Antibacterial multifunctional polyester fiber based on wormwood and preparation method thereof

Abstract

The invention discloses an antibacterial multifunctional polyester fiber based on wormwood and a preparation method of the antibacterial multifunctional polyester fiber, particularly relates to the technical field of fiber materials, and relates to the antibacterial multifunctional polyester fiber based on wormwood and the preparation method of the antibacterial multifunctional polyester fiber. The antibacterial multifunctional polyester fiber based on wormwood is prepared from terephthalic acid, ethylene glycol and wormwood extract. The preparation method specifically comprises the following steps: synthesizing polyester by taking terephthalic acid and ethylene glycol as raw materials, adding a wormwood extract during synthesis to obtain a polyester melt, and then spinning the polyester melt in a screw extruder to obtain nascent fibers; stretching, curling and shaping the nascent fiber to obtain the wormwood antibacterial multifunctional polyester fiber. The wormwood component with certain hygroscopicity is added, the hygroscopicity is improved, moisture can be absorbed, a water film is formed on the surface of the fiber, the flexibility of the fiber can be improved, heat exchange and moisture transfer between air and the fiber can be promoted, and the hygroscopicity is improved.

Description

Technical Field

[0001] The invention relates to the technical field of fiber materials, and more specifically to an antibacterial multifunctional polyester fiber based on wormwood and a preparation method thereof. Background Art

[0002] As people's living standards improve, the functional requirements for textiles are becoming more and more diversified. Polyester fiber, as a widely used synthetic fiber, is widely used in the textile industry, packaging industry, and home furnishing industry. It has the functions of moisture-proof and antibacterial, easy to clean and quick-drying, and tear-resistant. Therefore, it is of great significance to develop new fiber materials with antibacterial functions to meet the market demand for healthy and functional textiles.

[0003] The polyester fiber in the related technology is mainly prepared from isophthalic acid and 1,4-butanediol, wherein isophthalic acid is introduced into the polyester molecular chain as a modified monomer, which can improve the dyeing performance, flexibility and impact resistance of the polyester fiber, making the fiber have better dyeing affinity, while also improving the fiber's toughness and elasticity and reducing the fiber's brittleness; 1,4-butanediol can adjust the performance of polyester fibers and has good heat resistance and chemical resistance.

[0004] However, it still has some shortcomings in actual use, such as lack of antibacterial properties. Traditional polyester fibers themselves do not have antibacterial functions. In daily use, they are prone to breed bacteria and mold microorganisms, produce odors, and affect sleep quality and physical health; poor hygroscopicity. Traditional polyester fibers have a tight molecular structure and lack hydrophilic groups, resulting in poor hygroscopicity and weak water absorption. Sweat is difficult to be absorbed and dissipated by the fibers, and is not suitable for long-term use in high temperature and high humidity environments; poor air permeability. Traditional polyester fibers have a tight and regular molecular structure and a high degree of crystallinity, which makes the gaps inside the fibers relatively few and small, making it difficult for air to circulate freely, resulting in poor air permeability, making it difficult for heat and moisture to dissipate during use, seriously affecting sleep comfort. Summary of the invention

[0005] In order to improve the above problems and reduce the problems of traditional polyester fibers lacking antibacterial properties, poor hygroscopicity and easy dust absorption, the present invention provides a multifunctional polyester fiber based on antibacterial wormwood and a preparation method thereof to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A multifunctional polyester fiber based on the antibacterial property of mugwort, prepared from terephthalic acid, ethylene glycol and mugwort extract;

[0008] Specifically, polyester is synthesized with terephthalic acid and ethylene glycol as raw materials, and wormwood extract is added during the process to obtain a polyester melt, and then the polyester melt is spun in a screw extruder to obtain primary fibers; then the primary fibers are stretched, curled, and shaped to obtain wormwood antibacterial multifunctional polyester fibers;

[0009] The wormwood extract is prepared from wormwood, water and a silane coupling agent.

[0010] Preferably, the method for preparing the antibacterial multifunctional polyester fiber based on wormwood comprises the following steps:

[0011] A1. First, terephthalic acid, ethylene glycol and wormwood extract are added to a polymerization reactor in sequence, and a stirring device is turned on. The mixture is stirred for 15-25 min at a stirring speed of 100-150 r / min, and nitrogen is continuously introduced at 10-20 L / min until the oxygen content in the reactor is reduced to 100 ppm to obtain a mixture;

[0012] A2, close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240-280° C. at a heating rate of 5° C. / min, and then esterify for 1-2 hours at a temperature of 240-280° C., a pressure of 0.2-0.5 MPa, and a stirring speed of 150-200 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50-80 mg KOH / g, to obtain an esterified product;

[0013] A3. The esterification product obtained in A2 is reacted at a temperature of 270-290° C., a stirring speed of 200-260 r / min, and a pressure of 10-60 Pa for 2-4 hours, during which the viscosity of the reaction system is measured by a rotational viscometer until the viscosity reaches 800-1500 Pa·s, to obtain a polycondensation melt.

