parts of alcoholysis catalyst, 4-12 parts of flame retardant and antibacterial agent, 0.2-0.25 parts of polycondensation catalyst and 0.08-0.1 parts of heat stabilizer; Wherein, the flame retardant and antibacterial agent is prepared by the following steps: Step 1, ethyl methyl phosphite, methyl 4-aminonicotinate, benzaldehyde, iodine and cyclopentyl methyl ether are mixed in a container, stirred evenly, and reacted at a temperature of 30-40° C. for 15-40 min to obtain intermediate 1; Step 2, mixing intermediate 1, dodecane bromide and acetonitrile in a container, stirring evenly, and reacting at a temperature of 60-80° C. for 18-24 hours to obtain intermediate 2; Step 3: Mix the intermediate 2 and hydrochloric acid in a container, stir evenly, and react at 80° C. for 6-8 hours to obtain the flame retardant and antibacterial agent.

2. The antibacterial regenerated polyester fiber according to claim 1, characterized in that: The amount ratio of ethyl methyl hypophosphite, 4-aminonicotinic acid methyl ester, benzaldehyde, iodine and cyclopentyl methyl ether used in step 1 is 0.2-0.3 mol: 0.1-0.12 mol: 0.1 mol: 0.06 mol: 60-80 mL.

3. The antibacterial regenerated polyester fiber according to claim 1, characterized in that: The amount ratio of intermediate 1, bromododecane and acetonitrile used in step 2 is 0.08 mol: 0.1-0.12 mol: 40-60 mL.

4. The antibacterial regenerated polyester fiber according to claim 1, characterized in that: The hydrochloric acid used in step 3 is a hydrochloric acid aqueous solution with a mass fraction of 20%.

5. The antibacterial regenerated polyester fiber according to claim 1, characterized in that: The dosage ratio of intermediate 2 and hydrochloric acid used in step 3 is 0.07 mol: 60-80 mL.

6. A method for preparing the antibacterial regenerated polyester fiber according to any one of claims 1 to 5, characterized in that: The method comprises the following preparation steps: The first step is to weigh the raw materials according to the mass proportions: 80-100 parts of waste polyester fiber, 168-224 parts of ethylene glycol, 0.3-0.4 parts of alcoholysis catalyst, 4-12 parts of flame retardant and antibacterial agent, 0.2-0.25 parts of polycondensation catalyst, and 0.08-0.1 parts of heat stabilizer; The second step is to put the waste polyester fiber, ethylene glycol and alcoholysis catalyst into a nitrogen-protected reflux reaction vessel, and carry out alcoholysis reaction at a temperature of 185-215°C. After the reaction is completed, the temperature of the system in the container is reduced to 150°C, and the solid is filtered and removed. Then, deionized water is added to the filtrate and cooled to room temperature. The filter cake is vacuum filtered and washed with deionized water and then dried to obtain an alcoholysis product. The third step is to put the flame retardant and antibacterial agent and ethylene glycol into a reaction container and react at a temperature of 80°C, then put the alcoholysis product, polycondensation catalyst and thermal stabilizer in the second step into the container, and evacuate the air in the container to reduce the pressure to 0.01MPa, and then carry out polycondensation reaction at a temperature of 260-280°C to obtain antibacterial PET; The fourth step is to add the antibacterial PET into a twin-screw extruder for melt extrusion spinning to obtain an antibacterial regenerated polyester fiber.

7. The method for preparing an antibacterial regenerated polyester fiber according to claim 6, characterized in that: The alcoholysis catalyst used is zinc acetate, the polycondensation catalyst used is antimony trioxide, and the heat stabilizer is trimethyl phosphate.

8. The method for preparing an antibacterial regenerated polyester fiber according to claim 6, characterized in that: The alcoholysis reaction time in the second step is 8-10 hours. The amount of ethylene glycol used in the second step is twice that of the waste polyester fiber in terms of mass fraction.

9. The method for preparing an antibacterial regenerated polyester fiber according to claim 6, characterized in that: The time condition for the reaction of the flame retardant and antibacterial agent with ethylene glycol in the third step is 1-1.5 hours, and the time condition for the polycondensation reaction is 2.5-3 hours. The amount of ethylene glycol used in the third step is twice that of the flame retardant polyester fiber in terms of mass fraction.

10. The method for preparing an antibacterial regenerated polyester fiber according to claim 6, characterized in that: In the fourth step, the parameters of the twin-screw extruder are set to 280°C in zone 1, 285°C in zone 2, 285°C in zone 3, 295°C in zone 4, 290°C in zone 5, and 290°C in zone 6, the screw speed is 40-50rpm, and the spinning is cooled by side wind with a wind speed of 0.4-0.5m / s.

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