[0014] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250-270° C. in zone 1, 270-290° C. in zone 2, 290-310° C. in zone 3, and a screw speed of 25-50 r / min, filtering the melt through a filter, and spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140° C. to obtain nascent fibers;

[0015] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0016] Preferably, the components and weight proportions of the raw materials for preparing the antibacterial multifunctional polyester fiber based on wormwood are as follows:

[0017] 50-90 parts of terephthalic acid, 31-57 parts of ethylene glycol and 0.25-7.2 parts of mugwort extract.

[0018] Preferably, the method for preparing the wormwood extract comprises the following steps:

[0019] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, and then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% at a turning frequency of 5h / time for 48h until the moisture content of the wormwood is reduced to 10-15%, and then place the dried wormwood in a grinder, and grind it at a speed of 1500r / min and a 10-50 mesh screen to obtain wormwood powder;

[0020] C2, the wormwood powder obtained in C1 and water are mixed and added to the extraction tank, stirred at a stirring speed of 100r / min for 10min, and then the heating system of the extraction tank is started, and the temperature is raised to 80-100°C at a heating rate of 5°C / min, and then the temperature is maintained at 80-100°C and reflux extraction is performed for 3h under the conditions of stirring speed of 80r / min, condensation temperature of 30°C, and cooling water flow rate of 0.8m3 / h, and then the extract is added to a plate and frame filter press, and filtered at a delivery pipe flow rate of 0.5m3 / h, a suction pressure of 0.3MPa, and a 200-mesh filter cloth, and the supernatant is taken to obtain a wormwood extract;

[0021] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent, then add them to a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a vacuum distillation device, and perform vacuum distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40-60°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0022] Preferably, the wormwood powder and water are prepared in a mass ratio of 1:8-15.

[0023] Preferably, the wormwood extract and the silane coupling agent are prepared in a mass ratio of 1:5-10.

[0024] Preferably, the silane coupling agent is γ-aminopropyltriethoxysilane.

[0025] Preferably, the lubricity oil is fatty acid polyethylene glycol ester.

[0026] Technical effects and advantages of the present invention:

[0027] 1. The present invention uses wormwood as a raw material to obtain wormwood extract, wherein the wormwood extract contains natural antibacterial and anti-inflammatory effects, can effectively inhibit the growth and reproduction of bacteria and microorganisms, thereby providing a durable antibacterial property for the fabric;

[0028] 2. The present invention adds a wormwood component with a certain hygroscopicity, and its hygroscopicity is improved. It can absorb water and form a water film on the fiber surface, which can not only increase the flexibility of the fiber, but also promote heat exchange and moisture transfer between air and fiber, and improve hygroscopicity;

[0029] 3. The present invention utilizes the wormwood extract to form a special microstructure inside the fiber, thereby increasing the spaces and channels between the fibers, thereby facilitating the passage of air and improving air permeability. DETAILED DESCRIPTION

[0030] The present invention is further described in detail below in conjunction with the embodiments of the present invention. The raw materials used in the examples and embodiments of the present invention are all commercially available common materials unless otherwise specified below.

[0031] Preparation Example 1

[0032] A wormwood extract is prepared by the following preparation method:

[0033] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0034] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0035] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0036] The silane coupling agent is γ-aminopropyltriethoxysilane;

[0037] Preparation Example 2

[0038] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0039] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, and then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% at a turning frequency of 5h / time for 48h until the moisture content of the wormwood is reduced to 12%, and then place the dried wormwood in a grinder, grind it at a speed of 1500r / min and use a 30-mesh screen to obtain wormwood powder;

[0040] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0041] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0042] Preparation Example 3

[0043] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0044] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 10%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0045] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0046] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0047] Preparation Example 4

[0048] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0049] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 10-mesh screen to obtain wormwood powder;

[0050] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0051] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0052] Preparation Example 5

[0053] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0054] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, and then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder, grind it at a speed of 1500r / min and use a 50-mesh screen to obtain wormwood powder;

[0055] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0056] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0057] Preparation Example 6

[0058] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0059] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0060] C2. Mix the wormwood powder obtained in C1 and water at a mass ratio of 1:12 and add them to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0061] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0062] Preparation Example 7

[0063] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0064] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0065] C2. Mix the wormwood powder obtained in C1 and water at a mass ratio of 1:15 and add them to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0066] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0067] Preparation Example 8

[0068] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0069] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0070] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 80°C at a heating rate of 5°C / min, then maintain the temperature at 80°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 2 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0071] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0072] Preparation Example 9

[0073] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0074] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0075] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 100°C at a heating rate of 5°C / min, then maintain the temperature at 100°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 4 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0076] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0077] Preparation Example 10

[0078] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0079] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0080] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0081] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:7.5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0082] Preparation Example 11

[0083] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0084] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0085] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0086] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent at a mass ratio of 1:10, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0087] Preparation Example 12

[0088] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0089] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0090] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0091] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 50°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0092] Preparation Example 13

[0093] An wormwood extract, which is different from Preparation Example 1 in that the preparation method is as follows:

[0094] C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% for 48 hours at a turning frequency of 5 hours / time until the moisture content of the wormwood is reduced to 15%, and then place the dried wormwood in a grinder and grind it at a speed of 1500r / min using a 30-mesh screen to obtain wormwood powder;

[0095] C2. Mix the wormwood powder obtained in C1 with water at a mass ratio of 1:8 and add it to the extraction tank. Stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 90°C at a heating rate of 5°C / min, then maintain the temperature at 90°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract;

[0096] C3. Mix the wormwood extract obtained in C2 and the silane coupling agent in a mass ratio of 1:5, then add them into a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a reduced pressure distillation device, and perform reduced pressure distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 60°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

[0097] Preparation Examples 14-18

[0098] A multifunctional polyester fiber based on antibacterial wormwood, the preparation components and their corresponding proportions are shown in the following table, and the fiber is prepared by the following preparation method:

[0099] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0100] The wormwood extract is prepared by Preparation Example 1;

[0101] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0102] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0103] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0104] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0105] The lubricity oil is fatty acid polyethylene glycol ester;

[0106] Table: Components and mass ratios of raw materials in Preparation Examples 14-18 (kg)

[0107]

[0108] Preparation Example 19

[0109] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0110] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 125 r / min for 20 min, during which nitrogen was continuously introduced at a rate of 15 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0111] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0112] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0113] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0114] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0115] Preparation Example 20

[0116] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0117] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 150 r / min for 25 min, during which nitrogen was continuously introduced at 20 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0118] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0119] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0120] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0121] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0122] Preparation Example 21

[0123] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0124] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0125] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 260° C. at a heating rate of 5° C. / min, and then esterify for 1.5 h at a temperature of 260° C., a pressure of 0.3 MPa, and a stirring speed of 170 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 65 mg KOH / g, to obtain an esterified product;

[0126] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0127] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0128] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0129] Preparation Example 22

[0130] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0131] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0132] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 280° C. at a heating rate of 5° C. / min, and then esterify for 2 h at a temperature of 280° C., a pressure of 0.5 MPa, and a stirring speed of 200 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 80 mg KOH / g, to obtain an esterified product;

[0133] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0134] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0135] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0136] Preparation Example 23

[0137] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0138] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0139] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0140] A3. The esterification product obtained in A2 was reacted at a temperature of 280° C., a stirring speed of 220 r / min, and a pressure of 30 Pa for 3 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 1200 Pa·s, thereby obtaining a polycondensation melt.

[0141] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0142] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0143] Preparation Example 24

[0144] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0145] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0146] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0147] A3. The esterification product obtained in A2 was reacted at a temperature of 290° C., a stirring speed of 260 r / min, and a pressure of 60 Pa for 4 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 1500 Pa·s, thereby obtaining a polycondensation melt.

[0148] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250°C in zone 1, 270°C in zone 2, 290°C in zone 3, and a screw speed of 25 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0149] A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

[0150] Preparation Example 25

[0151] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0152] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0153] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0154] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0155] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 260°C in zone 1, 220°C in zone 2, 300°C in zone 3, and a screw speed of 35 r / min, then filtering the melt through a filter, spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0156] A5. The spun fiber obtained in A4 was cooled to room temperature at a cooling air temperature of 15°C and a wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product was then placed in a crimping device at a pressure of 0.5 MPa and an air flow speed of 10 m / s. 3 / h, 5 curls / m, and finally the curled fiber enters a shaping device. After shaping at 155°C for 10 seconds, 0.5% of the fiber mass of a smoothing oil agent is used for spraying oil to obtain a multifunctional polyester fiber based on the antibacterial type of wormwood.

[0157] Preparation Example 26

[0158] A multifunctional polyester fiber based on antibacterial wormwood, which is different from Preparation Example 1 in that the preparation method is as follows:

[0159] A1. First, terephthalic acid, ethylene glycol and wormwood extract were added to a polymerization reactor in sequence, and a stirring device was turned on. The mixture was stirred at a stirring speed of 100 r / min for 15 min, during which nitrogen was continuously introduced at a rate of 10 L / min until the oxygen content in the reactor was reduced to 100 ppm, to obtain a mixture;

[0160] A2. Close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240° C. at a heating rate of 5° C. / min, and then esterify for 1 h at a temperature of 240° C., a pressure of 0.2 MPa, and a stirring speed of 150 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50 mg KOH / g, to obtain an esterified product;

[0161] A3. The esterification product obtained in A2 was reacted at a temperature of 270° C., a stirring speed of 200 r / min, and a pressure of 10 Pa for 2 h. During the reaction, the viscosity of the reaction system was measured by a rotational viscometer until the viscosity reached 800 Pa·s, thereby obtaining a polycondensation melt.

[0162] A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing it at 270°C in zone 1, 290°C in zone 2, 310°C in zone 3, and a screw speed of 50 r / min, and then filtering it through a filter, spinning it on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140°C to obtain nascent fibers;

[0163] A5. The spun fiber obtained in A4 was cooled to room temperature at a cooling air temperature of 15°C and a wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product was then placed in a crimping device at a pressure of 0.5 MPa and an air flow speed of 10 m / s. 3 / h, 5 curls / m, and finally the curled fiber enters a shaping device. After shaping at 155°C for 10 seconds, 0.5% of the fiber mass of a smoothing oil agent is used for spraying oil to obtain a multifunctional polyester fiber based on the antibacterial type of wormwood.

[0164] Preparation Examples 27-38

[0165] A multifunctional polyester fiber with antibacterial properties of mugwort, which is different from Preparation Example 14 in that the usage of mugwort extracts used in its components is different, and the specific corresponding relationship is shown in the following table.

[0166] Table: Comparison of the use of wormwood extract in Preparation Examples 27-38

[0167] Group Wormwood Extract Preparation Example 27 Prepared from Preparation Example 2 Preparation Example 28 Prepared from Preparation Example 3 Preparation Example 29 Prepared by Preparation Example 4 Preparation Example 30 Prepared from Preparation Example 5 Preparation Example 31 Prepared from Preparation Example 6 Preparation Example 32 Prepared from Preparation Example 7 Preparation Example 33 Prepared from Preparation Example 8 Preparation Example 34 Prepared from Preparation Example 9 Preparation Example 35 Prepared from Preparation Example 10 Preparation Example 36 Prepared from Preparation Example 11 Preparation Example 37 Prepared from Preparation Example 12 Preparation Example 38 Prepared from Preparation Example 13

[0168] Performance testing

[0169] The multifunctional polyester fiber based on the antibacterial type of wormwood prepared in each embodiment was selected for testing, and the test objects were 250 parts of the multifunctional polyester fiber based on the antibacterial type of wormwood, 10 parts in each group; the antibacterial property, air permeability and hygroscopicity thereof were tested, and the specific testing steps were as follows:

[0170] Antimicrobial:

[0171] First, the multifunctional polyester fiber based on the antibacterial type of wormwood prepared in the embodiment was sampled and cut into a square sample with a side length of 5 cm×5 cm, and then 20 ml100 mL10 7 CFU / ml Staphylococcus aureus suspension was added to a 250mL triangular flask containing a sample, and cultured at an oscillation frequency of 150rpm and a culture temperature of 37°C for 24 hours. The multifunctional polyester fiber based on the antibacterial type of wormwood was sampled before and after 24 hours of culture, and the antibacterial rate before and after 24 hours of culture was calculated. The antibacterial property of the multifunctional polyester fiber based on the antibacterial type of wormwood was characterized based on this data; the test results and evaluation criteria are as follows:

[0172] Antibacterial rate>90% (considered as strong antibacterial property);

[0173] 70%<antibacterial rate<90% (considered as general antibacterial property)

[0174] The antibacterial rate is less than 70% (considered as weak antibacterial activity).

[0175] Breathability:

[0176] First, the multifunctional polyester fiber based on the antibacterial wormwood prepared in the embodiment is sampled and cut into a circular sample with a diameter of 70 mm. The sample is placed on the test head of the air permeability tester, and the test program is started. The instrument automatically adjusts the pressure difference and measures the air flow rate vertically passing through a given area of ​​the sample within a specified time, and then calculates the air permeability. The air permeability of the multifunctional polyester fiber based on the antibacterial wormwood is characterized based on this data; the test results and evaluation criteria are as follows:

[0177] Air permeability>200mm / s (considered as good air permeability);

[0178] 10mm / s<air permeability<200mm / s (regarded as normal air permeability);

[0179] Air permeability <10mm / s (considered as poor air permeability).

[0180] Hygroscopicity;

[0181] First, the multifunctional polyester fiber based on the antibacterial wormwood prepared in the embodiment is sampled, and the fiber sample is placed under standard atmospheric conditions for 24 hours, and then the sample is hung in a dryer filled with a saturated ammonium chloride solution and placed at a temperature of 20°C for 24 hours. The moisture absorption rate of the sample is calculated based on the difference in the mass of the sample before and after placement and the mass of the sample before placement. The moisture absorption of the multifunctional polyester fiber based on the antibacterial wormwood is characterized based on this data; the test results and evaluation criteria are as follows:

[0182] Moisture absorption rate> 2% (considered as good hygroscopicity);

[0183] 0.5%<hygroscopicity<2% (considered as normal hygroscopicity);

[0184] Moisture absorption rate <0.5% (considered as poor hygroscopicity).

[0185] It should be specifically noted that the above-mentioned antibacterial wormwood-based multifunctional polyester fiber is produced in a normal production method, and the defective antibacterial wormwood-based multifunctional polyester fiber produced is discarded.

[0186] Examples 1-5

[0187] A multifunctional polyester fiber based on antibacterial wormwood, and the corresponding relationship of the preparation method used is shown in the following table.

[0188] Table: Comparison table of the use of multifunctional polyester fibers based on wormwood antibacterial type in Examples 1-5

[0189] Group Multifunctional polyester fiber based on antibacterial properties of mugwort Example 1 Prepared from Preparation Example 14 Example 2 Prepared from Preparation Example 15 Example 3 Prepared from Preparation Example 16 Example 4 Prepared from Preparation Example 17 Example 5 Prepared from Preparation Example 18

[0190] The multifunctional polyester fibers based on the antibacterial wormwood in the above Examples 1-5 were selected, and their antibacterial properties, air permeability and hygroscopicity were tested according to the above measurement steps and measurement standards. The average values ​​of the test results were recorded in the following table.

[0191] Table: Performance test results of antibacterial rate, air permeability and moisture absorption rate of Examples 1-5

[0192]

[0193]

[0194] As can be seen from the above table, in the preparation process of the multifunctional polyester fiber based on the antibacterial wormwood in Examples 1-5, the production effect of the multifunctional polyester fiber based on the antibacterial wormwood is well improved. The carboxyl group in terephthalic acid undergoes a condensation reaction with the hydroxyl group in the ethylene glycol molecule to form a long-chain structure of the polyester molecule, which gives the fiber basic strength and toughness mechanical properties. The wormwood extract contains natural antibacterial and anti-inflammatory effects, which can effectively inhibit the growth and reproduction of bacteria and microorganisms, so that the fiber has an antibacterial function, and forms a water film on the fiber surface, which can not only increase the flexibility of the fiber, but also promote heat exchange and moisture transfer between air and fiber, and also form a special microstructure inside the fiber, which increases the gaps and channels between fibers, thereby facilitating the passage of air and improving air permeability, thereby achieving the purpose of improving the production effect of the multifunctional polyester fiber based on the antibacterial wormwood.

[0195] Its antibacterial rate is 92.4-94.3%, which is strong in antibacterial property; its air permeability is 217-234mm / s, which is considered to be good in air permeability; its moisture absorption rate is 2.45-2.59%, which is considered to be good in moisture absorption;

[0196] It can be seen that when the production raw materials are certain, the production effect of the multifunctional polyester fiber based on the antibacterial wormwood can be increased by adjusting the proportion of the preparation raw materials. Combined with the data in the above table, it is not difficult to see that when preparing the multifunctional polyester fiber based on the antibacterial wormwood, when 90 parts of terephthalic acid, 57 parts of ethylene glycol, and 7.2 parts of wormwood extract are used, the antibacterial property, air permeability, and hygroscopicity are the highest. The reason for this is that the higher the content of wormwood extract, the better the antibacterial and hygroscopicity of the fiber; a relatively high content of ethylene glycol will make the fiber structure relatively loose, which is conducive to air permeability; obtained from Examples 1-5.

[0197] Embodiment 6-13

[0198] A multifunctional polyester fiber based on antibacterial wormwood, and the corresponding relationship of the preparation method used is shown in the following table.

[0199] Table: Comparison table of the use of multifunctional polyester fibers based on wormwood antibacterial type in Examples 6-13

[0200]

[0201]

[0202] The multifunctional polyester fibers based on the antibacterial wormwood in the above Examples 6-13 were selected, and their antibacterial properties, air permeability and hygroscopicity were tested according to the above measurement steps and measurement standards. The average values ​​of the test results were recorded in the following table.

[0203] Table: Performance test results of antibacterial rate, air permeability and moisture absorption rate of Examples 1, 6-13

[0204]

[0205] As can be seen from the above table, in the preparation process of the multifunctional polyester fiber based on the antibacterial wormwood in Examples 6-13, the production effect of the multifunctional polyester fiber based on the antibacterial wormwood is well improved. The carboxyl group in terephthalic acid undergoes a condensation reaction with the hydroxyl group in the ethylene glycol molecule to form a long-chain structure of the polyester molecule, which gives the fiber basic strength and toughness mechanical properties. The wormwood extract contains natural antibacterial and anti-inflammatory effects, which can effectively inhibit the growth and reproduction of bacteria and microorganisms, so that the fiber has an antibacterial function, and forms a water film on the fiber surface, which can not only increase the flexibility of the fiber, but also promote heat exchange and moisture transfer between air and fiber, and also form a special microstructure inside the fiber, which increases the gaps and channels between fibers, thereby facilitating the passage of air and improving air permeability, thereby achieving the purpose of improving the production effect of the multifunctional polyester fiber based on the antibacterial wormwood.

[0206] Its antibacterial rate is 92.1-93.5%, which is strong in antibacterial property; its air permeability is 214-227mm / s, which is considered to be good in air permeability; its moisture absorption rate is 2.43-2.53%, which is considered to be good in moisture absorption;

[0207] It can be seen that when the production raw materials are certain, the production effect of the multifunctional polyester fiber based on the antibacterial type of wormwood can be increased by adjusting the proportion of the preparation raw materials. Combined with the data in the above table, it is not difficult to see that when preparing the multifunctional polyester fiber based on the antibacterial type of wormwood, the stirring speed in the hot pot stage is 125r / min for 20min, the nitrogen introduction rate is 15L / min, and the esterification process is esterified for 1.5h under the conditions of temperature 260℃, pressure 0.3MPa, and stirring speed 170r / min. The acid value in the reaction system is reduced to 65mg KOH / g, the temperature during the polycondensation process is 280°C, the stirring speed is 220r / min, and the pressure is 30Pa. The reaction is carried out for 3h until the viscosity of the reaction system reaches 1200Pa·s. The spinning stage is prepared by shearing at 260°C in the first zone, 220°C in the second zone, 300°C in the third zone, and a screw speed of 35r / min. The antibacterial property, air permeability and hygroscopicity are the highest under the conditions of shearing at 260°C in the first zone, 220°C in the second zone, 300°C in the third zone, and a screw speed of 35r / min; obtained from Examples 1 and 6-13.

[0208] Examples 14-25

[0209] A multifunctional polyester fiber based on antibacterial wormwood, and the corresponding relationship of the preparation method used is shown in the following table.

[0210] Table: Comparison table of the use of multifunctional polyester fibers based on wormwood antibacterial type in Examples 14-25

[0211]

[0212] The multifunctional polyester fibers based on the antibacterial wormwood in the above Examples 14-25 were selected, and their antibacterial properties, air permeability and hygroscopicity were tested according to the above measurement steps and measurement standards. The average values ​​of the test results were recorded in the following table.

[0213] Table: Performance test results of antibacterial rate, air permeability and moisture absorption rate of Examples 1, 14-25

[0214]

[0215]

[0216] As can be seen from the above table, in the preparation process of the multifunctional polyester fiber based on the antibacterial wormwood in Examples 14-25, the production effect of the multifunctional polyester fiber based on the antibacterial wormwood is well improved. The carboxyl group in terephthalic acid undergoes a condensation reaction with the hydroxyl group in the ethylene glycol molecule to form a long-chain structure of the polyester molecule, which gives the fiber basic strength and toughness mechanical properties. The wormwood extract contains natural antibacterial and anti-inflammatory effects, which can effectively inhibit the growth and reproduction of bacteria and microorganisms, so that the fiber has an antibacterial function, and forms a water film on the fiber surface, which can not only increase the flexibility of the fiber, but also promote heat exchange and moisture transfer between air and fiber, and also form a special microstructure inside the fiber, which increases the gaps and channels between fibers, thereby facilitating the passage of air and improving air permeability, thereby achieving the purpose of improving the production effect of the multifunctional polyester fiber based on the antibacterial wormwood.

[0217] Its antibacterial rate is 92.4-93.3%, which is strong in antibacterial property; its air permeability is 217-225mm / s, which is considered to be good in air permeability; its moisture absorption rate is 2.45-2.52%, which is considered to be good in moisture absorption;

[0218] It can be seen that when the production raw materials are certain, the production effect of the antibacterial multifunctional polyester fiber based on wormwood can be increased by adjusting the proportion of the prepared raw materials. Combined with the data in the above table, it is not difficult to see that the final moisture content of wormwood in the drying stage is reduced, a 30-mesh sieve is used in the crushing stage, the mass ratio of wormwood powder and water is increased, the reflux extraction process is refluxed at a temperature of 90°C, the mass ratio of wormwood extract and silane coupling agent is increased, and the temperature of the vacuum distillation process is increased. The antibacterial property, air permeability and hygroscopicity are all the highest. The reason for this is that high water content will cause some components to be diluted or hydrolyzed and lost during storage or the initial stage of extraction; increasing the mass ratio of wormwood powder and water can extract more wormwood extract; increasing the mass ratio of wormwood extract and silane coupling agent can allow more wormwood extract to react with silane coupling agent; reflux extraction at 90°C, this temperature is conducive to the dissolution of various antibacterial active ingredients in wormwood; increasing the vacuum distillation process temperature, which can more effectively remove the solvent and impurities in the extract; a 30-mesh screen is used in the crushing step, and the obtained wormwood powder particles are of moderate size, which is helpful to better mix the wormwood components with the polyester raw materials during the polyester synthesis process, so that a microstructure that is more conducive to the passage of gas is formed inside the fiber; more wormwood extract introduced into the polyester fiber will change the crystallization behavior of the polyester, interfere with the regular arrangement of the molecular chains, reduce the crystallinity or change the crystal morphology, thereby forming more pores and channels inside the fiber, which is conducive to the diffusion of gas molecules; increasing the vacuum distillation temperature increases the purity of the wormwood extract and reduces the interference of impurity components on the hydrophilic groups; the combined effect of the crushing step and the extraction conditions changes the microstructure of the fiber, which provides more pathways for water molecules to enter the fiber, and also increases the surface area inside the fiber for water molecules to adsorb, thereby improving hygroscopicity; obtained from Examples 1, 14-25.

[0219] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A multifunctional polyester fiber based on antibacterial wormwood, characterized in that: Prepared from terephthalic acid, ethylene glycol and wormwood extract; Specifically, polyester is synthesized with terephthalic acid and ethylene glycol as raw materials, and wormwood extract is added during the process to obtain a polyester melt, and then the polyester melt is spun in a screw extruder to obtain primary fibers; then the primary fibers are stretched, curled, and shaped to obtain wormwood antibacterial multifunctional polyester fibers; The wormwood extract is prepared from wormwood, water and a silane coupling agent.

2. The multifunctional polyester fiber based on the antibacterial property of wormwood according to claim 1, characterized in that: The components and weight proportions of the raw materials for preparing the multifunctional polyester fiber based on antibacterial wormwood are as follows: 50-90 parts of terephthalic acid, 31-57 parts of ethylene glycol and 0.25-7.2 parts of mugwort extract.

3. The multifunctional polyester fiber based on the antibacterial property of wormwood according to claim 1, characterized in that: The weight proportion of the mugwort extract is preferably 7.2 parts.

4. The multifunctional polyester fiber based on the antibacterial property of wormwood according to claim 1, characterized in that: The silane coupling agent is γ-aminopropyltriethoxysilane.

5. A method for preparing a multifunctional polyester fiber based on antibacterial wormwood as claimed in any one of claims 1 to 4, characterized in that: The following steps are involved: A1. First, terephthalic acid, ethylene glycol and wormwood extract are added to a polymerization reactor in sequence, and a stirring device is turned on. The mixture is stirred for 15-25 min at a stirring speed of 100-150 r / min, and nitrogen is continuously introduced at 10-20 L / min until the oxygen content in the reactor is reduced to 100 ppm to obtain a mixture; A2, close the feed port and exhaust port of the reactor, turn on the heating system, raise the temperature of the reaction system to 240-280° C. at a heating rate of 5° C. / min, and then esterify for 1-2 hours at a temperature of 240-280° C., a pressure of 0.2-0.5 MPa, and a stirring speed of 150-200 r / min, during which the water generated by the reaction is removed until the acid value in the reaction system is reduced to 50-80 mg KOH / g, to obtain an esterified product; A3, reacting the esterification product obtained in A2 at a temperature of 270-290° C., a stirring speed of 200-260 r / min, and a pressure of 10-60 Pa for 2-4 hours, during which the viscosity of the reaction system is measured by a rotational viscometer until the viscosity reaches 800-1500 Pa·s, to obtain a polycondensation melt; A4, placing the polycondensation melt obtained in A3 in a screw extruder, shearing the melt at 250-270° C. in zone 1, 270-290° C. in zone 2, 290-310° C. in zone 3, and a screw speed of 25-50 r / min, filtering the melt through a filter, and spinning the melt on a 100-hole spinneret at a pressure of 5 MPa, a spinning speed of 900 m / min, and a setting temperature of 140° C. to obtain nascent fibers; A5. The spun fiber obtained in A4 is cooled to room temperature under the conditions of cooling air temperature of 15°C and wind speed of 0.5 m / s, and then placed in a stretching device for stretching at a stretching temperature of 70°C and a stretching multiple of 2.5 times. The product is then placed in a curling device for curling at a pressure of 0.5 MPa, an air flow velocity of 10 m3 / h, and 5 curls / m. Finally, the curled fiber enters a shaping device, and after shaping at 155°C for 10 seconds, it is sprayed with a smoothness oil agent at a concentration of 0.5% by fiber mass to obtain a multifunctional polyester fiber based on the antibacterial property of wormwood.

6. The method for preparing a multifunctional polyester fiber based on antibacterial wormwood according to claim 5, characterized in that: The preparation method of the wormwood extract comprises the following steps: C1. Rinse the wormwood in 5 times the volume of clean water until there is no dirt on the surface, and then dry the washed wormwood at a temperature of 20°C and a relative humidity of 50% at a turning frequency of 5h / time for 48h until the moisture content of the wormwood is reduced to 10-15%, and then place the dried wormwood in a grinder, and grind it at a speed of 1500r / min and a 10-50 mesh screen to obtain wormwood powder; C2. Mix the wormwood powder obtained in C1 with water and add it to the extraction tank, stir for 10 minutes at a stirring speed of 100 r / min, then start the heating system of the extraction tank, raise the temperature to 80-100°C at a heating rate of 5°C / min, then maintain the temperature of 80-100°C at a stirring speed of 80 r / min, a condensation temperature of 30°C, and a cooling water flow rate of 0.8 m / s. 3 / h, reflux extraction was performed for 3 hours, and then the extract was added to the plate and frame filter press at a flow rate of 0.5m / h in the delivery pipe. 3 / h, filtration pressure of 0.3MPa, and filtration using a 200-mesh filter cloth, taking the supernatant to obtain an wormwood extract; C3. Mix the wormwood extract obtained in C2 and the silane coupling agent, then add them to a reactor, turn on the stirring device, react for 2 hours at a stirring speed of 200 r / min and a temperature of 50°C, then stop heating and stirring; wait for the reaction system to cool to 30°C, connect the reactor to a vacuum distillation device, and perform vacuum distillation at a vacuum degree of -0.08 MPa, a distillation rate of 2 ml / min, and a temperature of 40-60°C. When the volume of the remaining liquid in the distillation device no longer decreases, obtain the wormwood extract.

7. The method for preparing a multifunctional polyester fiber based on antibacterial wormwood according to claim 6, characterized in that: The wormwood powder and water are prepared in a mass ratio of 1:8-15.

8. The method for preparing a multifunctional polyester fiber based on antibacterial wormwood according to claim 6, characterized in that: The extract and the silane coupling agent are prepared in a mass ratio of 1:5-10.

9. The method for preparing a multifunctional polyester fiber based on antibacterial wormwood according to claim 6, characterized in that: When the mugwort is crushed, a sieve with a mesh size of 30 is preferably used.

10. The method for preparing the antibacterial multifunctional polyester fiber based on wormwood according to claim 5, characterized in that: The lubricity oil agent is fatty acid polyethylene glycol ester.

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